CN112760982A - High-flame-retardant antistatic yarn and processing method thereof - Google Patents
High-flame-retardant antistatic yarn and processing method thereof Download PDFInfo
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- CN112760982A CN112760982A CN202011579755.3A CN202011579755A CN112760982A CN 112760982 A CN112760982 A CN 112760982A CN 202011579755 A CN202011579755 A CN 202011579755A CN 112760982 A CN112760982 A CN 112760982A
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- flame
- solution
- retardant
- antistatic
- temperature
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 92
- 238000003672 processing method Methods 0.000 title claims abstract description 8
- 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 claims abstract description 76
- 239000000835 fiber Substances 0.000 claims abstract description 47
- 239000002216 antistatic agent Substances 0.000 claims abstract description 35
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000009987 spinning Methods 0.000 claims abstract description 26
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 23
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 23
- 229920000742 Cotton Polymers 0.000 claims abstract description 22
- 229920000728 polyester Polymers 0.000 claims abstract description 22
- 210000002268 wool Anatomy 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 20
- AXKZIDYFAMKWSA-UHFFFAOYSA-N 1,6-dioxacyclododecane-7,12-dione Chemical compound O=C1CCCCC(=O)OCCCCO1 AXKZIDYFAMKWSA-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 238000001291 vacuum drying Methods 0.000 claims abstract description 13
- 238000002074 melt spinning Methods 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000004804 winding Methods 0.000 claims abstract description 8
- WNLRTRBMVRJNCN-UHFFFAOYSA-L adipate(2-) Chemical compound [O-]C(=O)CCCCC([O-])=O WNLRTRBMVRJNCN-UHFFFAOYSA-L 0.000 claims abstract description 6
- -1 polybutylene terephthalate Polymers 0.000 claims abstract description 6
- 229920001707 polybutylene terephthalate Polymers 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 86
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 60
- 238000003756 stirring Methods 0.000 claims description 35
- VHYFNPMBLIVWCW-UHFFFAOYSA-N 4-Dimethylaminopyridine Chemical compound CN(C)C1=CC=NC=C1 VHYFNPMBLIVWCW-UHFFFAOYSA-N 0.000 claims description 34
- 239000012752 auxiliary agent Substances 0.000 claims description 33
- 238000006243 chemical reaction Methods 0.000 claims description 32
- 239000000306 component Substances 0.000 claims description 32
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 30
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 30
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 20
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 claims description 20
- 239000011259 mixed solution Substances 0.000 claims description 20
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 19
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- SUBJHSREKVAVAR-UHFFFAOYSA-N sodium;methanol;methanolate Chemical compound [Na+].OC.[O-]C SUBJHSREKVAVAR-UHFFFAOYSA-N 0.000 claims description 15
- 239000003153 chemical reaction reagent Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- YAYNEUUHHLGGAH-UHFFFAOYSA-N 1-chlorododecane Chemical compound CCCCCCCCCCCCCl YAYNEUUHHLGGAH-UHFFFAOYSA-N 0.000 claims description 12
- BSYJHYLAMMJNRC-UHFFFAOYSA-N 2,4,4-trimethylpentan-2-ol Chemical compound CC(C)(C)CC(C)(C)O BSYJHYLAMMJNRC-UHFFFAOYSA-N 0.000 claims description 12
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- QOSSAOTZNIDXMA-UHFFFAOYSA-N Dicylcohexylcarbodiimide Chemical group C1CCCCC1N=C=NC1CCCCC1 QOSSAOTZNIDXMA-UHFFFAOYSA-N 0.000 claims description 10
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 claims description 10
- 238000004821 distillation Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 238000010992 reflux Methods 0.000 claims description 10
- FALRKNHUBBKYCC-UHFFFAOYSA-N 2-(chloromethyl)pyridine-3-carbonitrile Chemical compound ClCC1=NC=CC=C1C#N FALRKNHUBBKYCC-UHFFFAOYSA-N 0.000 claims description 9
- 229940014800 succinic anhydride Drugs 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000002270 dispersing agent Substances 0.000 claims description 7
- 230000000149 penetrating effect Effects 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 7
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical class [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 5
- 150000008064 anhydrides Chemical class 0.000 claims description 5
- 239000012295 chemical reaction liquid Substances 0.000 claims description 5
- 238000002425 crystallisation Methods 0.000 claims description 5
- 230000008025 crystallization Effects 0.000 claims description 5
- 239000012065 filter cake Substances 0.000 claims description 5
- 239000012530 fluid Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000012074 organic phase Substances 0.000 claims description 5
- 238000003828 vacuum filtration Methods 0.000 claims description 5
- 229940043237 diethanolamine Drugs 0.000 description 22
- 230000003068 static effect Effects 0.000 description 7
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 230000005611 electricity Effects 0.000 description 5
- 239000000654 additive Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 238000007259 addition reaction Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 229920000587 hyperbranched polymer Polymers 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 238000012805 post-processing Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 201000004624 Dermatitis Diseases 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000011514 reflex Effects 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Classifications
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/507—Polyesters
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
- D02G3/04—Blended or other yarns or threads containing components made from different materials
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/44—Yarns or threads characterised by the purpose for which they are designed
- D02G3/441—Yarns or threads with antistatic, conductive or radiation-shielding properties
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/44—Yarns or threads characterised by the purpose for which they are designed
- D02G3/443—Heat-resistant, fireproof or flame-retardant yarns or threads
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/10—Animal fibres
- D06M2101/12—Keratin fibres or silk
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/30—Flame or heat resistance, fire retardancy properties
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2201/00—Cellulose-based fibres, e.g. vegetable fibres
- D10B2201/01—Natural vegetable fibres
- D10B2201/02—Cotton
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2211/00—Protein-based fibres, e.g. animal fibres
- D10B2211/01—Natural animal fibres, e.g. keratin fibres
- D10B2211/02—Wool
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
- D10B2331/04—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyesters, e.g. polyethylene terephthalate [PET]
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2401/00—Physical properties
- D10B2401/13—Physical properties anti-allergenic or anti-bacterial
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2401/00—Physical properties
- D10B2401/16—Physical properties antistatic; conductive
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a high flame-retardant antistatic yarn and a processing method thereof, wherein the yarn comprises the following raw materials in parts by weight: 100-160 parts of polybutylene terephthalate/adipate, 1-3 parts of polyethylene glycol, 0.6-1 part of antistatic agent, 3-5 parts of flame retardant, 70-90 parts of wool fiber and 70-90 parts of cotton fiber; the processing method comprises the following steps: respectively carrying out vacuum drying on the poly (terephthalic acid)/butylene adipate and the polyethylene glycol, blending the poly (terephthalic acid)/butylene adipate and the polyethylene glycol with the antistatic agent and the flame retardant after drying treatment, carrying out melt spinning by a screw type spinning machine at the temperature of 250-290 ℃ and the spinning speed of 800-1200r/min, cooling, oiling, pre-drafting and winding to obtain polyester fiber; and secondly, performing flame retardant treatment on the wool fibers and the cotton fibers, twisting the wool fibers and the cotton fibers into a thread, and then performing a spinning process on the thread and the polyester fibers to obtain the high-flame-retardant antistatic yarn.
Description
Technical Field
The invention belongs to the technical field of spinning, and particularly relates to a high-flame-retardant antistatic yarn and a processing method thereof.
Background
The conventional textile fibers, especially the chemical fibers, are mostly combustible or inflammable materials and have high insulating property. In consideration of these two defects, both durability and comfort of the garment are considered to ensure the safety of workers involved in dangerous fields such as mining, fire fighting, and military industry. When people wear the clothes, people have a trouble that static electricity is easily generated, and the use of people is influenced.
The polyester fiber is difficult to bundle and wound on a machine part due to static electricity generated by friction during post processing; the finished product is easy to stain and absorb dust; when the shoe is worn, a human body has uncomfortable feeling due to electrostatic phenomenon, and particularly under a low relative humidity environment, the human body has electric shock feeling, stimulates nerves of the human body, generates adverse physiological reaction, and can cause skin inflammation and blood pH value increase locally; when electronic equipment is operated, static electricity generated by friction interferes with precise electronic equipment and electronic components, causes misoperation and component damage of the equipment and even whole circuit failure, and limits the application of polyester fiber in many fields.
Disclosure of Invention
In order to overcome the technical problems, the invention provides a high flame-retardant antistatic yarn and a processing method thereof.
The technical problems to be solved by the invention are as follows:
the chemical fiber not only belongs to combustible or inflammable materials, but also is difficult to bundle and wound on a machine part due to static electricity generated by friction during post processing; the finished product is easy to stain and absorb dust; the static electricity makes the human body feel uncomfortable when wearing the clothes.
The purpose of the invention can be realized by the following technical scheme:
the high-flame-retardant antistatic yarn comprises the following raw materials in parts by weight:
160 parts of polybutylene terephthalate/adipate, 1-3 parts of polyethylene glycol, 0.6-1 part of antistatic agent, 3-5 parts of flame retardant, 70-90 parts of wool fiber, 70-90 parts of cotton fiber and 200 parts of flame retardant treatment fluid;
the high flame-retardant antistatic yarn is processed by the following steps:
respectively carrying out vacuum drying on the poly (terephthalic acid)/butylene adipate and the polyethylene glycol to ensure that the water content is less than 200ppm, blending the poly (terephthalic acid)/butylene adipate and the polyethylene glycol with an antistatic agent and a flame retardant after drying treatment, carrying out melt spinning on the poly (terephthalic acid)/butylene adipate and the polyethylene glycol by a screw type spinning machine at the conditions of 290 ℃ of temperature plus 250 ℃ and 1200r/min of spinning speed, cooling, and carrying out oiling, pre-drafting and 800m/min of winding treatment of 700 plus 700) to obtain polyester fibers;
and secondly, soaking and drying wool fibers and cotton fibers in flame-retardant treatment liquid, twisting the wool fibers and the cotton fibers into a thread, and then spinning the thread and polyester fibers to prepare the high-flame-retardant antistatic yarn, wherein the flame-retardant treatment liquid is a flame retardant FPK8002, a WA dispersant, a penetrating agent JFC and deionized water according to a mass ratio of 8: 0.7: 0.3: 91 by mixing.
A spinning process: b412 sliver mixing-B423 head needle-B432 two needles-B442 three needles-B452 four needles-FB 441 roving one-FB 441 roving two-spun yarn-automatic spooling-doubling-double twisting-yarn steaming.
Further, the antistatic agent is prepared by the following steps:
adding an antistatic component and dichloromethane into a round-bottom flask, adding a reagent and an auxiliary agent under the conditions of-20 ℃ and 400r/min of rotation speed, keeping the rotation speed unchanged at 25 ℃ and continuing stirring for 12 hours, extracting with saturated ammonium chloride and dichloromethane after the reaction is finished, and concentrating an organic phase at 30 ℃ under reduced pressure by using a rotary evaporator to obtain the antistatic agent.
Further, the reagent is N, N' -dicyclohexylcarbodiimide, 4-dimethylaminopyridine and dichloromethane in a dosage ratio of 11 mmol: 3 mmol: 5mL, and the dosage ratio of the antistatic component, dichloromethane, reagent and auxiliary agent is 5 g: 10mL of: 0.5-0.7 g: 1g of the total weight of the composition.
Further, the antistatic component is prepared by the following steps:
step S11, adding chlorododecane and absolute ethyl alcohol into a three-neck flask, setting the temperature to be 70-80 ℃ and the rotating speed to be 400r/min, dropwise adding a diethanolamine solution while stirring, then adding sodium hydroxide, keeping the temperature unchanged, carrying out reflux reaction for 4-5h, and after the reaction is finished, carrying out reduced pressure distillation on the obtained reaction liquid to remove the absolute ethyl alcohol to obtain an intermediate A;
step S12, mixing diethanolamine and N, N-dimethylacetamide according to the dosage ratio of 12-13 g: 10mL of the mixture is mixed to obtain a solution a, and succinic anhydride and N, N-dimethylacetamide are mixed according to the dosage ratio of 12 g: 10mL of the solution a is mixed to obtain a solution B, the solution a is added into a three-neck flask, the solution B with the same volume is dripped under the conditions that the temperature is 30 ℃ and the rotating speed is 400r/min, the dripping time is 1h, and after the dripping is finished, the solution B is stirred and mixed for 3h under the condition of 26 ℃ to obtain a mixed solution B;
and S13, adding the intermediate A into the mixed solution B, then adding toluene and p-toluenesulfonic acid, setting the temperature at 110 ℃ and the rotating speed at 400r/min, heating and refluxing for 1-3h, after the reaction is finished, concentrating under reduced pressure at 60 ℃ in a rotary evaporator until the volume is unchanged to obtain a concentrated solution, adding the obtained concentrated solution into N, N-dimethylacetamide, then adding 4-dimethylaminopyridine, setting the temperature at 80 ℃ and the rotating speed at 400r/min, dropwise adding the solution B prepared in the step S12 while stirring, keeping the temperature and the rotating speed unchanged after dropwise adding, and continuously stirring for 6h to obtain the antistatic component.
Taking chlorododecane as a core, carrying out hyperbranched reaction on a monomer synthesized by diethanol amine and succinic anhydride through esterification reaction, and then reacting partial hydroxyl at the tail end with succinic anhydride under the catalysis of 4-dimethylamino pyridine to introduce carboxyl so as to prepare the antistatic component. The antistatic component is a hyperbranched polymer, has a three-dimensional structure, is high in branching degree and good in stability and dispersibility, a branched chain of the antistatic component contains a large number of hydrophilic groups such as hydroxyl groups, carboxyl groups and the like, and the hydrophilic groups in the prepared antistatic agent can counteract static charges generated by friction in polyester fibers to play an antistatic role; the carboxyl on the branched chain in the antistatic component and the amino in the auxiliary agent are condensed, and the auxiliary agent is introduced into the molecular chain of the antistatic component, so that the flame retardance of the antistatic agent is endowed.
Further, in the step S11, the diethanolamine solution is diethanolamine and absolute ethanol according to a dosage ratio of 1 g: 5mL, and the dosage ratio of the chlorododecane, the absolute ethyl alcohol, the diethanolamine solution and the sodium hydroxide is 4 g: 50mL of: 10mL of: 0.8-1 g; in the step S13, the dosage ratio of the intermediate A, the mixed liquid B, the toluene and the p-toluenesulfonic acid is 5 g: 20mL of: 50mL of: 0.1 g; the dosage ratio of the concentrated solution, the N, N-dimethylacetamide, the 4-dimethylaminopyridine and the solution b is 40 mL: 80mL of: 0.6-0.8 g: 2-4 mL.
Further, the flame retardant is prepared by the following steps:
adding an auxiliary agent, dioxane and triethylamine into a three-neck flask, setting the temperature at 45 ℃ and the rotating speed at 400r/min, dropwise adding cyanuric chloride mixed solution while stirring, controlling the dropwise adding speed at 1-3 drops/second, keeping the temperature and the rotating speed unchanged after dropwise adding, continuously stirring for 4 hours, and removing dioxane by reduced pressure distillation to obtain the flame retardant; wherein the cyanuric chloride mixed solution is cyanuric chloride and dioxane in a mass ratio of 1: 7, the mass ratio of the auxiliary agent, dioxane, triethylamine and cyanuric chloride is 20: 50: 12: 80.
the additive is prepared by the addition reaction of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and acrylamide, the prepared additive participates in the synthesis of the antistatic agent and the synthesis of the flame retardant, and the synthesized flame retardant has good thermal stability.
Further, the auxiliary agent is prepared by the following steps:
adding 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, dioxane and acrylamide into a three-neck flask, setting the temperature at 40 ℃ and the rotating speed at 300r/min, dropwise adding a sodium methoxide methanol solution under the condition of nitrogen protection, after dropwise adding, heating the temperature to 80 ℃, keeping the rotating speed unchanged, continuing stirring for reaction for 5 hours, after the reaction is finished, cooling for crystallization, carrying out vacuum filtration, and drying the obtained filter cake at 40 ℃ to constant weight to obtain an auxiliary agent; wherein the sodium methoxide methanol solution is prepared from sodium methoxide and methanol according to the dosage ratio of 3-5 g: 10mL, and the dosage ratio of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, dioxane, acrylamide and sodium methoxide methanol solution is 0.2 mol: 20mL of: 0.2 mol: 5g of the total weight.
A processing method of high flame-retardant antistatic yarn comprises the following steps:
respectively carrying out vacuum drying on the poly (terephthalic acid)/butylene adipate and the polyethylene glycol to ensure that the water content is less than 200ppm, blending the poly (terephthalic acid)/butylene adipate and the polyethylene glycol with an antistatic agent and a flame retardant after drying treatment, carrying out melt spinning on the poly (terephthalic acid)/butylene adipate and the polyethylene glycol by a screw type spinning machine at the conditions of 290 ℃ of temperature plus 250 ℃ and 1200r/min of spinning speed, cooling, and carrying out oiling, pre-drafting and 800m/min of winding treatment of 700 plus 700) to obtain polyester fibers;
and secondly, soaking and drying wool fibers and cotton fibers in flame-retardant treatment liquid, twisting the wool fibers and the cotton fibers into a thread, and then spinning the thread and polyester fibers to prepare the high-flame-retardant antistatic yarn, wherein the flame-retardant treatment liquid is a flame retardant FPK8002, a WA dispersant, a penetrating agent JFC and deionized water according to a mass ratio of 8: 0.7: 0.3: 91 by mixing.
The invention has the beneficial effects that:
taking chlorododecane as a core, carrying out hyperbranched reaction on a monomer synthesized by diethanol amine and succinic anhydride through esterification reaction, and then reacting partial hydroxyl at the tail end with succinic anhydride under the catalysis of 4-dimethylamino pyridine to introduce carboxyl so as to prepare the antistatic component. The antistatic component is a hyperbranched polymer, has a three-dimensional structure, is high in branching degree and good in stability and dispersibility, a branched chain of the antistatic component contains a large number of hydrophilic groups such as hydroxyl groups, carboxyl groups and the like, and the hydrophilic groups in the prepared antistatic agent can counteract static charges generated by friction in polyester fibers to play an antistatic role; the carboxyl on the branched chain in the antistatic component and the amino in the auxiliary agent are condensed, and the auxiliary agent is introduced into the molecular chain of the antistatic component, so that the flame retardance of the antistatic agent is endowed.
The additive is prepared by the addition reaction of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and acrylamide, the prepared additive participates in the synthesis of the antistatic agent and the synthesis of the flame retardant, and the synthesized flame retardant has good thermal stability. The antistatic agent and the flame retardant are added into the synthetic polyester fiber, and the antistatic agent has an aliphatic hydrocarbon structure and good compatibility with the polyester fiber, so that the antistatic agent is better dispersed to play an antistatic role.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The high-flame-retardant antistatic yarn comprises the following raw materials in parts by weight:
100 parts of polybutylene terephthalate/adipate, 1 part of polyethylene glycol, 0.6 part of antistatic agent, 3 parts of flame retardant, 70 parts of wool fiber, 70 parts of cotton fiber and 100 parts of flame-retardant treatment fluid;
the high flame-retardant antistatic yarn is processed by the following steps:
respectively carrying out vacuum drying on poly (terephthalic acid)/butylene adipate and polyethylene glycol to ensure that the water content is less than 200ppm, blending with an antistatic agent and a flame retardant after drying treatment, carrying out melt spinning through a screw type spinning machine at the temperature of 250 ℃ and the spinning speed of 800r/min, cooling, oiling, pre-drafting and winding at the speed of 700m/min to obtain polyester fibers;
and secondly, soaking and drying wool fibers and cotton fibers in flame-retardant treatment liquid, twisting the wool fibers and the cotton fibers into a thread, and then spinning the thread and polyester fibers to prepare the high-flame-retardant antistatic yarn, wherein the flame-retardant treatment liquid is a flame retardant FPK8002, a WA dispersant, a penetrating agent JFC and deionized water according to a mass ratio of 8: 0.7: 0.3: 91 by mixing.
Wherein the antistatic agent is prepared by the following steps:
adding an antistatic component and dichloromethane into a round-bottom flask, adding a reagent and an auxiliary agent under the conditions of-20 ℃ and 400r/min of rotation speed, keeping the rotation speed unchanged at 25 ℃ and continuing stirring for 12 hours, extracting with saturated ammonium chloride and dichloromethane after the reaction is finished, and concentrating an organic phase at 30 ℃ under reduced pressure by using a rotary evaporator to obtain the antistatic agent.
Wherein the reagent is N, N' -dicyclohexylcarbodiimide, 4-dimethylaminopyridine and dichloromethane according to the dosage ratio of 11 mmol: 3 mmol: 5mL, and the dosage ratio of the antistatic component, dichloromethane, reagent and auxiliary agent is 5 g: 10mL of: 0.5 g: 1g of the total weight of the composition.
Wherein the antistatic component is prepared by the following steps:
step S11, adding chlorododecane and absolute ethyl alcohol into a three-neck flask, setting the temperature to be 70 ℃ and the rotating speed to be 400r/min, dropwise adding a diethanolamine solution while stirring, then adding sodium hydroxide, keeping the temperature unchanged, carrying out reflux reaction for 4 hours, and after the reaction is finished, carrying out reduced pressure distillation on the obtained reaction liquid to remove the absolute ethyl alcohol to obtain an intermediate A;
step S12, mixing diethanolamine and N, N-dimethylacetamide according to the dosage ratio of 12 g: 10mL of the mixture is mixed to obtain a solution a, and succinic anhydride and N, N-dimethylacetamide are mixed according to the dosage ratio of 12 g: 10mL of the solution a is mixed to obtain a solution B, the solution a is added into a three-neck flask, the solution B with the same volume is dripped under the conditions that the temperature is 30 ℃ and the rotating speed is 400r/min, the dripping time is 1h, and after the dripping is finished, the solution B is stirred and mixed for 3h under the condition of 26 ℃ to obtain a mixed solution B;
and S13, adding the intermediate A into the mixed solution B, adding toluene and p-toluenesulfonic acid, setting the temperature at 110 ℃ and the rotating speed at 400r/min, heating and refluxing for 1h, after the reaction is finished, concentrating under reduced pressure at 60 ℃ in a rotary evaporator until the volume is unchanged to obtain a concentrated solution, adding the obtained concentrated solution into N, N-dimethylacetamide, adding 4-dimethylaminopyridine, setting the temperature at 80 ℃ and the rotating speed at 400r/min, dropwise adding the solution B prepared in the step S12 while stirring, keeping the temperature and the rotating speed unchanged after dropwise adding, and continuously stirring for 6h to obtain the antistatic component.
Wherein the diethanolamine solution in the step S11 is diethanolamine and absolute ethyl alcohol according to the dosage ratio of 1 g: 5mL, and the dosage ratio of the chlorododecane, the absolute ethyl alcohol, the diethanolamine solution and the sodium hydroxide is 4 g: 50mL of: 10mL of: 0.8 g; in the step S13, the dosage ratio of the intermediate A, the mixed liquid B, the toluene and the p-toluenesulfonic acid is 5 g: 20mL of: 50mL of: 0.1 g; the dosage ratio of the concentrated solution, the N, N-dimethylacetamide, the 4-dimethylaminopyridine and the solution b is 40 mL: 80mL of: 0.6 g: 2 mL.
Wherein, the flame retardant is prepared by the following steps:
adding an auxiliary agent, dioxane and triethylamine into a three-neck flask, setting the temperature at 45 ℃ and the rotating speed at 400r/min, dropwise adding cyanuric chloride mixed solution while stirring, controlling the dropwise adding speed at 1 drop/second, keeping the temperature and the rotating speed unchanged after dropwise adding, continuously stirring for 4 hours, and removing dioxane by reduced pressure distillation to obtain the flame retardant; wherein the cyanuric chloride mixed solution is cyanuric chloride and dioxane in a mass ratio of 1: 7, the mass ratio of the auxiliary agent, dioxane, triethylamine and cyanuric chloride is 20: 50: 12: 80.
the auxiliary agent is prepared by the following steps:
adding 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, dioxane and acrylamide into a three-neck flask, setting the temperature at 40 ℃ and the rotating speed at 300r/min, dropwise adding a sodium methoxide methanol solution under the condition of nitrogen protection, after dropwise adding, heating the temperature to 80 ℃, keeping the rotating speed unchanged, continuing stirring for reaction for 5 hours, after the reaction is finished, cooling for crystallization, carrying out vacuum filtration, and drying the obtained filter cake at 40 ℃ to constant weight to obtain an auxiliary agent; wherein the sodium methoxide methanol solution is prepared from sodium methoxide and methanol according to the dosage ratio of 3 g: 10mL, and the dosage ratio of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, dioxane, acrylamide and sodium methoxide methanol solution is 0.2 mol: 20mL of: 0.2 mol: 5g of the total weight.
Example 2
The high-flame-retardant antistatic yarn comprises the following raw materials in parts by weight:
130 parts of polybutylene terephthalate/adipate, 2 parts of polyethylene glycol, 0.8 part of antistatic agent, 4 parts of flame retardant, 80 parts of wool fiber, 80 parts of cotton fiber and 150 parts of flame retardant treatment fluid;
the high flame-retardant antistatic yarn is processed by the following steps:
respectively carrying out vacuum drying on poly (terephthalic acid)/butylene adipate and polyethylene glycol to ensure that the water content is less than 200ppm, blending with an antistatic agent and a flame retardant after drying treatment, carrying out melt spinning at the spinning speed of 1000r/min at 270 ℃ by a screw type spinning machine, cooling, oiling, pre-drafting and winding at 750m/min to obtain polyester fibers;
and secondly, soaking and drying wool fibers and cotton fibers in flame-retardant treatment liquid, twisting the wool fibers and the cotton fibers into a thread, and then spinning the thread and polyester fibers to prepare the high-flame-retardant antistatic yarn, wherein the flame-retardant treatment liquid is a flame retardant FPK8002, a WA dispersant, a penetrating agent JFC and deionized water according to a mass ratio of 8: 0.7: 0.3: 91 by mixing.
Wherein the antistatic agent is prepared by the following steps:
adding an antistatic component and dichloromethane into a round-bottom flask, adding a reagent and an auxiliary agent under the conditions of-20 ℃ and 400r/min of rotation speed, keeping the rotation speed unchanged at 25 ℃ and continuing stirring for 12 hours, extracting with saturated ammonium chloride and dichloromethane after the reaction is finished, and concentrating an organic phase at 30 ℃ under reduced pressure by using a rotary evaporator to obtain the antistatic agent.
Wherein the reagent is N, N' -dicyclohexylcarbodiimide, 4-dimethylaminopyridine and dichloromethane according to the dosage ratio of 11 mmol: 3 mmol: 5mL, and the dosage ratio of the antistatic component, dichloromethane, reagent and auxiliary agent is 5 g: 10mL of: 0.6 g: 1g of the total weight of the composition.
Wherein the antistatic component is prepared by the following steps:
step S11, adding chlorododecane and absolute ethyl alcohol into a three-neck flask, setting the temperature to be 75 ℃ and the rotating speed to be 400r/min, dropwise adding a diethanolamine solution while stirring, then adding sodium hydroxide, keeping the temperature unchanged, carrying out reflux reaction for 4.5 hours, and after the reaction is finished, carrying out reduced pressure distillation on the obtained reaction liquid to remove the absolute ethyl alcohol to obtain an intermediate A;
step S12, mixing diethanolamine and N, N-dimethylacetamide according to the dosage ratio of 12.5 g: 10mL of the mixture is mixed to obtain a solution a, and succinic anhydride and N, N-dimethylacetamide are mixed according to the dosage ratio of 12 g: 10mL of the solution a is mixed to obtain a solution B, the solution a is added into a three-neck flask, the solution B with the same volume is dripped under the conditions that the temperature is 30 ℃ and the rotating speed is 400r/min, the dripping time is 1h, and after the dripping is finished, the solution B is stirred and mixed for 3h under the condition of 26 ℃ to obtain a mixed solution B;
and S13, adding the intermediate A into the mixed solution B, then adding toluene and p-toluenesulfonic acid, setting the temperature at 110 ℃ and the rotating speed at 400r/min, heating and refluxing for 1-3h, after the reaction is finished, concentrating under reduced pressure at 60 ℃ in a rotary evaporator until the volume is unchanged to obtain a concentrated solution, adding the obtained concentrated solution into N, N-dimethylacetamide, then adding 4-dimethylaminopyridine, setting the temperature at 80 ℃ and the rotating speed at 400r/min, dropwise adding the solution B prepared in the step S12 while stirring, keeping the temperature and the rotating speed unchanged after dropwise adding, and continuously stirring for 6h to obtain the antistatic component.
Wherein the diethanolamine solution in the step S11 is diethanolamine and absolute ethyl alcohol according to the dosage ratio of 1 g: 5mL, and the dosage ratio of the chlorododecane, the absolute ethyl alcohol, the diethanolamine solution and the sodium hydroxide is 4 g: 50mL of: 10mL of: 0.9 g; in the step S13, the dosage ratio of the intermediate A, the mixed liquid B, the toluene and the p-toluenesulfonic acid is 5 g: 20mL of: 50mL of: 0.1 g; the dosage ratio of the concentrated solution, the N, N-dimethylacetamide, the 4-dimethylaminopyridine and the solution b is 40 mL: 80mL of: 0.7 g: 3 mL.
Wherein, the flame retardant is prepared by the following steps:
adding an auxiliary agent, dioxane and triethylamine into a three-neck flask, setting the temperature at 45 ℃ and the rotating speed at 400r/min, dropwise adding cyanuric chloride mixed solution while stirring, controlling the dropwise adding speed at 2 drops/second, keeping the temperature and the rotating speed unchanged after dropwise adding, continuously stirring for 4 hours, and removing dioxane by reduced pressure distillation to obtain the flame retardant; wherein the cyanuric chloride mixed solution is cyanuric chloride and dioxane in a mass ratio of 1: 7, the mass ratio of the auxiliary agent, dioxane, triethylamine and cyanuric chloride is 20: 50: 12: 80.
the auxiliary agent is prepared by the following steps:
adding 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, dioxane and acrylamide into a three-neck flask, setting the temperature at 40 ℃ and the rotating speed at 300r/min, dropwise adding a sodium methoxide methanol solution under the condition of nitrogen protection, after dropwise adding, heating the temperature to 80 ℃, keeping the rotating speed unchanged, continuing stirring for reaction for 5 hours, after the reaction is finished, cooling for crystallization, carrying out vacuum filtration, and drying the obtained filter cake at 40 ℃ to constant weight to obtain an auxiliary agent; wherein the sodium methoxide methanol solution is prepared from sodium methoxide and methanol according to the dosage ratio of 4 g: 10mL, and the dosage ratio of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, dioxane, acrylamide and sodium methoxide methanol solution is 0.2 mol: 20mL of: 0.2 mol: 5g of the total weight.
Example 3
The high-flame-retardant antistatic yarn comprises the following raw materials in parts by weight:
160 parts of polybutylene terephthalate/adipate, 3 parts of polyethylene glycol, 1 part of antistatic agent, 5 parts of flame retardant, 90 parts of wool fiber, 90 parts of cotton fiber and 200 parts of flame-retardant treatment fluid;
the high flame-retardant antistatic yarn is processed by the following steps:
respectively carrying out vacuum drying on poly (terephthalic acid)/butylene adipate and polyethylene glycol to ensure that the water content is less than 200ppm, blending with an antistatic agent and a flame retardant after drying treatment, carrying out melt spinning at 290 ℃ and the spinning speed of 1200r/min by a screw type spinning machine, cooling, oiling, pre-drafting and winding at 800m/min to obtain polyester fibers;
and secondly, soaking and drying wool fibers and cotton fibers in flame-retardant treatment liquid, twisting the wool fibers and the cotton fibers into a thread, and then spinning the thread and polyester fibers to prepare the high-flame-retardant antistatic yarn, wherein the flame-retardant treatment liquid is a flame retardant FPK8002, a WA dispersant, a penetrating agent JFC and deionized water according to a mass ratio of 8: 0.7: 0.3: 91 by mixing.
Wherein the antistatic agent is prepared by the following steps:
adding an antistatic component and dichloromethane into a round-bottom flask, adding a reagent and an auxiliary agent under the conditions of-20 ℃ and 400r/min of rotation speed, keeping the rotation speed unchanged at 25 ℃ and continuing stirring for 12 hours, extracting with saturated ammonium chloride and dichloromethane after the reaction is finished, and concentrating an organic phase at 30 ℃ under reduced pressure by using a rotary evaporator to obtain the antistatic agent.
Wherein the reagent is N, N' -dicyclohexylcarbodiimide, 4-dimethylaminopyridine and dichloromethane according to the dosage ratio of 11 mmol: 3 mmol: 5mL, and the dosage ratio of the antistatic component, dichloromethane, reagent and auxiliary agent is 5 g: 10mL of: 0.7 g: 1g of the total weight of the composition.
Wherein the antistatic component is prepared by the following steps:
step S11, adding chlorododecane and absolute ethyl alcohol into a three-neck flask, setting the temperature to be 80 ℃ and the rotating speed to be 400r/min, dropwise adding a diethanolamine solution while stirring, then adding sodium hydroxide, keeping the temperature unchanged, carrying out reflux reaction for 4.5 hours, and after the reaction is finished, carrying out reduced pressure distillation on the obtained reaction liquid to remove the absolute ethyl alcohol to obtain an intermediate A;
step S12, mixing diethanolamine and N, N-dimethylacetamide according to the dosage ratio of 13 g: 10mL of the mixture is mixed to obtain a solution a, and succinic anhydride and N, N-dimethylacetamide are mixed according to the dosage ratio of 12 g: 10mL of the solution a is mixed to obtain a solution B, the solution a is added into a three-neck flask, the solution B with the same volume is dripped under the conditions that the temperature is 30 ℃ and the rotating speed is 400r/min, the dripping time is 1h, and after the dripping is finished, the solution B is stirred and mixed for 3h under the condition of 26 ℃ to obtain a mixed solution B;
and S13, adding the intermediate A into the mixed solution B, adding toluene and p-toluenesulfonic acid, setting the temperature at 110 ℃ and the rotating speed at 400r/min, heating and refluxing for 2h, after the reaction is finished, concentrating under reduced pressure at 60 ℃ in a rotary evaporator until the volume is unchanged to obtain a concentrated solution, adding the obtained concentrated solution into N, N-dimethylacetamide, adding 4-dimethylaminopyridine, setting the temperature at 80 ℃ and the rotating speed at 400r/min, dropwise adding the solution B prepared in the step S12 while stirring, keeping the temperature and the rotating speed unchanged after dropwise adding, and continuously stirring for 6h to obtain the antistatic component.
Wherein the diethanolamine solution in the step S11 is diethanolamine and absolute ethyl alcohol according to the dosage ratio of 1 g: 5mL, and the dosage ratio of the chlorododecane, the absolute ethyl alcohol, the diethanolamine solution and the sodium hydroxide is 4 g: 50mL of: 10mL of: 1g of a compound; in the step S13, the dosage ratio of the intermediate A, the mixed liquid B, the toluene and the p-toluenesulfonic acid is 5 g: 20mL of: 50mL of: 0.1 g; the dosage ratio of the concentrated solution, the N, N-dimethylacetamide, the 4-dimethylaminopyridine and the solution b is 40 mL: 80mL of: 0.8 g: 4 mL.
Wherein, the flame retardant is prepared by the following steps:
adding an auxiliary agent, dioxane and triethylamine into a three-neck flask, setting the temperature at 45 ℃ and the rotating speed at 400r/min, dropwise adding cyanuric chloride mixed solution while stirring, controlling the dropwise adding speed at 3 drops/second, keeping the temperature and the rotating speed unchanged after dropwise adding, continuously stirring for 4 hours, and removing dioxane by reduced pressure distillation to obtain the flame retardant; wherein the cyanuric chloride mixed solution is cyanuric chloride and dioxane in a mass ratio of 1: 7, the mass ratio of the auxiliary agent, dioxane, triethylamine and cyanuric chloride is 20: 50: 12: 80.
the auxiliary agent is prepared by the following steps:
adding 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, dioxane and acrylamide into a three-neck flask, setting the temperature at 40 ℃ and the rotating speed at 300r/min, dropwise adding a sodium methoxide methanol solution under the condition of nitrogen protection, after dropwise adding, heating the temperature to 80 ℃, keeping the rotating speed unchanged, continuing stirring for reaction for 5 hours, after the reaction is finished, cooling for crystallization, carrying out vacuum filtration, and drying the obtained filter cake at 40 ℃ to constant weight to obtain an auxiliary agent; wherein the sodium methoxide methanol solution is prepared from sodium methoxide and methanol according to the dosage ratio of 5 g: 10mL, and the dosage ratio of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, dioxane, acrylamide and sodium methoxide methanol solution is 0.2 mol: 20mL of: 0.2 mol: 5g of the total weight.
Comparative example 1
The antistatic agent of example 1 was not added, and the remaining raw materials and preparation process remained unchanged.
Comparative example 2
The flame retardant of example 1 was not added, and the remaining raw materials and preparation process remained unchanged.
The yarns prepared in examples 1-3 and comparative example 1 are subjected to performance test, and the vertical burning is tested by adopting the GB2409-87 standard; the test results are shown in table 1 below:
TABLE 1
Categories | Oxygen index% | Flame retardant rating | Volume resistivity omega cm | Strength cN/dtex |
Example 1 | 34 | FV-0 | 1.5×1010 | 2.6 |
Example 2 | 34 | FV-0 | 1.5×1010 | 2.6 |
Example 3 | 34 | FV-0 | 1.5×1010 | 2.6 |
Comparative example 1 | 28 | FV-1 | 2.5×1011 | 2.5 |
Comparative example 2 | 25 | FV-2 | 2.0×1010 | 2.5 |
From the above table 1, it can be seen that the yarn prepared by the invention has good antistatic property and flame retardant property, and the prepared antistatic agent and the flame retardant are matched with each other, so that the flame retardant property and the antistatic property are improved.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (8)
1. The high-flame-retardant antistatic yarn is characterized by comprising the following raw materials in parts by weight:
160 parts of polybutylene terephthalate/adipate, 1-3 parts of polyethylene glycol, 0.6-1 part of antistatic agent, 3-5 parts of flame retardant, 70-90 parts of wool fiber, 70-90 parts of cotton fiber and 200 parts of flame retardant treatment fluid;
the high flame-retardant antistatic yarn is processed by the following steps:
respectively carrying out vacuum drying on the poly (terephthalic acid)/butylene adipate and the polyethylene glycol to ensure that the water content is less than 200ppm, blending the poly (terephthalic acid)/butylene adipate and the polyethylene glycol with an antistatic agent and a flame retardant after drying treatment, carrying out melt spinning on the poly (terephthalic acid)/butylene adipate and the polyethylene glycol by a screw type spinning machine at the conditions of 290 ℃ of temperature plus 250 ℃ and 1200r/min of spinning speed, cooling, and carrying out oiling, pre-drafting and 800m/min of winding treatment of 700 plus 700) to obtain polyester fibers;
and secondly, soaking and drying wool fibers and cotton fibers in flame-retardant treatment liquid, twisting the wool fibers and the cotton fibers into a thread, and then spinning the thread and polyester fibers to prepare the high-flame-retardant antistatic yarn, wherein the flame-retardant treatment liquid is a flame retardant FPK8002, a WA dispersant, a penetrating agent JFC and deionized water according to a mass ratio of 8: 0.7: 0.3: 91 by mixing.
2. The high flame-retardant antistatic yarn according to claim 1, wherein the antistatic agent is prepared by the following steps:
adding an antistatic component and dichloromethane into a round-bottom flask, adding a reagent and an auxiliary agent under the conditions of-20 ℃ and 400r/min of rotation speed, keeping the rotation speed unchanged at 25 ℃ and continuing stirring for 12 hours, extracting with saturated ammonium chloride and dichloromethane after the reaction is finished, and concentrating an organic phase at 30 ℃ under reduced pressure by using a rotary evaporator to obtain the antistatic agent.
3. The high flame-retardant antistatic yarn as claimed in claim 2, wherein the agent is N, N' -dicyclohexylcarbodiimide, 4-dimethylaminopyridine and dichloromethane in a ratio of 11 mmol: 3 mmol: 5mL, and the dosage ratio of the antistatic component, dichloromethane, reagent and auxiliary agent is 5 g: 10mL of: 0.5-0.7 g: 1g of the total weight of the composition.
4. The high flame-retardant antistatic yarn according to claim 2, wherein the antistatic component is prepared by the following steps:
step S11, adding chlorododecane and absolute ethyl alcohol into a three-neck flask, setting the temperature to be 70-80 ℃ and the rotating speed to be 400r/min, dropwise adding a diethanolamine solution while stirring, then adding sodium hydroxide, keeping the temperature unchanged, carrying out reflux reaction for 4-5h, and after the reaction is finished, carrying out reduced pressure distillation on the obtained reaction liquid to remove the absolute ethyl alcohol to obtain an intermediate A;
step S12, mixing diethanolamine and N, N-dimethylacetamide according to the dosage ratio of 12-13 g: 10mL of the mixture is mixed to obtain a solution a, and succinic anhydride and N, N-dimethylacetamide are mixed according to the dosage ratio of 12 g: 10mL of the solution a is mixed to obtain a solution B, the solution a is added into a three-neck flask, the solution B with the same volume is dripped under the conditions that the temperature is 30 ℃ and the rotating speed is 400r/min, the dripping time is 1h, and after the dripping is finished, the solution B is stirred and mixed for 3h under the condition of 26 ℃ to obtain a mixed solution B;
and S13, adding the intermediate A into the mixed solution B, then adding toluene and p-toluenesulfonic acid, setting the temperature at 110 ℃ and the rotating speed at 400r/min, heating and refluxing for 1-3h, after the reaction is finished, concentrating under reduced pressure at 60 ℃ in a rotary evaporator until the volume is unchanged to obtain a concentrated solution, adding the obtained concentrated solution into N, N-dimethylacetamide, then adding 4-dimethylaminopyridine, setting the temperature at 80 ℃ and the rotating speed at 400r/min, dropwise adding the solution B prepared in the step S12 while stirring, keeping the temperature and the rotating speed unchanged after dropwise adding, and continuously stirring for 6h to obtain the antistatic component.
5. The high flame-retardant antistatic yarn as claimed in claim 4, wherein the diethanolamine solution in the step S11 is diethanolamine and absolute ethanol in a ratio of 1 g: 5mL, and the dosage ratio of the chlorododecane, the absolute ethyl alcohol, the diethanolamine solution and the sodium hydroxide is 4 g: 50mL of: 10mL of: 0.8-1 g; in the step S13, the dosage ratio of the intermediate A, the mixed liquid B, the toluene and the p-toluenesulfonic acid is 5 g: 20mL of: 50mL of: 0.1 g; the dosage ratio of the concentrated solution, the N, N-dimethylacetamide, the 4-dimethylaminopyridine and the solution b is 40 mL: 80mL of: 0.6-0.8 g: 2-4 mL.
6. The high flame-retardant antistatic yarn as claimed in claim 1, wherein the flame retardant is prepared by the following steps:
adding an auxiliary agent, dioxane and triethylamine into a three-neck flask, setting the temperature at 45 ℃ and the rotating speed at 400r/min, dropwise adding cyanuric chloride mixed solution while stirring, controlling the dropwise adding speed at 1-3 drops/second, keeping the temperature and the rotating speed unchanged after dropwise adding, continuously stirring for 4 hours, and removing dioxane by reduced pressure distillation to obtain the flame retardant; wherein the cyanuric chloride mixed solution is cyanuric chloride and dioxane in a mass ratio of 1: 7, the mass ratio of the auxiliary agent, dioxane, triethylamine and cyanuric chloride is 20: 50: 12: 80.
7. the high flame-retardant antistatic yarn as claimed in claim 2, wherein the auxiliary is prepared by the following steps:
adding 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, dioxane and acrylamide into a three-neck flask, setting the temperature at 40 ℃ and the rotating speed at 300r/min, dropwise adding a sodium methoxide methanol solution under the condition of nitrogen protection, after dropwise adding, heating the temperature to 80 ℃, keeping the rotating speed unchanged, continuing stirring for reaction for 5 hours, after the reaction is finished, cooling for crystallization, carrying out vacuum filtration, and drying the obtained filter cake at 40 ℃ to constant weight to obtain an auxiliary agent; wherein the sodium methoxide methanol solution is prepared from sodium methoxide and methanol according to the dosage ratio of 3-5 g: 10mL, and the dosage ratio of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, dioxane, acrylamide and sodium methoxide methanol solution is 0.2 mol: 20mL of: 0.2 mol: 5g of the total weight.
8. The processing method of the high flame-retardant antistatic yarn as claimed in claim 1, characterized by comprising the following steps:
respectively carrying out vacuum drying on the poly (terephthalic acid)/butylene adipate and the polyethylene glycol to ensure that the water content is less than 200ppm, blending the poly (terephthalic acid)/butylene adipate and the polyethylene glycol with an antistatic agent and a flame retardant after drying treatment, carrying out melt spinning on the poly (terephthalic acid)/butylene adipate and the polyethylene glycol by a screw type spinning machine at the conditions of 290 ℃ of temperature plus 250 ℃ and 1200r/min of spinning speed, cooling, and carrying out oiling, pre-drafting and 800m/min of winding treatment of 700 plus 700) to obtain polyester fibers;
and secondly, soaking and drying wool fibers and cotton fibers in flame-retardant treatment liquid, twisting the wool fibers and the cotton fibers into a thread, and then spinning the thread and polyester fibers to prepare the high-flame-retardant antistatic yarn, wherein the flame-retardant treatment liquid is a flame retardant FPK8002, a WA dispersant, a penetrating agent JFC and deionized water according to a mass ratio of 8: 0.7: 0.3: 91 by mixing.
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CN104278349A (en) * | 2013-07-02 | 2015-01-14 | 上海杰事杰新材料(集团)股份有限公司 | Antistatic and flame retardant copolyester fiber and preparation method thereof |
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