CN106854295A - A kind of whiteness red phosphorus, nylon distribute whiteness red phosphorus flame-retardant masterbatch and preparation method thereof with low smell is low - Google Patents
A kind of whiteness red phosphorus, nylon distribute whiteness red phosphorus flame-retardant masterbatch and preparation method thereof with low smell is low Download PDFInfo
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- CN106854295A CN106854295A CN201611105835.9A CN201611105835A CN106854295A CN 106854295 A CN106854295 A CN 106854295A CN 201611105835 A CN201611105835 A CN 201611105835A CN 106854295 A CN106854295 A CN 106854295A
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- red phosphorus
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- nylon
- whiteness
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 239000004677 Nylon Substances 0.000 title claims abstract description 36
- 229920001778 nylon Polymers 0.000 title claims abstract description 36
- 239000003063 flame retardant Substances 0.000 title claims abstract description 34
- 239000004594 Masterbatch (MB) Substances 0.000 title claims abstract description 33
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 18
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 18
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 15
- 238000001179 sorption measurement Methods 0.000 claims abstract description 15
- 239000000314 lubricant Substances 0.000 claims abstract description 9
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 18
- 239000005011 phenolic resin Substances 0.000 claims description 18
- 229920001568 phenolic resin Polymers 0.000 claims description 18
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 15
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 14
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 12
- 229920002292 Nylon 6 Polymers 0.000 claims description 11
- 239000003094 microcapsule Substances 0.000 claims description 11
- -1 pentaerythritol ester Chemical class 0.000 claims description 11
- 229910000077 silane Inorganic materials 0.000 claims description 11
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 10
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical group CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000001125 extrusion Methods 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 229920001296 polysiloxane Polymers 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 6
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical group O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 6
- 235000019260 propionic acid Nutrition 0.000 claims description 5
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 5
- 229940123457 Free radical scavenger Drugs 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 230000002421 anti-septic effect Effects 0.000 claims description 4
- ZYGHJZDHTFUPRJ-UHFFFAOYSA-N coumarin Chemical compound C1=CC=C2OC(=O)C=CC2=C1 ZYGHJZDHTFUPRJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000005189 flocculation Methods 0.000 claims description 4
- 230000016615 flocculation Effects 0.000 claims description 4
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 150000008301 phosphite esters Chemical class 0.000 claims description 4
- 239000002516 radical scavenger Substances 0.000 claims description 4
- 229920005989 resin Polymers 0.000 claims description 4
- 239000011347 resin Substances 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 229910021536 Zeolite Inorganic materials 0.000 claims description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 239000003610 charcoal Substances 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 3
- 229940056319 ferrosoferric oxide Drugs 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 3
- 239000002808 molecular sieve Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 235000011837 pasties Nutrition 0.000 claims description 3
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 3
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 3
- 239000010457 zeolite Substances 0.000 claims description 3
- 239000011701 zinc Substances 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 2
- DQMUQFUTDWISTM-UHFFFAOYSA-N O.[O-2].[Fe+2].[Fe+2].[O-2] Chemical compound O.[O-2].[Fe+2].[Fe+2].[O-2] DQMUQFUTDWISTM-UHFFFAOYSA-N 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- XIVNZHXRIPJOIZ-UHFFFAOYSA-N octadecanoic acid;zinc Chemical compound [Zn].CCCCCCCCCCCCCCCCCC(O)=O XIVNZHXRIPJOIZ-UHFFFAOYSA-N 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims 2
- 239000004411 aluminium Substances 0.000 claims 1
- 229910052782 aluminium Inorganic materials 0.000 claims 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims 1
- 238000009775 high-speed stirring Methods 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 1
- 239000004408 titanium dioxide Substances 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 239000000428 dust Substances 0.000 abstract description 2
- 239000004480 active ingredient Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 229920002401 polyacrylamide Polymers 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003856 thermoforming Methods 0.000 description 2
- 239000005909 Kieselgur Substances 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 101150103639 PB1 gene Proteins 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 244000061458 Solanum melongena Species 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004359 castor oil Substances 0.000 description 1
- 235000019438 castor oil Nutrition 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004079 fireproofing Methods 0.000 description 1
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical class OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000000979 retarding effect Effects 0.000 description 1
- 231100000004 severe toxicity Toxicity 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2477/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K2003/026—Phosphorus
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
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Abstract
The invention discloses a kind of nylon with low smell, it is low distribute, whiteness red phosphorus flame-retardant masterbatch and preparation method thereof, it is prepared from by weight by following components：50 85 parts of whiteness red phosphorus, 15 parts of hydrophobic type odor adsorption master batch, 0.2~1.0 part of antioxidant, 0.2 1 parts of lubricant.The red phosphorus flame-retardant masterbatch versatility for preparing of the invention is wide, active ingredient is high, low without obvious smell, addition, and preparation method is simple, while also breaching the limitation in color, product is not limited to dark product, and dust pollution can be effectively reduced, improve work situation.
Description
Technical field
The present invention relates to a kind of whiteness red phosphorus, low smell, low distribute modified red phosphorus flame-retardant nylon material and its preparation side
Method, belongs to technical field of polymer materials.
Background technology
Nylon is the general engineering plastic with excellent comprehensive performance, with excellent mechanical performance and wear-resisting, solvent resistant,
The advantages of oil resistant, it is widely used in every profession and trade.But nylon belongs to combustible material, in order to meet flame retardant products requirement, it is necessary to
Numerous studies are carried out to fire-retardant aspect.And red phosphorus is a kind of excellent halogen-free environment-friendly type flame-proof agent, flame retarding efficiency is high, with other resistances
Combustion agent is compared, and addition needed for reaching identical fire-retardant rank is few, thus small on the physical and mechanical property influence of material.But it is also deposited
Such as oxidizable rotten in atmosphere in some shortcomings, the easy moisture absorption, oxidation generate phosphoric acid and discharge severe toxicity in atmosphere for exposure
Phosphine gas, the aubergine of itself has limitation to preparing light plastic products.Therefore, red phosphorus is used as fire retardant, only
Have by just there is actual application value after surface treatment.
The content of the invention
It is an object of the invention to provide a kind of whiteness red phosphorus, nylon with low smell, it is low distribute, whiteness red phosphorus flame-retardant it is female
Grain and preparation method thereof.
In order to realize the purpose of the present invention, the invention provides a kind of whiteness red phosphorus, described whiteness red phosphorus is micro-
Capsule red phosphorus, described microcapsule red phosphorus are aluminium hydroxide and the double encapsulated red phosphorus of phenolic resin, the preparation of the microcapsule red phosphorus：
It is made of the raw material including following weight proportion：Red phosphorus 25-35%, aluminum sulfate 5-15%, urea 10-15%, water 50-
59%, oil-soluble phenolic resin resin 1-5%；Aluminium hydroxide coats process：Aluminum sulfate is added to the water first, stirring has been allowed to
CL, then puts into red phosphorus, stirs 20min, then is transferred in ball mill and is ground to red phosphorus particle diameter untill 5-10um,
Then it is transferred in reactor, adds caustic soda (5-15wt% solution) slowly while stirring, untill the PH=5-6 of system, then
It (can be the flocculation agents such as conventional PB1 gene or polyacrylamide PAM, consumption may generally be system to add flocculation agent
The 0.1%-1% of weight), stir, in 75-85 DEG C of scope inside holding 1.5h, filtering is eventually passed, washed, be dried to obtain
Aluminium hydroxide encapsulated red phosphorus；Phenolic resin coats process：Dimethylbenzene first with 2.5-3.0 times of volume is dilute by oil-soluble phenolic resin
Release, then aluminium hydroxide encapsulated red phosphorus are mixed with oil-soluble phenolic resin dilution, stir into pasty state homogeneous state, send into band
Reclaim in the drier of xylene unit, 60 ± 5 DEG C of temperature of control is dried, and obtains final product aluminium hydroxide and phenolic resin double-contracting is covered
Red phosphorus.
Present invention also offers a kind of nylon with low smell, it is low distribute, whiteness red phosphorus flame-retardant masterbatch, pressed by following components
Weight portion is prepared from：
Whiteness red phosphorus 20-50,
The 45-80 of nylon 6
1-5 parts of hydrophobic type odor adsorption master batch,
Silane coupler 0.5-1 parts
0.2~1.0 part of antioxidant
0.2~1.0 part of lubricant
Described whiteness red phosphorus is microcapsule red phosphorus, and described microcapsule red phosphorus are aluminium hydroxide and phenolic resin double-contracting
Cover red phosphorus.
The described inherent viscosity of nylon 6 is 2.0-3.6.
Described hydrophobic type odor adsorption master batch is made up of the component of following weight portion：40~75 parts of PA6, hydrophobicity silicon
10~20 parts of diatomaceous earth, 1~5 part of ferriferous oxide, 0~10 part of hydrophobic active charcoal, 5~10 parts of needle-like zeolite molecular sieve, castor oil
5~10 parts of sour zinc, 5~10 parts of antiseptic, 0.1-0.5 parts of Benzopyranone kind the free radical scavenger, [β-(3,5- of antioxidant four
Di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 0.2-0.5 parts, antioxidant three [2.4- di-tert-butyl-phenyls] phosphorous acid
Ester 0.2-0.5 parts, 0.5-1.0 parts of lubricant stearic acid zinc；Described antiseptic is the nano-silica of grafting polymer quaternary ammonium salt
SiClx；Described Benzopyranone kind free radical scavenger is 5,7- bis--(2,2- dimethyl ethyls) -3- (3,4- dimethyl benzenes
Base) -2-3 hydrogen-benzofuranone.The ferriferous oxide is ferroso-ferric oxide and di-iron trioxide 1：The active iron oxidation of 1 mixing
Thing.
Described silane coupler is gamma-aminopropyl-triethoxy-silane (KH550) or γ-(methacryloxypropyl) propyl group
Trimethoxy silane (KH570).
Described antioxidant is four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters, N, N'- be double-
(3- (3,5- di-tert-butyl-hydroxy phenyl) propiono) hexamethylene diamine, the mixing of three [2.4- di-tert-butyl-phenyls] phosphite esters
Thing.
Described lubricant is silicone powder.
It is a further object to provide above-mentioned nylon with low smell, it is low distribute, whiteness red phosphorus flame-retardant masterbatch
Preparation method, comprises the following steps：
Microcapsule red phosphorus, hydrophobicity odor adsorption master batch, nylon, silane coupler, antioxidant and lubricant are poured into height
In fast mixer, high-speed stirred mixes into uniform rear addition double screw extruder, is granulated after melting extrusion, and low gas is obtained
Taste, it is low distribute, high abrasion-proof and high temperature resistant nylon.
The area's temperature of the double screw extruder one is 200-230 DEG C, and two area's temperature are 200-230 DEG C, and three area's temperature are
200-240 DEG C, four area's temperature are 210-240 DEG C, and five area's temperature are 210-250 DEG C, and six area's temperature are 220-250 DEG C；Twin-screw
Engine speed is 250-500rpm.
Beneficial effects of the present invention：
1. hydrophobic type odor adsorption master batch of the present invention significantly reduces phosphatization in red phosphorus flame-retardant masterbatch thermoforming process
The release of hydrogen, significantly reduces total volatile organism TVOC, is also maintained while guarantee fire-retardant master granule low odor property
Relatively low water absorption rate；The molding processibility that does not then interfere with matrix plastic is added in nylon matrix plastics as fire-retardant master granule
Energy.
Whiteness red phosphorus after 2 claddings, substantially overcomes the easy moisture absorption of red phosphorus, oxidizable problem, while in smell
The PH3 generating capacities in thermoforming process are significantly reduced under the synergy for adsorbing master batch, while also breaching in color
Limitation, product is not limited to dark product.
Specific embodiment
Below by way of the description of specific embodiment, the invention will be further described, but this is not to limit of the invention
System, those skilled in the art's basic thought of the invention, various modifications may be made or improves, but without departing from this
The basic thought of invention, within the scope of the present invention.
Specific embodiment
Below by way of the description of specific embodiment, the invention will be further described, used in embodiments below
Whiteness red phosphorus and odor adsorption master batch are prepared from by following method：
The preparation of whiteness red phosphorus：Red phosphorus 30%, aluminum sulfate 10%, urea 5%, water 50%, oil-soluble phenolic resin
5%.Aluminium hydroxide coats process：Aluminum sulfate is added to the water first, stirring is allowed to be completely dissolved, and then puts into red phosphorus, stirs
Mix 20min, then be transferred in ball mill and be ground to red phosphorus particle diameter untill 5-10um, be then transferred in reactor, side stirring
While addition caustic soda (10wt% solution) that blows slowly, untill the PH=5-6 of system, adds flocculation agent polyacrylamide, stir
Uniformly, in 75-85 DEG C of scope inside holding 1.5h, filtering is eventually passed, is washed, is dried to obtain aluminium hydroxide encapsulated red phosphorus.Phenolic aldehyde
Resin-coating process：Oil-soluble phenolic resin is diluted with 2.5-3.0 times of dimethylbenzene first, then by aluminium hydroxide encapsulated red phosphorus with oil
Dissolubility phenolic resin dilution is mixed, and stirs into pasty state homogeneous state, and feeding is controlled with the drier for reclaiming xylene unit
60 ± 5 DEG C of temperature processed is dried, and obtains final product aluminium hydroxide and the double encapsulated red phosphorus of phenolic resin.
The preparation of hydrophobic type odor adsorption master batch：6 50 parts of nylon, 15 parts of hydrophobicity diatomite, 2 parts of ferroso-ferric oxide, three
Aoxidize 2 parts of two iron, 5 parts of hydrophobic active charcoal, 10 parts of needle-like zeolite molecular sieve, 10 parts of zinc ricinate, high molecular quaternary connects
5 parts of nano silicon of branch, 5,7- bis--(2,2- dimethyl ethyl) -3- (3,4- 3,5-dimethylphenyl) -2-3 hydrogen-benzofuranone
0.1 part, antioxidant four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] 0.2 part of pentaerythritol ester, [2.4- of antioxidant three
Di-tert-butyl-phenyl] 0.2 part of phosphite ester, 0.5 part of addition high-speed mixer of zinc stearate is well mixed, then crowded in twin-screw
Go out extruding pelletization in machine and obtain hydrophobic type odor adsorption master batch.
Embodiment 1
By 40 parts of whiteness red phosphorus, 55 parts of nylon, 6,3 parts of hydrophobic type odor adsorption master batches, 0.6 part of silane coupler, 0.2
Part 1098,0.2 part of irgasfos 168 of antioxidant and 1 part of silicone powder are poured into homogenizer, high-speed stirred, are mixed to after uniform
Add in double screw extruder, granulated after melting extrusion, be obtained the low smell of nylon, it is low distribute, whiteness red phosphorus flame-retardant it is female
Grain.
Wherein the area's temperature of double screw extruder one is 200 DEG C, and two area's temperature are 210 DEG C, and three area's temperature are 220 DEG C, 4th area
Temperature is 230 DEG C, and five area's temperature are 240 DEG C, and six area's temperature are 250 DEG C；Twin-screw engine speed is 350rpm.
Embodiment 2
By 20 parts of whiteness red phosphorus, 77 parts of nylon, 6,1 part of hydrophobic type odor adsorption master batch, 0.8 part of silane coupler, 0.5
Part 1098,0.5 part of irgasfos 168 of antioxidant and 0.2 part of silicone powder are poured into homogenizer, high-speed stirred, are mixed to uniform
Afterwards add double screw extruder in, after melting extrusion granulate, be obtained nylon with low smell, it is low distribute, whiteness red phosphorus flame-retardant
Master batch.
Wherein the area's temperature of double screw extruder one is 230 DEG C, and two area's temperature are 230 DEG C, and three area's temperature are 240 DEG C, 4th area
Temperature is 240 DEG C, and five area's temperature are 250 DEG C, and six area's temperature are 250 DEG C；Twin-screw engine speed is 500rpm.
Embodiment 3
By 50 parts of whiteness red phosphorus, 43 parts of nylon, 6,5 parts of hydrophobic type odor adsorption master batches, 1 part of silane coupler, 0.2 part
1098,0.3 part of irgasfos 168 of antioxidant and 0.5 part of silicone powder are poured into homogenizer, high-speed stirred, are mixed to after uniform
Add in double screw extruder, granulated after melting extrusion, be obtained the low smell of nylon, it is low distribute, whiteness red phosphorus flame-retardant it is female
Grain.
Wherein the area's temperature of double screw extruder one is 205 DEG C, and two area's temperature are 205 DEG C, and three area's temperature are 210 DEG C, 4th area
Temperature is 215 DEG C, and five area's temperature are 220 DEG C, and six area's temperature are 225 DEG C；Twin-screw engine speed is 250rpm.
Comparative example 1
By 40 parts of untreated red phosphorus, 55 parts of nylon, 6,3 parts of hydrophobic type odor adsorption master batches, 0.6 part of silane coupler, 0.2
Part 1098,0.2 part of irgasfos 168 of antioxidant and 1 part of silicone powder are poured into homogenizer, high-speed stirred, are mixed to after uniform
Add in double screw extruder, granulated after melting extrusion, prepared nylon red phosphorus flame-retardant masterbatch.
Wherein the area's temperature of double screw extruder one is 200 DEG C, and two area's temperature are 210 DEG C, and three area's temperature are 220 DEG C, 4th area
Temperature is 230 DEG C, and five area's temperature are 240 DEG C, and six area's temperature are 250 DEG C；Twin-screw engine speed is 350rpm.
Comparative example 2
By 40 parts of untreated red phosphorus, 58 parts of nylon, 6,0.6 part of silane coupler, 0.2 part of antioxidant, 1098,0.2 part of antioxygen
Agent 168 and 1 part of silicone powder are poured into homogenizer, high-speed stirred, are mixed into uniform rear addition double screw extruder, through molten
Granulated after melting extrusion, prepared nylon red phosphorus flame-retardant masterbatch.
Wherein the area's temperature of double screw extruder one is 200 DEG C, and two area's temperature are 210 DEG C, and three area's temperature are 220 DEG C, 4th area
Temperature is 230 DEG C, and five area's temperature are 240 DEG C, and six area's temperature are 250 DEG C；Twin-screw engine speed is 350rpm.
According to the effective flame retardance element of equivalent of embodiment 1, by the nylon made by above-described embodiment 1-3 with low smell, low dissipate
Hair, whiteness red phosphorus flame-retardant masterbatch are respectively applied in PA6, and embodiment 4-6 is obtained.It is effective fire-retardant group according to the equivalent of embodiment 1
Point, the nylon red phosphorus flame-retardant masterbatch made by comparative example 1-2 is respectively applied in PA6, comparative example 3-4 is obtained.According to reality
The effective flame retardance element of equivalent of example 1 is applied, the untreated red phosphorus of equivalent is applied to comparative example 5 is obtained in PA6.Material modified proportioning
And performance is as shown in the table, wherein mechanical property is detected using ASTM standard, and oder levels, TVOC are entered using GMW standards
Row detection, fire resistance is determined according to UL94 standards.
The performance data of table 1
Can be seen by upper table 1, after nylon red phosphorus flame-retardant masterbatch prepared by the present invention mixes with nylon-6 matrix body, its is fire-retardant
Performance can reach UL94V-0 grades, and oder levels reach 6.5 grades, and tensile strength, the impact strength of material have due to not
Treatment red phosphorus institute prepared material, improves the comprehensive mechanical property and processing characteristics of fire proofing to a certain extent.
In addition, using nylon red phosphorus flame-retardant masterbatch of the invention dust pollution can be reduced, improve environmental protection and to human body without
Evil；And compatibility is good between resin matrix, the physical and chemical performance of modified resin is also correspondingly improve.
The description of above specific embodiment is that the invention will be further described, but this is not to limit of the invention
System, those skilled in the art's basic thought of the invention, various modifications may be made or improves, but without departing from this
The basic thought of invention, within the scope of the present invention.
Claims (10)
1. a kind of whiteness red phosphorus, described whiteness red phosphorus is microcapsule red phosphorus, and described microcapsule red phosphorus are aluminium hydroxide
With the double encapsulated red phosphorus of phenolic resin, the preparation of the microcapsule red phosphorus：It is made of the raw material including following weight proportion：Red phosphorus
25-35%, aluminum sulfate 5-15%, urea 10-15%, water 50-59%, oil-soluble phenolic resin resin 1-5%；Hydroxide
Aluminium coats process：Aluminum sulfate is added to the water first, stirring is allowed to be completely dissolved, and then puts into red phosphorus, stirs 20min, then
It is transferred in ball mill and is ground to red phosphorus particle diameter untill 5-10um, be then transferred in reactor, adds slowly while stirring
Caustic soda, untill the PH=5-6 of system, adds flocculation agent, stirs, in 75-85 DEG C of scope inside holding 1.5h, finally
By filtering, washing, being dried to obtain aluminium hydroxide encapsulated red phosphorus；Phenolic resin coats process：First with 2.5-3.0 times the two of volume
Toluene dilutes oil-soluble phenolic resin, then aluminium hydroxide encapsulated red phosphorus are mixed with oil-soluble phenolic resin dilution,
Pasty state homogeneous state is stirred into, with the drier for reclaiming xylene unit, 60 ± 5 DEG C of temperature of control is dried feeding, obtains final product
Aluminium hydroxide and the double encapsulated red phosphorus of phenolic resin.
2. a kind of nylon with low smell, it is low distribute, whiteness red phosphorus flame-retardant masterbatch, it is characterised in that：By following components by by weight
Amount part is prepared from：
20-50 parts of whiteness red phosphorus described in claim 1,
45-80 parts of nylon 6
1-5 parts of hydrophobic type odor adsorption master batch,
Silane coupler 0.5-1 parts
0.2~1.0 part of antioxidant
0.2~1.0 part of lubricant.
3. a kind of nylon according to claim 2 with low smell, it is low distribute, whiteness red phosphorus flame-retardant masterbatch, its feature exists
In：Described whiteness red phosphorus is microcapsule red phosphorus, described microcapsule red phosphorus for aluminium hydroxide and phenolic resin double-contracting cover it is red
Phosphorus.
4. a kind of nylon according to claim 2 with low smell, it is low distribute, whiteness red phosphorus flame-retardant masterbatch, its feature exists
In：The described inherent viscosity of nylon 6 is 2.0-3.6.
5. a kind of nylon according to claim 2 with low smell, it is low distribute, whiteness red phosphorus flame-retardant masterbatch, its feature exists
In：Described hydrophobic type odor adsorption master batch is made up of the component of following weight portion：40~75 parts of PA6, hydrophobicity diatomite 10
~20 parts, 1~5 part of ferriferous oxide, 0~10 part of hydrophobic active charcoal, 5~10 parts of needle-like zeolite molecular sieve, zinc ricinate 5~
10 parts, 5~10 parts of antiseptic, 0.1-0.5 parts of Benzopyranone kind free radical scavenger, antioxidant four [β-（3,5- bis- tertiary fourths
Base -4- hydroxy phenyls）Propionic acid] pentaerythritol ester 0.2-0.5 parts, antioxidant three [2.4- di-tert-butyl-phenyls] phosphite ester
0.2-0.5 parts, 0.5-1.0 parts of lubricant stearic acid zinc；Described antiseptic is the nanometer titanium dioxide of grafting polymer quaternary ammonium salt
Silicon；Described Benzopyranone kind free radical scavenger is 5,7- bis--(2,2- dimethyl ethyls) -3- (3,4- dimethyl benzenes
Base) -2-3 hydrogen-benzofuranone, the ferriferous oxide is ferroso-ferric oxide and di-iron trioxide by weight 1：The work of 1 mixing
Property ferriferous oxide.
6. a kind of nylon according to right 2 with low smell, it is low distribute, whiteness red phosphorus flame-retardant masterbatch, it is characterised in that：Institute
The silane coupler stated be gamma-aminopropyl-triethoxy-silane or γ-（Methacryloxypropyl）Propyl trimethoxy silicane.
7. a kind of low smell according to claim 2, low distribute modified red phosphorus flame-retardant nylon material, it is characterised in that：Institute
The antioxidant stated be four [β-（3,5- di-tert-butyl-hydroxy phenyls）Propionic acid] pentaerythritol ester, N, N'- pair-(3- (3,5- bis-
Tert-butyl-hydroxy phenyl) propiono) hexamethylene diamine, the mixture of three [2.4- di-tert-butyl-phenyls] phosphite esters.
8. a kind of low smell according to claim 2, low distribute modified red phosphorus flame-retardant nylon material, it is characterised in that：Institute
The lubricant stated is silicone powder.
9. a kind of nylon according to claim any one of 1-8 with low smell, it is low distribute, whiteness red phosphorus flame-retardant masterbatch
Preparation method, it is characterised in that comprise the following steps：
Whiteness red phosphorus, hydrophobicity odor adsorption master batch, nylon 6, silane coupler, antioxidant and lubricant are poured into high-speed stirring
In mixing machine, high-speed stirred mixes into adding double screw extruder after uniform, is granulated after melting extrusion, and low smell, low is obtained
Distribute, high abrasion-proof and high temperature resistant nylon.
10. preparation method according to claim 9, it is characterised in that：The area's temperature of the double screw extruder one is 200-
230 DEG C, two area's temperature are 200-230 DEG C, and three area's temperature are 200-240 DEG C, and four area's temperature are 210-240 DEG C, and five area's temperature are
210-250 DEG C, six area's temperature are 220-250 DEG C；Twin-screw engine speed is 250-500rpm.
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| CN107974257A (en) * | 2017-10-24 | 2018-05-01 | 什邡市太丰新型阻燃剂有限责任公司 | High whiteness red phosphorus of a kind of flame retarding efficiency and preparation method thereof |
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| CN110499671A (en) * | 2019-08-19 | 2019-11-26 | 四川金路高新材料有限公司 | A kind of preparation method of fire resistance fibre wallpaper |
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| CN114410056B (en) * | 2022-01-11 | 2024-03-01 | 宁波帅特龙集团有限公司 | Flame-retardant ABS composite material and preparation method thereof |
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