CN111961540A - Preparation process of efficient decontamination type washing powder - Google Patents
Preparation process of efficient decontamination type washing powder Download PDFInfo
- Publication number
- CN111961540A CN111961540A CN202010675261.9A CN202010675261A CN111961540A CN 111961540 A CN111961540 A CN 111961540A CN 202010675261 A CN202010675261 A CN 202010675261A CN 111961540 A CN111961540 A CN 111961540A
- Authority
- CN
- China
- Prior art keywords
- heating
- sodium
- stirring
- decontamination
- washing powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000005202 decontamination Methods 0.000 title claims abstract description 46
- 230000003588 decontaminative effect Effects 0.000 title claims abstract description 46
- 238000005406 washing Methods 0.000 title claims abstract description 44
- 239000000843 powder Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 229920000642 polymer Polymers 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000003756 stirring Methods 0.000 claims abstract description 32
- -1 alkyl glycoside Chemical class 0.000 claims abstract description 31
- 239000003607 modifier Substances 0.000 claims abstract description 24
- 230000004913 activation Effects 0.000 claims abstract description 23
- 239000000178 monomer Substances 0.000 claims abstract description 22
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 18
- 239000003599 detergent Substances 0.000 claims abstract description 16
- VTIIJXUACCWYHX-UHFFFAOYSA-L disodium;carboxylatooxy carbonate Chemical compound [Na+].[Na+].[O-]C(=O)OOC([O-])=O VTIIJXUACCWYHX-UHFFFAOYSA-L 0.000 claims abstract description 12
- 229940045872 sodium percarbonate Drugs 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 9
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 9
- 238000001694 spray drying Methods 0.000 claims abstract description 8
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 6
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 6
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 6
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229930182470 glycoside Natural products 0.000 claims abstract description 6
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims abstract description 6
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 6
- 235000013599 spices Nutrition 0.000 claims abstract description 6
- 239000010457 zeolite Substances 0.000 claims abstract description 6
- 238000005086 pumping Methods 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 53
- 238000010438 heat treatment Methods 0.000 claims description 42
- 239000000243 solution Substances 0.000 claims description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- 239000000047 product Substances 0.000 claims description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 17
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 16
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 15
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 15
- 239000013078 crystal Substances 0.000 claims description 14
- 238000010992 reflux Methods 0.000 claims description 13
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 12
- GYHFUZHODSMOHU-UHFFFAOYSA-N nonanal Chemical compound CCCCCCCCC=O GYHFUZHODSMOHU-UHFFFAOYSA-N 0.000 claims description 12
- 238000002390 rotary evaporation Methods 0.000 claims description 12
- DMBHHRLKUKUOEG-UHFFFAOYSA-N N-phenyl aniline Natural products C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 claims description 10
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 claims description 10
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 10
- 238000001704 evaporation Methods 0.000 claims description 9
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000003999 initiator Substances 0.000 claims description 8
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 8
- BDDLHHRCDSJVKV-UHFFFAOYSA-N 7028-40-2 Chemical compound CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O BDDLHHRCDSJVKV-UHFFFAOYSA-N 0.000 claims description 7
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 7
- 239000002585 base Substances 0.000 claims description 7
- 125000001453 quaternary ammonium group Chemical group 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 6
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 claims description 6
- 229940106681 chloroacetic acid Drugs 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- OWXJKYNZGFSVRC-NSCUHMNNSA-N (e)-1-chloroprop-1-ene Chemical compound C\C=C\Cl OWXJKYNZGFSVRC-NSCUHMNNSA-N 0.000 claims description 5
- XPWMIGFSEWFXEZ-UHFFFAOYSA-N 2-prop-2-enoxybenzoic acid Chemical compound OC(=O)C1=CC=CC=C1OCC=C XPWMIGFSEWFXEZ-UHFFFAOYSA-N 0.000 claims description 5
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 claims description 5
- 239000011592 zinc chloride Substances 0.000 claims description 5
- 235000005074 zinc chloride Nutrition 0.000 claims description 5
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 4
- PDRZPYPZSSNYRP-UHFFFAOYSA-N NC1=CC=CC=C1.NC1=CC=CC=C1.C(C)(=O)O.C(C)(=O)O.C(C)(=O)O.C(C)(=O)O Chemical compound NC1=CC=CC=C1.NC1=CC=CC=C1.C(C)(=O)O.C(C)(=O)O.C(C)(=O)O.C(C)(=O)O PDRZPYPZSSNYRP-UHFFFAOYSA-N 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 3
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 3
- HRYZWHHZPQKTII-UHFFFAOYSA-N chloroethane Chemical compound CCCl HRYZWHHZPQKTII-UHFFFAOYSA-N 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 229960003750 ethyl chloride Drugs 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims description 3
- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical compound [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 claims description 3
- 235000009518 sodium iodide Nutrition 0.000 claims description 3
- ACWQWHCYOAGAKV-UHFFFAOYSA-N C1(=CC=CC=C1)NC1=CC=CC=C1.C(C)(=O)O.C(C)(=O)O.C(C)(=O)O.C(C)(=O)O Chemical compound C1(=CC=CC=C1)NC1=CC=CC=C1.C(C)(=O)O.C(C)(=O)O.C(C)(=O)O.C(C)(=O)O ACWQWHCYOAGAKV-UHFFFAOYSA-N 0.000 claims description 2
- 229960004050 aminobenzoic acid Drugs 0.000 claims description 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 2
- 238000006386 neutralization reaction Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 230000003213 activating effect Effects 0.000 claims 1
- 238000007865 diluting Methods 0.000 claims 1
- 238000000034 method Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 14
- 150000007524 organic acids Chemical class 0.000 abstract description 14
- 238000005502 peroxidation Methods 0.000 abstract description 7
- 238000006116 polymerization reaction Methods 0.000 abstract description 3
- 239000003921 oil Substances 0.000 description 18
- 235000019198 oils Nutrition 0.000 description 18
- 239000004744 fabric Substances 0.000 description 13
- 238000004061 bleaching Methods 0.000 description 11
- 125000000217 alkyl group Chemical group 0.000 description 8
- 102100040255 Tubulin-specific chaperone C Human genes 0.000 description 7
- BKIMMITUMNQMOS-UHFFFAOYSA-N nonane Chemical group CCCCCCCCC BKIMMITUMNQMOS-UHFFFAOYSA-N 0.000 description 7
- 108010093459 tubulin-specific chaperone C Proteins 0.000 description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- 239000012190 activator Substances 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 5
- 150000001451 organic peroxides Chemical class 0.000 description 5
- 235000002568 Capsicum frutescens Nutrition 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000008280 blood Substances 0.000 description 4
- 210000004369 blood Anatomy 0.000 description 4
- 239000000049 pigment Substances 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 3
- 150000001336 alkenes Chemical group 0.000 description 3
- 150000001408 amides Chemical class 0.000 description 3
- 238000010526 radical polymerization reaction Methods 0.000 description 3
- 230000002087 whitening effect Effects 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 125000002091 cationic group Chemical group 0.000 description 2
- 235000013353 coffee beverage Nutrition 0.000 description 2
- 238000004042 decolorization Methods 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 150000002338 glycosides Chemical class 0.000 description 2
- 229920000587 hyperbranched polymer Polymers 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- AFFLGGQVNFXPEV-UHFFFAOYSA-N n-decene Natural products CCCCCCCCC=C AFFLGGQVNFXPEV-UHFFFAOYSA-N 0.000 description 2
- RASPWLYDBYZRCR-UHFFFAOYSA-N pyrrolidin-1-ium-2-one;chloride Chemical compound Cl.O=C1CCCN1 RASPWLYDBYZRCR-UHFFFAOYSA-N 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical compound CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 description 1
- QGMGHALXLXKCBD-UHFFFAOYSA-N 4-amino-n-(2-aminophenyl)benzamide Chemical compound C1=CC(N)=CC=C1C(=O)NC1=CC=CC=C1N QGMGHALXLXKCBD-UHFFFAOYSA-N 0.000 description 1
- ORKQJTBYQZITLA-UHFFFAOYSA-N 4-octylaniline Chemical compound CCCCCCCCC1=CC=C(N)C=C1 ORKQJTBYQZITLA-UHFFFAOYSA-N 0.000 description 1
- 235000002566 Capsicum Nutrition 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 239000006002 Pepper Substances 0.000 description 1
- 235000016761 Piper aduncum Nutrition 0.000 description 1
- 235000017804 Piper guineense Nutrition 0.000 description 1
- 244000203593 Piper nigrum Species 0.000 description 1
- 235000008184 Piper nigrum Nutrition 0.000 description 1
- 235000019484 Rapeseed oil Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- VAZSKTXWXKYQJF-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)OOS([O-])=O VAZSKTXWXKYQJF-UHFFFAOYSA-N 0.000 description 1
- 125000002490 anilino group Chemical group [H]N(*)C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000003236 benzoyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C(*)=O 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 239000010635 coffee oil Substances 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 239000008233 hard water Substances 0.000 description 1
- 235000021539 instant coffee Nutrition 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005935 nucleophilic addition reaction Methods 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012764 semi-quantitative analysis Methods 0.000 description 1
- QSKQNALVHFTOQX-UHFFFAOYSA-M sodium nonanoyloxybenzenesulfonate Chemical compound [Na+].CCCCCCCCC(=O)OC1=CC=CC=C1S([O-])(=O)=O QSKQNALVHFTOQX-UHFFFAOYSA-M 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- FRPJTGXMTIIFIT-UHFFFAOYSA-N tetraacetylethylenediamine Chemical compound CC(=O)C(N)(C(C)=O)C(N)(C(C)=O)C(C)=O FRPJTGXMTIIFIT-UHFFFAOYSA-N 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/86—Mixtures of anionic, cationic, and non-ionic compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D207/00—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D207/02—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D207/18—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member
- C07D207/22—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D207/24—Oxygen or sulfur atoms
- C07D207/26—2-Pyrrolidones
- C07D207/263—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms
- C07D207/27—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms with substituted hydrocarbon radicals directly attached to the ring nitrogen atom
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F116/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical
- C08F116/12—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical by an ether radical
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D11/00—Special methods for preparing compositions containing mixtures of detergents
- C11D11/02—Preparation in the form of powder by spray drying
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/046—Salts
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/08—Silicates
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/10—Carbonates ; Bicarbonates
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
- C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
- C11D3/1246—Silicates, e.g. diatomaceous earth
- C11D3/128—Aluminium silicates, e.g. zeolites
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/39—Organic or inorganic per-compounds
- C11D3/3942—Inorganic per-compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/50—Perfumes
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/008—Polymeric surface-active agents
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/22—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/38—Cationic compounds
- C11D1/62—Quaternary ammonium compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/662—Carbohydrates or derivatives
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/10—Objects to be cleaned
- C11D2111/12—Soft surfaces, e.g. textile
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Detergent Compositions (AREA)
Abstract
The invention discloses a preparation process of high-efficiency decontamination washing powder, which comprises the following specific preparation processes: adding sodium dodecyl benzene sulfonate, alkyl glycoside, hyperbranched active decontamination polymer, 4A zeolite, sodium percarbonate, sodium silicate, sodium carbonate, spice and anhydrous sodium sulfate into water, stirring for 40-50min to obtain detergent slurry, and pumping the detergent slurry into a spray drying tower for spray drying to obtain the washing powder. A large amount of activation modifiers are uniformly distributed at the branched chain end of the hyperbranched active decontamination polymer prepared by the invention, and the activation modifiers generate high-activity peroxidation organic acid under the action of sodium percarbonate, so that the polymer after polymerization contains peroxidation organic acid in each monomer, the content of the peroxidation organic acid simultaneously acting on stains is improved, and the decontamination performance is improved.
Description
Technical Field
The invention belongs to the field of detergent preparation, and relates to a preparation process of high-efficiency decontamination washing powder.
Background
In the fabric washing process, colored stains which are difficult to wash usually need to use a detergent with a whitening function, so that a whitening agent and a bleaching activator are usually added into the detergent, and the whitening washing temperature of textiles can be reduced to 40-60 ℃ by using more bleaching activators such as tetraacetylethylenediamine and sodium nonanoyloxybenzenesulfonate, but the physical and chemical properties of the two bleaching activators at room temperature cannot meet the requirements.
Based on the above problems, research has been made in the prior art on a bleaching activator N- [4- (triethylammoniumtetramethylene benzoyl) ] butyrolactam chloride TBCC capable of reacting with hydrogen peroxide to generate a peroxygenated organic acid with high activity, and a high low-temperature bleaching effect can be achieved at normal temperature, which is widely used.
Disclosure of Invention
The invention aims to provide a preparation process of a high-efficiency decontamination type washing powder, which can effectively remove oil stains and stains by preparing a hyperbranched active decontamination polymer with high-efficiency bleaching and oil stain removal performances simultaneously, wherein a large amount of activation modifiers are uniformly distributed at the ends of branched chains in the prepared polymer, and the activation modifiers generate high-activity peroxyorganic acid under the action of sodium percarbonate, so that the polymerized polymer contains the peroxyorganic acid in each monomer, the content of the peroxyorganic acid simultaneously acting on the stains is increased, and the decontamination performance is improved.
The purpose of the invention can be realized by the following technical scheme:
a preparation process of high-efficiency decontamination washing powder comprises the following specific preparation processes:
firstly, continuously introducing nitrogen into a reaction tank for 30min, then adding a branched active monomer, an initiator and water, heating to 60-65 ℃, stirring for dissolving, reacting at a constant temperature for 1-2h, heating to 80 ℃, performing reflux reaction for 4h, and evaporating a product to remove the solvent to obtain the hyperbranched active decontamination polymer;
and secondly, adding sodium dodecyl benzene sulfonate, alkyl glycoside APG, hyperbranched active decontamination polymer, 4A zeolite, sodium percarbonate, sodium silicate, sodium carbonate, spice and anhydrous sodium sulfate into water, stirring for 40-50min to obtain detergent slurry, and pumping the detergent slurry into a spray drying tower for spray drying to obtain the washing powder.
The hyperbranched active decontamination polymer contains four olefin groups and four activation modifiers in four different directions respectively, can perform free radical polymerization reaction under the action of an initiator to generate a hyperbranched polymer, has high dispersion performance, and a large amount of activation modifiers are uniformly distributed at the end of a polymer branched chain, and the activation modifiers generate high-activity peroxidation organic acid under the action of sodium percarbonate, so that the polymerized polymer contains peroxidation organic acid in each monomer, the content of the peroxidation organic acid simultaneously acting on stains is improved, the decontamination efficiency is improved, meanwhile, each monomer contains two quaternary ammonium salts and one nonane chain, as the quaternary ammonium salts have high hydrophilicity and the nonane groups have high lipophilicity, the lipophilic groups can be adsorbed on oily or granular stains, and the peroxidation organic acid can effectively oxidize pigments in the stains, the polymer has a hyperbranched structure and high dispersion performance, so that the lipophilic group can be dispersed and dissolved in water after adsorbing the oil stain, and a high-efficiency decontamination effect is realized;
preferably, 39-43g of initiator and 4.3-4.5L of water are added into each kilogram of branched active monomer in the first step, wherein the initiator is one of sodium persulfate and ammonium persulfate;
preferably, the weight parts of the raw materials in the second step are as follows: 8-11 parts of sodium dodecyl benzene sulfonate, 7.3-9.2 parts of alkyl glycoside, 18.1-21.4 parts of hyperbranched active decontamination polymer, 8.6-9.4 parts of 4A zeolite, 6.7-7.1 parts of sodium percarbonate, 12.3-16.8 parts of sodium silicate, 7.4-7.6 parts of sodium carbonate, 0.1-0.13 part of spice and 41.2-46.3 parts of anhydrous sodium sulfate;
the specific preparation process of the branched reactive monomer is as follows:
step 1: adding aniline into a reaction tank, heating to 80-85 ℃, then adding hydrochloric acid and nonanal with the mass concentration of 30%, heating to 110-115 ℃, discharging air in the reaction tank, then continuously heating to 135 ℃, keeping the pressure at 0.12MPa, carrying out heat preservation reaction for 11-12h, stopping heating, adding water for dilution, adding alkali for neutralization to neutrality, then evaporating to remove unreacted aniline, simultaneously adding activated carbon for decolorization, filtering, cooling and crystallizing to obtain long-chain alkyl diphenylamine;
preferably, 42-47g of hydrochloric acid solution and 660g of nonanal 650-;
step 2: adding long-chain alkyl diphenylamine into an ethanol solution, stirring and dissolving, then dropwise adding a chloroacetic acid aqueous solution with the mass concentration of 35% into the ethanol solution under the control of the reaction temperature below 20 ℃, completely dropwise adding the chloroacetic acid aqueous solution under the control of the reaction temperature within 2 hours, then heating to 30-35 ℃, adding a sodium hydroxide solution with the mass concentration of 30% and a potassium iodide solution with the mass concentration of 6%, keeping the temperature, stirring and reacting for 2 hours, standing overnight, heating to 80-85 ℃ the next day, stirring and refluxing for 3-4 hours, then cooling and filtering, adjusting the pH of filtrate to 1 with hydrochloric acid, precipitating crystals, filtering, washing with distilled water to 3-4, and then drying to obtain tetraacetate diphenylamine;
preferably, 6.5 to 6.7L of ethanol solution is added into each kilogram of long-chain alkyl diphenylamine, 6.3 to 6.4kg of chloroacetic acid aqueous solution is added, 4.83 to 4.87kg of sodium hydroxide solution is added, and 0.14 to 0.15kg of potassium iodide solution is added;
and step 3: adding tetraacetate dianiline and acetone into a reaction tank, heating to 70-80 ℃, continuously introducing chloroethane into the reaction tank, carrying out reflux reaction for 7-8h, and carrying out rotary evaporation on the product to obtain quaternary ammonium base tetraacetic acid;
and 4, step 4: adding quaternary ammonium base tetraacetic acid, an activation modifier, zinc chloride and N, N-dimethylformamide into a reaction tank at the same time, heating to 85-90 ℃, stirring and mixing for 30min, then cooling to 65 ℃, adding phosphorus oxychloride, heating to 70-75 ℃, reacting for 4-5h, then adding water into the reaction tank, heating to 90-100 ℃, reacting for 40-50min, performing rotary evaporation on a product to remove a solvent in the product, adding water, stirring and dissolving, then cooling to 0 ℃, separating out crystals, washing the separated crystals with diethyl ether, and drying to obtain a branched active monomer;
preferably, 1.48-1.49kg of activation modifier is added into each kg of quaternary ammonium base tetraacetic acid, 321-328g of zinc chloride is added, and 261-268mL of phosphorus oxychloride is added;
the preparation method of the activation modifier comprises the following steps:
adding o-hydroxybenzoic acid and ethanol into a reaction tank at the same time, adding sodium ethoxide and sodium iodide after stirring and dissolving, heating to 60-65 ℃, dropwise adding chloropropene into the reaction tank, controlling the dropwise adding to be complete within 1h, then keeping the temperature for reaction for 7-8h, cooling to room temperature, then evaporating to remove the solvent, washing the obtained product once with ethyl ether, extracting with a sodium carbonate solution with the mass concentration of 5-7%, then adjusting the pH to 2 with hydrochloric acid, cooling to 5 ℃, separating out crystals, recrystallizing the separated crystals with ethanol with the mass concentration of 50%, and obtaining allyloxy benzoic acid;
preferably, in the step (i), the o-hydroxybenzoic acid and the chloropropene are added according to the mass ratio of 1: 1.23-1.26;
adding allyl aminobenzoic acid into the acetone solution, stirring and dissolving, adding thionyl chloride, heating to 70-75 ℃, performing reflux reaction for 8-9h, performing rotary evaporation, and removing dissolved and unreacted thionyl chloride to obtain allyloxy benzoyl chloride;
preferably, the allyloxybenzoic acid and the thionyl chloride are mixed according to the mass ratio of 1: 2.4-2.5;
thirdly, adding allyl benzoyl chloride into the acetone solution, stirring and dissolving, then adding 2-pyrrolidone and triethylamine, heating to 40-45 ℃, reacting for 4-5h, then filtering, simultaneously carrying out rotary evaporation on the filtrate, adding the obtained product into deionized water, and washing for 5-6 times to obtain an activation modifier; the prepared activation modifier contains an amide group, hydrogen peroxide decomposed by sodium percarbonate in the washing powder forms hydrogen peroxide anions under an alkaline condition, and carbonyl in the amide and the hydrogen peroxide anions perform nucleophilic addition to enable cyclic amine to leave, so that high-activity organic acid peroxide is formed, the pigment can be damaged, and the decontamination and bleaching performance is realized;
preferably, the ratio of the allyl benzoyl chloride, the 2-pyrrolidone and the triethylamine in terms of the amount of the substances is 1: 1.03-1.04: 2.12-2.16;
the invention has the beneficial effects that:
1. the hyperbranched active decontamination polymer prepared by the invention contains four olefin groups and four activation modifiers in four different directions respectively, can carry out free radical polymerization under the action of an initiator to generate a hyperbranched polymer, has higher dispersion performance, and a large amount of activation modifiers are uniformly distributed at the branched chain end of the polymer, and the activation modifiers generate high-activity peroxygenated organic acid under the action of sodium percarbonate, so that the polymerized polymer contains the peroxygenated organic acid in each monomer, the content of the peroxygenated organic acid simultaneously acting on stains is improved, the decontamination performance is improved, and the problem that the content of the peroxygenated organic acid simultaneously and effectively acting on the stains is reduced due to partial electrostatic repulsion of cationic groups when the TBCC bleaching activator directly acts on the stains in the prior art is solved, thereby reducing the decontamination bleaching effect.
2. Each monomer of the hyperbranched active decontamination polymer prepared by the invention contains two quaternary ammonium salts and one nonane chain, because the quaternary ammonium salts have higher hydrophilicity and the nonane groups have higher lipophilicity, the lipophilic groups can be adsorbed on oily or granular dirt, the peroxidized organic acid can effectively oxidize pigments in the dirt, and the peroxidized organic acid forms hydrophilic carboxylic acid anions after oxidation, so that the polymer contains a large amount of hydrophilic groups, the lipophilic groups can be dissolved in water after absorbing the oil dirt, and the oil dirt is prevented from being adhered, and because the polymer has a hyperbranched structure and higher dispersion performance, the lipophilic groups can be dispersed and dissolved in water after absorbing the oil dirt, thereby realizing high-efficiency decontamination effect, enabling the dirt and the oil dirt on fabrics to be removed when being overlapped, and further effectively solving the problem that the existing TBCC is difficult to be adsorbed on the oily dirt, thereby reducing contact with the stain and further reducing stain removal performance.
3. According to the invention, the long-chain lipophilic alkyl and the hydrophilic quaternary ammonium salt are directly introduced to the monomer in the preparation process of the hyperbranched active decontamination polymer, so that the action point positions of the lipophilic group and the hydrophilic group can be effectively controlled in the polymerization process, the prepared polymer has stable performance, and the influence on the overall performance of the polymer due to the uneven dispersion of the long-chain alkyl in the polymer caused by the direct polymerization of the branched monomer and the monomer containing the long-chain alkyl is effectively avoided.
Detailed Description
Example 1:
the preparation method of the activation modifier comprises the following steps:
adding 1mol of o-hydroxybenzoic acid and 500mL of ethanol into a reaction tank at the same time, stirring and dissolving, adding 24g of sodium ethoxide and 13g of sodium iodide, heating to 60 ℃, dropwise adding 1.24mol of chloropropene, controlling the dropwise addition within 1h to be complete, then keeping the temperature and reacting for 7h, cooling to room temperature, evaporating to remove the solvent, washing the obtained product once with diethyl ether, extracting with a 7% sodium carbonate solution, adjusting the pH to 2 with hydrochloric acid, cooling to 5 ℃, separating out crystals, and recrystallizing the separated crystals with 50% ethanol to obtain allyloxybenzoic acid; the product was analyzed by infrared analysis at 1649cm-1(olefin characteristic peaks);
adding 1mol of allyloxybenzoic acid into 500mL of acetone solution, stirring for dissolving, adding 2.4mol of thionyl chloride, heating to 75 ℃, carrying out reflux reaction for 9 hours, and then carrying out rotary evaporation to remove the dissolved thionyl chloride and unreacted thionyl chloride to obtain allyloxybenzoyl chloride; the product was analyzed by infrared analysis at 1784cm-1(characteristic peaks of acid chloride);
③ adding 1mol of allyl benzoyl chloride into 700mL of acetone solution, stirring and dissolving, then adding 1.03mol of 2-pyrrolidone and 2.14mol of triethylamine, heating to 40-4 ℃, reacting for 5 hours, then filtering, simultaneously carrying out rotary evaporation on the filtrate, adding the obtained product into deionized water, and washing for 5-6 times to obtain an activation modifier; the product was analyzed by infrared analysis at 1674cm-1(amide characteristic peak).
Example 2:
a preparation process of high-efficiency decontamination washing powder comprises the following specific preparation processes:
the first step is as follows: adding 1kg aniline into a reaction tank, heating to 85 deg.C, adding 45g hydrochloric acid with 30% mass concentration and 650g nonanal, heating to 115 deg.C, discharging air from the reaction tank, heating to 135 deg.C under 0.12MPa, and maintaining the temperatureReacting for 12h, stopping heating, adding alkali to neutralize to neutrality after adding water for dilution, then evaporating to remove unreacted aniline, simultaneously adding activated carbon for decolorization, filtering, cooling and crystallizing to obtain long-chain alkyl diphenylamine, and detecting by GC-MS: long chain alkyl bis-anilines (C)21H30N2) Has a molecular weight of 310.163;
the second step is that: adding 1kg of long-chain alkyl diphenylamine into 6.6L of ethanol solution, stirring for dissolving, controlling the reaction temperature below 20 ℃, dropwise adding 6.4kg of chloroacetic acid aqueous solution with the mass concentration of 35%, controlling the dropwise addition to be complete within 2h, heating to 35 ℃, adding 4.85kg of sodium hydroxide solution with the mass concentration of 30% and 0.14kg of potassium iodide solution with the mass concentration of 6%, keeping the temperature, stirring for reacting for 2h, standing overnight, heating to 85 ℃ the next day, stirring and refluxing for reacting for 4h, cooling and filtering, adjusting the pH of filtrate to 1 with hydrochloric acid, precipitating crystals, filtering, washing with distilled water to 3, drying to obtain tetraacetate dianiline, wherein the reaction formula is shown below, and the infrared analysis on the product shows that 1712cm of the product-1(characteristic peaks of carboxyl group) and-NH-in anilino group2The double peak of (1) disappears;
the third step: adding 1kg of tetraacetoxy dianiline and 4L of acetone into a reaction tank, heating to 80 ℃, then continuously introducing chloroethane into the reaction tank, carrying out reflux reaction for 7-8h, carrying out rotary evaporation on the product to obtain quaternary ammonium base tetraacetic acid, and carrying out X-ray photoelectron spectroscopy (XPS) analysis on the product to know that the percentage content of chlorine atoms is 11.6%, so that chlorine elements are successfully introduced into the product, and a certain error exists between a measured value and an actual value because the XPS is semi-quantitative analysis;
the fourth step: 1kg of quaternary ammonium base tetraacetic acid, 1.486kg of the activation modifier prepared in example 1, 325g of zinc chloride and 5LN, N-dimethylformamide are added into a reaction tank at the same time, the temperature is increased to 90 ℃, stirring and mixing are carried out for 30min, then the reaction tank is cooled to 65 ℃, 266mL of phosphorus oxychloride is added, the reaction tank is heated to 70 ℃ for 5h, then water is added, and the temperature is increased to 70 DEG, and the reaction tank is heated to 70 DEG, reacted for 5hHeating to 100 deg.C for 40min, performing rotary evaporation to remove solvent, adding into water, stirring for dissolving, cooling to 0 deg.C to precipitate crystal, washing with diethyl ether, and oven drying to obtain branched active monomer, performing infrared analysis on the product, 1674cm-1(amide characteristic Peak) at 1712cm-1The absorption peak of carboxyl groups at (A) disappears,
fifthly, continuously introducing nitrogen into the reaction tank for 30min, then adding 1kg of branched active monomer, 40g of sodium persulfate and 4.4L of water, heating to 65 ℃, stirring for dissolving, reacting at constant temperature for 1.5h, heating to 80 ℃, performing reflux reaction for 4h, and evaporating the product to remove the solvent to obtain the hyperbranched active decontamination polymer;
sixthly, adding 80g of sodium dodecyl benzene sulfonate, 75g of alkyl glycoside APG, 190g of hyperbranched active decontamination polymer, 87g of 4A zeolite, 68g of sodium percarbonate, 140g of sodium silicate, 75g of sodium carbonate, 1.2g of spice and 424g of anhydrous sodium sulfate into water, stirring for 40-50min to obtain detergent slurry, controlling the water addition amount until the slurry flows, and pumping the detergent slurry into a spray drying tower for spray drying to obtain the washing powder.
Adding the prepared washing powder into water, stirring and dissolving, controlling the addition of 3-5g of washing powder per liter of water, soaking the colored fabric in water at 50 ℃ and 30 ℃ for 5 hours respectively, rinsing, and observing that the colored fabric does not fade.
Example 3:
the preparation process of the efficient decontamination washing powder is the same as that in the example 2, and the nonanal used in the first step in the example 2 is replaced by formaldehyde.
Example 4:
the preparation process of the efficient decontamination washing powder is the same as that in the embodiment 2, the preparation process in the first step in the embodiment 2 is omitted, and the long-chain alkyl diphenylamine in the preparation process in the second step is replaced by 4-octylaniline.
Example 5:
a preparation process of efficient decontamination type washing powder is the same as that in example 2, nonanal used in the first step in example 2 is replaced by formaldehyde, nitrogen is continuously introduced into a reaction tank for 30min in the fifth step reaction process, then 1kg of branched active monomer, 40g of sodium persulfate and 4.4L of water are added into the reaction tank, the temperature is increased to 65 ℃, the mixture is stirred and dissolved, the constant temperature reaction is carried out for 1.5h, then the temperature is increased to 80 ℃, 102g of n-decene is added into the reaction tank for reflux reaction for 4h, and the product is evaporated to remove the solvent in the reaction tank, so that the hyperbranched active decontamination polymer is obtained.
Example 6:
a preparation process of high-efficiency decontamination type washing powder is the same as that in example 2, and the hyperbranched active decontamination polymer in example 2 is replaced by N- [4- (triethylammonium methylene benzoyl) ] butyrolactam chloride TBCC.
Test example:
taking the same white cotton fiber cloth, soaking the cloth in instant coffee with the concentration of 0.2g/mL for 2h, fishing out, drying, pouring rapeseed oil on the surface of the cloth, drying in the air, wherein coffee stains and oil stains are arranged on the surface of the cloth, simultaneously pouring chili oil and pig blood on the surface of two groups of cloth, drying in the air, wherein the chili oil stains and blood stains are arranged on the cloth, placing the dried cloth for a week, washing by using the washing powder prepared in the above examples 2-6, testing the cloth with the coffee oil stains, the blood stains and the chili oil stains by using an RHLQ-III type vertical decontamination machine (experimental conditions are that the washing concentration is 0.2%, the washing concentration is 30 ℃, 250ppm hard water, the washing time is 20min, and the rotating speed is 120rpm), then determining the whiteness value P0 before the stain staining of the sample is detected by using a WSD-3C full-automatic whiteness meter according to GB/T13174 + 2008, and determining the whiteness value of the cloth before the stain of the sample is washed and the sample is located on the The whiteness values of spots, bloodstains and pepper oil spots are P1, the whiteness retention ratio W is calculated to be P1/P0 multiplied by 100%, the larger the P value is, the better the stain removal effect is, and the measurement results are shown in Table 1;
TABLE 1 measurement of whiteness retention%
| Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | |
| Oil stain of coffee | 98.7 | 85.2 | 87.6 | 94.3 | 79.8 |
| Blood stain | 98.1 | 83.3 | 84.5 | 93.1 | 77.4 |
| Chili oil | 98.3 | 81.6 | 88.6 | 94.9 | 76.8 |
As can be seen from table 1, the laundry powder prepared in example 2 has high detergency, because the laundry powder is added with the hyperbranched active detergent polymer, a large number of activation modifiers are uniformly distributed at the ends of the branched chains of the hyperbranched active detergent polymer, and the activation modifiers generate high-activity organic peroxide under the action of sodium percarbonate, each monomer in the polymerized polymer contains organic peroxide, so that the content of the organic peroxide simultaneously acting on stains is increased, and the detergency efficiency is improved, and each monomer contains two quaternary ammonium salts and one nonane chain, because the quaternary ammonium salts have high hydrophilicity, and the nonane groups have high lipophilicity, the lipophilic group can be adsorbed on oily or granular stains, so that the organic peroxide can effectively oxidize pigments in the stains, and the organic peroxide oxidizes to form hydrophilic carboxylic acid anions, the polymer contains a large amount of hydrophilic groups, so that the lipophilic groups can be dissolved in water after absorbing oil stains to prevent the oil stains from being adhered, and the polymer has a hyperbranched structure and high dispersing performance, and can be dispersed and dissolved in water after the lipophilic groups absorb the oil stains to realize an efficient decontamination effect; while in example 3, the nonane bond is not introduced to the monomer, so that the content of lipophilic groups is reduced, the adsorption performance with oil stains is reduced, and the stain removal performance of the detergent is reduced, meanwhile, in example 4, the prepared polymer is not a hyperbranched structure, so that the content of introduced organic acid peroxide is reduced, the action sites on the stains are reduced, and the stain removal performance of the detergent powder is reduced, meanwhile, in example 5, since the long-chain alkyl is directly introduced in a free radical polymerization manner, the alkyl chain is easily dispersed unevenly, the adsorption sites are uneven, and the stain removal performance is reduced, in example 6, the TBCC is directly added, the TBCC is hardly adsorbed on the oily stains, so that the contact with the stains is reduced, and the bleaching performance is reduced, and meanwhile, when the TBCC bleaching activator directly acts on the stains, due to partial electrostatic repulsion of cationic groups, so that the content of the organic acid peroxide which effectively acts on the stains is reduced, and the decontamination effect is reduced.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (9)
1. A preparation process of high-efficiency decontamination washing powder is characterized by comprising the following specific preparation processes:
adding long-chain alkyl diphenylamine into an ethanol solution, stirring and dissolving, then dropwise adding a chloroacetic acid aqueous solution with the mass concentration of 35% into the ethanol solution at the reaction temperature of below 20 ℃, heating to 30-35 ℃, adding a sodium hydroxide solution with the mass concentration of 30% and a potassium iodide solution with the mass concentration of 6%, keeping the temperature, stirring and reacting for 2 hours, standing overnight, heating to 80-85 ℃ the next day, stirring and refluxing for 3-4 hours, then cooling and filtering, adjusting the pH value of the filtrate to be 1 by hydrochloric acid, precipitating crystals, filtering, washing by using distilled water until the pH value is 3-4, and then drying to obtain tetraacetate diphenylamine;
the second step is that: adding tetraacetate dianiline and acetone into a reaction tank, heating to 70-80 ℃, continuously introducing chloroethane into the reaction tank, carrying out reflux reaction for 7-8h, and carrying out rotary evaporation on the product to obtain quaternary ammonium base tetraacetic acid;
the third step: adding quaternary ammonium base tetraacetic acid, an activation modifier, zinc chloride and N, N-dimethylformamide into a reaction tank at the same time, heating to 85-90 ℃, stirring and mixing for 30min, then cooling to 65 ℃, adding phosphorus oxychloride, heating to 70-75 ℃, reacting for 4-5h, then adding water into the reaction tank, heating to 90-100 ℃, reacting for 40-50min, performing rotary evaporation on a product to remove a solvent in the product, adding water, stirring and dissolving, then cooling to 0 ℃, separating out crystals, washing the separated crystals with diethyl ether, and drying to obtain a branched active monomer;
step four, continuously introducing nitrogen into the reaction tank for 30min, then adding a branched active monomer, an initiator and water, heating to 60-65 ℃, stirring for dissolving, reacting at constant temperature for 1-2h, heating to 80 ℃, performing reflux reaction for 4h, and evaporating the product to remove the solvent to obtain the hyperbranched active decontamination polymer;
and fifthly, adding sodium dodecyl benzene sulfonate, alkyl glycoside, hyperbranched active decontamination polymer, 4A zeolite, sodium percarbonate, sodium silicate, sodium carbonate, spice and anhydrous sodium sulfate into water, stirring for 40-50min to obtain detergent slurry, and pumping the detergent slurry into a spray drying tower for spray drying to obtain the washing powder.
2. The process of claim 1, wherein in the second step, 6.5 to 6.7L of ethanol solution, 6.3 to 6.4kg of chloroacetic acid aqueous solution, 4.83 to 4.87kg of sodium hydroxide solution and 0.14 to 0.15kg of potassium iodide solution are added to each kg of long-chain alkyl diphenylamine.
3. The process for preparing the detergent powder according to claim 1, wherein in the third step, 1.48-1.49kg of activating modifier, 321-328g of zinc chloride and 261-268mL of phosphorus oxychloride are added to each kg of quaternary ammonium salt tetraacetic acid.
4. The process for preparing the high-efficiency decontamination type washing powder according to claim 1, wherein in the fourth step, 39-43g of initiator is added per kilogram of branched active monomer, and 4.3-4.5L of water is added, wherein the initiator is one of sodium persulfate and ammonium persulfate.
5. The preparation process of the efficient decontamination type washing powder according to claim 1, wherein the fifth step comprises the following raw materials in parts by weight: 8-11 parts of sodium dodecyl benzene sulfonate, 7.3-9.2 parts of alkyl glycoside, 18.1-21.4 parts of hyperbranched active decontamination polymer, 8.6-9.4 parts of 4A zeolite, 6.7-7.1 parts of sodium percarbonate, 12.3-16.8 parts of sodium silicate, 7.4-7.6 parts of sodium carbonate, 0.1-0.13 part of spice and 41.2-46.3 parts of anhydrous sodium sulfate.
6. The preparation process of the high-efficiency decontamination type washing powder according to claim 1 or 2, characterized in that the long-chain alkyl diphenylamine is prepared by the following steps: adding aniline into a reaction tank, heating to 80-85 ℃, then adding hydrochloric acid and nonanal with the mass concentration of 30%, heating to 110-115 ℃, discharging air in the reaction tank, then heating to 135 ℃ for reaction for 11-12h, stopping heating, adding alkali for neutralization to neutrality after diluting with water, then evaporating to remove unreacted aniline, filtering, cooling and crystallizing to obtain long-chain alkyl diphenylamine.
7. The preparation process of the high-efficiency decontamination type washing powder according to claim 1, wherein the preparation method of the activation modifier is as follows:
adding o-hydroxybenzoic acid and ethanol into a reaction tank at the same time, adding sodium ethoxide and sodium iodide after stirring and dissolving, heating to 60-65 ℃, dropwise adding chloropropene into the reaction tank, controlling the dropwise adding to be complete within 1h, then keeping the temperature for reaction for 7-8h, cooling to room temperature, then evaporating to remove the solvent, washing the obtained product once with ethyl ether, extracting with a sodium carbonate solution with the mass concentration of 5-7%, then adjusting the pH to 2 with hydrochloric acid, cooling to 5 ℃, separating out crystals, recrystallizing the separated crystals with ethanol with the mass concentration of 50%, and obtaining allyloxy benzoic acid;
adding allyl aminobenzoic acid into the acetone solution, stirring and dissolving, adding thionyl chloride, heating to 70-75 ℃, performing reflux reaction for 8-9h, performing rotary evaporation, and removing dissolved and unreacted thionyl chloride to obtain allyloxy benzoyl chloride;
③ adding allyl benzoyl chloride into acetone solution, stirring and dissolving, then adding 2-pyrrolidone and triethylamine, heating to 40-45 ℃, reacting for 4-5h, then filtering, simultaneously carrying out rotary evaporation on the filtrate, adding the obtained product into deionized water, and washing to obtain the activation modifier.
8. The preparation process of the efficient decontamination type washing powder according to claim 7, wherein in the step (i), the o-hydroxybenzoic acid and the chloropropene are added according to the mass ratio of 1: 1.23-1.26.
9. The preparation process of the efficient decontamination type washing powder according to claim 7, wherein the ratio of the allyl benzoyl chloride, the 2-pyrrolidone and the triethylamine in the step (c) is 1: 1.03-1.04: 2.12-2.16.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010675261.9A CN111961540B (en) | 2020-07-14 | 2020-07-14 | Preparation process of decontamination type washing powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010675261.9A CN111961540B (en) | 2020-07-14 | 2020-07-14 | Preparation process of decontamination type washing powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111961540A true CN111961540A (en) | 2020-11-20 |
| CN111961540B CN111961540B (en) | 2021-08-31 |
Family
ID=73361634
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010675261.9A Active CN111961540B (en) | 2020-07-14 | 2020-07-14 | Preparation process of decontamination type washing powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111961540B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113081886A (en) * | 2021-04-15 | 2021-07-09 | 南京泛成生物科技有限公司 | Alkyl polyglycoside solid preparation, preparation method and application |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5047577A (en) * | 1985-10-01 | 1991-09-10 | Ethyl Corporation | Quaternary ammonium compounds |
| JPH0733722A (en) * | 1993-07-20 | 1995-02-03 | Lion Corp | Acyloxyanilide derivative, bleach activation agent and bleaching agent composition, bleaching detergent and fungicide containing the agent |
| CN1133340A (en) * | 1994-11-08 | 1996-10-16 | 花王株式会社 | Liquid bleaching agent compositions |
| CN1160419A (en) * | 1994-08-31 | 1997-09-24 | 普罗格特-甘布尔公司 | Perhydrolysis-selective bleach activators |
| US6214785B1 (en) * | 1998-09-09 | 2001-04-10 | Clariant Gmbh | Bleach activator granules |
| US20090233829A1 (en) * | 2004-11-01 | 2009-09-17 | Stacie Ellen Hecht | Multiphase cleaning compositions having ionic liquid phase |
| CN103554024A (en) * | 2013-11-22 | 2014-02-05 | 江南大学 | Synthesis method for cationic bleaching activating agents with surface activity |
| CN104877807A (en) * | 2015-04-16 | 2015-09-02 | 江南大学 | Synthesis method of polymerizable cationic bleaching activator |
| CN109053527A (en) * | 2018-07-27 | 2018-12-21 | 江南大学 | A kind of synthetic method and application of macromolecule cation type bleach-activating |
-
2020
- 2020-07-14 CN CN202010675261.9A patent/CN111961540B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5047577A (en) * | 1985-10-01 | 1991-09-10 | Ethyl Corporation | Quaternary ammonium compounds |
| JPH0733722A (en) * | 1993-07-20 | 1995-02-03 | Lion Corp | Acyloxyanilide derivative, bleach activation agent and bleaching agent composition, bleaching detergent and fungicide containing the agent |
| CN1160419A (en) * | 1994-08-31 | 1997-09-24 | 普罗格特-甘布尔公司 | Perhydrolysis-selective bleach activators |
| CN1133340A (en) * | 1994-11-08 | 1996-10-16 | 花王株式会社 | Liquid bleaching agent compositions |
| US6214785B1 (en) * | 1998-09-09 | 2001-04-10 | Clariant Gmbh | Bleach activator granules |
| US20090233829A1 (en) * | 2004-11-01 | 2009-09-17 | Stacie Ellen Hecht | Multiphase cleaning compositions having ionic liquid phase |
| CN103554024A (en) * | 2013-11-22 | 2014-02-05 | 江南大学 | Synthesis method for cationic bleaching activating agents with surface activity |
| CN104877807A (en) * | 2015-04-16 | 2015-09-02 | 江南大学 | Synthesis method of polymerizable cationic bleaching activator |
| CN109053527A (en) * | 2018-07-27 | 2018-12-21 | 江南大学 | A kind of synthetic method and application of macromolecule cation type bleach-activating |
Non-Patent Citations (1)
| Title |
|---|
| CHANGHAI XU: "Bleaching cellulosic fibers via pre-sorption of N -[4-(triethylammoniomethyl)-benzoyl]-butyrolactam chloride", 《CELLULOSE》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113081886A (en) * | 2021-04-15 | 2021-07-09 | 南京泛成生物科技有限公司 | Alkyl polyglycoside solid preparation, preparation method and application |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111961540B (en) | 2021-08-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Hebeish et al. | Synthesis of carboxymethyl cellulose (CMC) and starch-based hybrids and their applications in flocculation and sizing | |
| CN105613506B (en) | A kind of halogen amine/quaternary ammonium olefines antiseptic and its application in Biodegradable nano fibrous material | |
| Hashem et al. | Crosslinking of partially carboxymethylated cotton fabric via cationization | |
| JP7153286B2 (en) | Multifunctional resin and its production method and application | |
| CN111961540B (en) | Preparation process of decontamination type washing powder | |
| Mondal et al. | Graft polymerization of vinyl monomers onto cotton fibres pretreated with amines: Mechanical property and moisture sorption | |
| Cerkez et al. | Antimicrobial coatings for polyester and polyester/cotton blends | |
| FR2460971A1 (en) | VINYL ALCOHOL COPOLYMERS CONTAINING CATIONIC RADICALS, USEFUL IN PAPERMAKING, AND PROCESS FOR THEIR PREPARATION | |
| FR2466474A1 (en) | POLYMER EMULSION WITH CATIONIC CHARACTER | |
| CN108467465A (en) | A kind of preparation method of graphene modified ethylene acetate-copolymer-maleic anhydride flame-retardant leather retanning agent | |
| JP5141915B2 (en) | High whiteness discoloration resistance cross-linked acrylate fiber | |
| WO2001058967A1 (en) | Polymer compositions useful as dye complexing agents, and processes for preparing same | |
| CN101389803B (en) | Process for production of composite fiber | |
| CN107474178A (en) | Pigment adsorbent and preparation method thereof | |
| JP6139991B2 (en) | Carboxyl group-containing polymer composition | |
| CN105924573A (en) | Perfluoroalkyl polyene ester waterproof agent, preparation method and application | |
| CN109053527B (en) | Synthetic method and application of high-molecular cationic bleaching activator | |
| Ma et al. | Antibacterial modification of cotton fabric through argon plasma-induced grafting polymerization | |
| CN106084243B (en) | The method that backbone modification isocyanates grafted cation side chain prepares polycarboxylate water-reducer | |
| CN115678192B (en) | Repairable hydrogel composition, preparation method and application | |
| EP3870182A1 (en) | Functionalized materials and compounds | |
| CN110820339A (en) | High-concentration fluorine-containing water and oil repellent agent for textiles and preparation method thereof | |
| KR101542710B1 (en) | Whiteness enhancers for peroxide bleaching and fluorescent dyestuff dyeing | |
| JP2010216050A (en) | High brightness crosslinked acrylate-based fiber having color fastness and method for producing the same | |
| RU2435890C1 (en) | Composition for fire-proof treatment of polyether fibres |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |