CN108179492A - A kind of preparation method of estersil cladded type flame-retardant polypropylene long filament - Google Patents
A kind of preparation method of estersil cladded type flame-retardant polypropylene long filament Download PDFInfo
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- CN108179492A CN108179492A CN201711277918.0A CN201711277918A CN108179492A CN 108179492 A CN108179492 A CN 108179492A CN 201711277918 A CN201711277918 A CN 201711277918A CN 108179492 A CN108179492 A CN 108179492A
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- 239000004743 Polypropylene Substances 0.000 title claims abstract description 59
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 59
- -1 polypropylene Polymers 0.000 title claims abstract description 48
- 239000003063 flame retardant Substances 0.000 title claims abstract description 23
- 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 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 claims abstract description 7
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000005253 cladding Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 239000006185 dispersion Substances 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 235000019441 ethanol Nutrition 0.000 claims description 12
- 238000005576 amination reaction Methods 0.000 claims description 10
- 239000006210 lotion Substances 0.000 claims description 10
- DCXXMTOCNZCJGO-UHFFFAOYSA-N tristearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCCCCCC DCXXMTOCNZCJGO-UHFFFAOYSA-N 0.000 claims description 10
- 230000001476 alcoholic effect Effects 0.000 claims description 9
- 239000003054 catalyst Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims description 8
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 8
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 8
- 238000001125 extrusion Methods 0.000 claims description 8
- 229910000077 silane Inorganic materials 0.000 claims description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 6
- 230000036571 hydration Effects 0.000 claims description 5
- 238000006703 hydration reaction Methods 0.000 claims description 5
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 4
- 239000000908 ammonium hydroxide Substances 0.000 claims description 4
- 239000011575 calcium Substances 0.000 claims description 4
- 229910052791 calcium Inorganic materials 0.000 claims description 4
- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical compound CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- 230000009467 reduction Effects 0.000 claims description 4
- WBHHMMIMDMUBKC-XLNAKTSKSA-N ricinelaidic acid Chemical compound CCCCCC[C@@H](O)C\C=C\CCCCCCCC(O)=O WBHHMMIMDMUBKC-XLNAKTSKSA-N 0.000 claims description 4
- 229960003656 ricinoleic acid Drugs 0.000 claims description 4
- FEUQNCSVHBHROZ-UHFFFAOYSA-N ricinoleic acid Natural products CCCCCCC(O[Si](C)(C)C)CC=CCCCCCCCC(=O)OC FEUQNCSVHBHROZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000009987 spinning Methods 0.000 claims description 4
- 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 4
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims 1
- 230000032050 esterification Effects 0.000 abstract description 6
- 238000005886 esterification reaction Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 2
- 230000004888 barrier function Effects 0.000 abstract description 2
- 239000003610 charcoal Substances 0.000 abstract description 2
- 239000000835 fiber Substances 0.000 description 22
- 239000004744 fabric Substances 0.000 description 5
- 239000000654 additive Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000002604 ultrasonography Methods 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 239000012209 synthetic fiber Substances 0.000 description 3
- 229920002994 synthetic fiber Polymers 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 235000012489 doughnuts Nutrition 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241001502050 Acis Species 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 241000876833 Emberizinae Species 0.000 description 1
- 206010046996 Varicose vein Diseases 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- OMUGFZNEOIWQOD-UHFFFAOYSA-N boric acid;zinc Chemical compound [Zn].OB(O)O OMUGFZNEOIWQOD-UHFFFAOYSA-N 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000012433 hydrogen halide Substances 0.000 description 1
- 229910000039 hydrogen halide Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 238000009940 knitting Methods 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- 239000006259 organic additive Substances 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- 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
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a kind of preparation methods of estersil cladded type flame-retardant polypropylene long filament, zinc borate, Ludox, the talcum powder of the material addition of the present invention can play good fire retardant performance, wherein esterification cladding material can form stable charcoal ball in burning, the effect of good gas phase barrier is played, achievees the effect that further to reduce the intensity of a fire.
Description
Technical field
The invention belongs to polypropylene filament yarn fields, and in particular to a kind of preparation method of estersil cladded type flame-retardant polypropylene long filament.
Background technology
Polypropylene filament yarn is to make that raw material is aggregated, fiber made from melt spinning as propylene.Polypropylene fibre in nineteen fifty-seven formally
Industrialized production is the up-and-coming youngster in synthetic fibers.Since polypropylene fibre has simple production process, product is inexpensive, and intensity is high, phase
The advantages that light to density, so polypropylene fibre develops quickly.Polypropylene fibre has been the fourth-largest kind of synthetic fibers at present, is general chemical
Most light fiber in fiber.The kind of polypropylene fibre have long filament (including not deformed long filament and varicosity modified continuous filament), staple fiber, bristlelike monofilament,
Film-fibre, doughnut, profiled filament, various composite fibres and bonded fabric etc..It is mainly used for making carpet (including ground
Blanket base fabric and matte), bunting, furniture stuff, various ropes, band, fishing net, asphalt felt, building reinforcing material, packaging material and
Industrial cloth, such as filter cloth, bagging.In addition in terms of clothing using also increasingly extensively, can with multiple fiber is blended that difference is made
Shirt, coat, sweat shirt, socks etc. can be made after knitting is processed in the blended fabric of type.By polypropylene fibre doughnut system
Into wadding quilt, light, warming, elasticity is good.Fiber obtained.Polypropylene fibre formally starts industrialized production in nineteen fifty-seven, is synthesis
Up-and-coming youngster in fiber.Due to the advantages that polypropylene fibre has simple production process, and product is inexpensive, and intensity is high, and relative density is light, institute
Develop quickly with polypropylene fibre.Polypropylene fibre has been the fourth-largest kind of synthetic fibers at present, is fiber most light in general chemical fiber;
However polypropylene is mainly made of elements such as carbon, hydrogen, material poor fire itself, is easily dropped under the action of heat
Solution generates imflammable gas, easily burning, and so as to which fire occur, great harm is brought to the safety of life and property of people, because
This often adds multiple additives wherein when polypropylene fibre is prepared, including inorganic additive and organic additive, wherein
Inorganic additive is easily reduced the mechanical property of finished product long filament due to the poor compatibility with polymeric matrix, and organic filament master
If containing halogen and phosphorous fire retardant, the fire retardant particularly containing chlorine, bromine is even more to be widely used, but it is special in burning
It does not release the hydrogen halide of irritation and radiativity easily, there is very strong harm to human body;
It is therefore an object of the present invention to provide a kind of anti-flammability preferable polypropylene filament yarn, it is made also to have very in burning
Good Safety and Environmental Protection, while the problem of improve poor compatibility of the inorganic fire-retarded additive of tradition in polypropylene matrix, effectively
Raising finished product mechanical property.
Invention content
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of estersil cladded type flame-retardant polypropylene is long
The preparation method of silk.
To achieve the above object, the present invention uses following technical scheme:
A kind of preparation method of estersil cladded type flame-retardant polypropylene long filament, includes the following steps:
(1) lauryl mercaptan of 2-3 parts by weight is taken, is added in the absolute ethyl alcohol of 10-12 times of its weight, stirring is equal
It is even, the ricinoleic acid calcium of 0.6-1 parts by weight is added in, insulated and stirred 4-5 minutes at 60-65 DEG C, obtains compound alcoholic solution;
(2) presoma of 36-40 parts by weight is taken, is added in above-mentioned compound alcoholic solution, adds in the diformazan of 1-2 parts by weight
Amine, it is 10-15 minutes ultrasonic, obtain amination alcohol dispersion liquid;
(3) hydration zinc borate of 4-5 parts by weight is taken, is added in the deionized water of 20-30 times of its weight, stirs evenly,
Above-mentioned amination alcohol dispersion liquid is added in, raising temperature is 50-60 DEG C, adds in the Dodecydimethylammonium bronides of 0.7-1 parts by weight,
Insulated and stirred 10-20 minutes, reduction temperature are room temperature, and the ammonium hydroxide of dropwise addition 5-6 parts by weight, a concentration of 10-13% is added dropwise
After be stirred to react 3-4 hours, obtain Sol-gel Coated solution;
(4) talcum powder of 4-5 parts by weight is taken, is added in the deionized water of 17-20 times of its weight, adds in 10-14 weight
The orthosilicic acid of part, stirs evenly, obtains silicate solution;
(5) above-mentioned Sol-gel Coated solution, silicate solution mixing are taken, stirs evenly, is sent in reaction kettle, adjust reaction kettle
Temperature is 90-95 DEG C, and the catalyst solution of 2-3 parts by weight is added dropwise, is added dropwise latter insulated and stirred 3-4 hours, discharges, obtains estersil
Sol-gel Coated solution;
(6) glyceryl tristearate of 0.3-0.5 parts by weight is taken, is added in above-mentioned estersil Sol-gel Coated solution, is stirred
Uniformly, estersil Sol-gel Coated lotion is obtained;
(7) isotactic polypropylene of 110-120 parts by weight is taken, is added to 6-9 times of its weight, 70-75% ethanol solution
In, the gamma-aminopropyl-triethoxy-silane of 3-4 parts by weight is added in, it is 10-29 minutes ultrasonic, obtain silane polypropylene dispersion liquid;
(8) above-mentioned estersil Sol-gel Coated lotion, the mixing of silane polypropylene dispersion liquid are taken, is sent to 65-70 DEG C of thermostatted water
In bath, insulated and stirred 16-20 hours discharges, and precipitation is washed in filtering, and it is 0.1- to be dried at 46-50 DEG C of vacuum to water content
0.2%, it is cooled to room temperature, obtains estersil Sol-gel Coated modified polypropene;
(9) above-mentioned estersil Sol-gel Coated modified polypropene is taken, is sent in screw extruder, melting extrusion, extrusion temperature
It is 270-300 DEG C, melt is subjected to spinning, by receives silk processing to get the estersil cladded type flame-retardant polypropylene long filament.
The presoma is ethyl orthosilicate.
The preparation method of the catalyst solution is:
The p-methyl benzenesulfonic acid of 1-2 parts by weight is taken, is added in the deionized water of 24-30 times of its weight, stirs evenly, i.e.,
.
Advantages of the present invention:
The present invention is disperseed in alcoholic solution, is handled using dimethylamine, obtained first using ethyl orthosilicate as presoma in advance
Amination dispersion liquid, then using hydration zinc borate as raw material, Dodecydimethylammonium bronides are dispersant, by ethyl orthosilicate water
Solution by hydrolysis by sol deposition to boric acid zinc surface, obtains amination Sol-gel Coated solution, then mixes it with orthosilicic acid,
Esterification is carried out under catalyst action, obtains esters of silicon acis cladding Sol-gel Coated solution, then disperse by glyceryl tristearate,
Dispersion esterification lotion is obtained, isotactic polypropylene is handled using amino silicane coupling agent later, obtains amino silane polypropylene dispersion liquid,
Finally by itself and dispersion esterification emulsion blending dispersion, esterification lotion the having in polypropylene containing inorganic coating filler is realized
It imitates compatible, effectively raises the mechanical property of finished product polypropylene fibre, zinc borate that material of the invention adds in, Ludox, talcum powder
Good fire retardant performance can be played, wherein esterification cladding material can form stable charcoal ball in burning, is played very
The effect of good gas phase barrier, achievees the effect that further to reduce the intensity of a fire.
Specific embodiment
Embodiment 1
A kind of preparation method of estersil cladded type flame-retardant polypropylene long filament, includes the following steps:
(1) lauryl mercaptan of 3 parts by weight is taken, is added in the absolute ethyl alcohol of 12 times of its weight, stirs evenly, is added in
The ricinoleic acid calcium of 1 parts by weight, insulated and stirred 5 minutes at 65 DEG C, obtains compound alcoholic solution;
(2) presoma of 40 parts by weight is taken, is added in above-mentioned compound alcoholic solution, adds in the dimethylamine of 2 parts by weight, ultrasound
15 minutes, obtain amination alcohol dispersion liquid;
(3) hydration zinc borate of 5 parts by weight is taken, is added in the deionized water of 30 times of its weight, stirs evenly, in addition
Amination alcohol dispersion liquid is stated, raising temperature is 60 DEG C, adds in the Dodecydimethylammonium bronides of 1 parts by weight, and insulated and stirred 20 is divided
Clock, reduction temperature are room temperature, and 6 parts by weight, a concentration of 13% ammonium hydroxide is added dropwise, is stirred to react 4 hours, obtains molten after being added dropwise
Glue cladding solution;
(4) talcum powder of 5 parts by weight is taken, is added in the deionized water of 20 times of its weight, adds in the former silicon of 14 parts by weight
Acid stirs evenly, and obtains silicate solution;
(5) above-mentioned Sol-gel Coated solution, silicate solution mixing are taken, stirs evenly, is sent in reaction kettle, adjust reaction kettle
Temperature is 95 DEG C, and the catalyst solution of 3 parts by weight is added dropwise, rear insulated and stirred is added dropwise 4 hours, discharges, obtains estersil colloidal sol packet
Cover solution;
(6) glyceryl tristearate of 0.5 parts by weight is taken, is added in above-mentioned estersil Sol-gel Coated solution, stirs evenly,
Obtain estersil Sol-gel Coated lotion;
(7) isotactic polypropylene of 120 parts by weight is taken, is added in 9 times of its weight, 75% ethanol solution, adds in 4 weights
The gamma-aminopropyl-triethoxy-silane of part is measured, ultrasound 29 minutes obtains silane polypropylene dispersion liquid;
(8) above-mentioned estersil Sol-gel Coated lotion, the mixing of silane polypropylene dispersion liquid are taken, is sent to 70 DEG C of water bath with thermostatic control
In, insulated and stirred 20 hours discharges, and precipitation is washed in filtering, and it is 0.2% to be dried at 50 DEG C of vacuum to water content, is cooled to often
Temperature obtains estersil Sol-gel Coated modified polypropene;
(9) above-mentioned estersil Sol-gel Coated modified polypropene is taken, is sent in screw extruder, melting extrusion, extrusion temperature
It is 300 DEG C, melt is subjected to spinning, by receives silk processing to get the estersil cladded type flame-retardant polypropylene long filament.
The presoma is ethyl orthosilicate.
The preparation method of the catalyst solution is:
Take the p-methyl benzenesulfonic acid of 2 parts by weight, be added in the deionized water of 30 times of its weight, stir evenly to get.
Embodiment 2
A kind of preparation method of estersil cladded type flame-retardant polypropylene long filament, includes the following steps:
(1) lauryl mercaptan of 2 parts by weight is taken, is added in the absolute ethyl alcohol of 10 times of its weight, stirs evenly, is added in
The ricinoleic acid calcium of 0.6 parts by weight, insulated and stirred 4 minutes at 60 DEG C, obtains compound alcoholic solution;
(2) presoma of 36 parts by weight is taken, is added in above-mentioned compound alcoholic solution, adds in the dimethylamine of 1 parts by weight, ultrasound
10 minutes, obtain amination alcohol dispersion liquid;
(3) hydration zinc borate of 4 parts by weight is taken, is added in the deionized water of 20 times of its weight, stirs evenly, in addition
Amination alcohol dispersion liquid is stated, raising temperature is 50 DEG C, adds in the Dodecydimethylammonium bronides of 0.7 parts by weight, insulated and stirred 10
Minute, reduction temperature is room temperature, and 5 parts by weight, a concentration of 10% ammonium hydroxide is added dropwise, is stirred to react 3 hours, obtains after being added dropwise
Sol-gel Coated solution;
(4) talcum powder of 4 parts by weight is taken, is added in the deionized water of 17 times of its weight, adds in the former silicon of 10 parts by weight
Acid stirs evenly, and obtains silicate solution;
(5) above-mentioned Sol-gel Coated solution, silicate solution mixing are taken, stirs evenly, is sent in reaction kettle, adjust reaction kettle
Temperature is 90 DEG C, and the catalyst solution of 2 parts by weight is added dropwise, rear insulated and stirred is added dropwise 3 hours, discharges, obtains estersil colloidal sol packet
Cover solution;
(6) glyceryl tristearate of 0.3 parts by weight is taken, is added in above-mentioned estersil Sol-gel Coated solution, stirs evenly,
Obtain estersil Sol-gel Coated lotion;
(7) isotactic polypropylene of 110 parts by weight is taken, is added in 6 times of its weight, 70% ethanol solution, adds in 3 weights
The gamma-aminopropyl-triethoxy-silane of part is measured, ultrasound 10 minutes obtains silane polypropylene dispersion liquid;
(8) above-mentioned estersil Sol-gel Coated lotion, the mixing of silane polypropylene dispersion liquid are taken, is sent to 65 DEG C of water bath with thermostatic control
In, insulated and stirred 16 hours discharges, and precipitation is washed in filtering, and it is 0.1% to be dried at 46 DEG C of vacuum to water content, is cooled to often
Temperature obtains estersil Sol-gel Coated modified polypropene;
(9) above-mentioned estersil Sol-gel Coated modified polypropene is taken, is sent in screw extruder, melting extrusion, extrusion temperature
It is 270 DEG C, melt is subjected to spinning, by receives silk processing to get the estersil cladded type flame-retardant polypropylene long filament.
The presoma is ethyl orthosilicate.
The preparation method of the catalyst solution is:
Take the p-methyl benzenesulfonic acid of 1 parts by weight, be added in the deionized water of 24 times of its weight, stir evenly to get.
Performance test:
The estersil cladded type flame-retardant polypropylene long filament of embodiment 1:
Intensity is 9.9g/d, and elongation at break 13.9%, oxygen index (OI) 32, UL-94 are V-1 ranks;
The estersil cladded type flame-retardant polypropylene long filament of embodiment 2:
Intensity is 10.3g/d, and elongation at break 14.5%, oxygen index (OI) 33, UL-94 are V-1 ranks;
Commercially available polypropylene filament yarn:
Intensity is 4-5g/d, and elongation at break 10-12%, oxygen index (OI) 20-25, UL-94 are V-2 ranks;
As can be seen that the estersil cladded type flame-retardant polypropylene long filament of the present invention has better mechanical property and fire-retardant fireproof
Property.
Claims (3)
1. a kind of preparation method of estersil cladded type flame-retardant polypropylene long filament, which is characterized in that include the following steps:
(1) lauryl mercaptan of 2-3 parts by weight is taken, is added in the absolute ethyl alcohol of 10-12 times of its weight, stirs evenly, add
Enter the ricinoleic acid calcium of 0.6-1 parts by weight, insulated and stirred 4-5 minutes at 60-65 DEG C, obtain compound alcoholic solution;
(2) presoma of 36-40 parts by weight is taken, is added in above-mentioned compound alcoholic solution, adds in the dimethylamine of 1-2 parts by weight, is surpassed
Sound 10-15 minutes obtains amination alcohol dispersion liquid;
(3) hydration zinc borate of 4-5 parts by weight is taken, is added in the deionized water of 20-30 times of its weight, stirs evenly, is added in
Above-mentioned amination alcohol dispersion liquid, raising temperature are 50-60 DEG C, add in the Dodecydimethylammonium bronides of 0.7-1 parts by weight, heat preservation
Stirring 10-20 minutes, reduction temperature are room temperature, and the ammonium hydroxide of dropwise addition 5-6 parts by weight, a concentration of 10-13% stirs after being added dropwise
Reaction 3-4 hours is mixed, obtains Sol-gel Coated solution;
(4) talcum powder of 4-5 parts by weight is taken, is added in the deionized water of 17-20 times of its weight, adds in 10-14 parts by weight
Orthosilicic acid stirs evenly, and obtains silicate solution;
(5) above-mentioned Sol-gel Coated solution, silicate solution mixing are taken, stirs evenly, is sent in reaction kettle, adjust temperature of reaction kettle
It is 90-95 DEG C, the catalyst solution of 2-3 parts by weight is added dropwise, is added dropwise latter insulated and stirred 3-4 hours, discharges, obtain estersil colloidal sol
Cladding solution;
(6) glyceryl tristearate of 0.3-0.5 parts by weight is taken, is added in above-mentioned estersil Sol-gel Coated solution, stirs evenly,
Obtain estersil Sol-gel Coated lotion;
(7) isotactic polypropylene of 110-120 parts by weight is taken, in ethanol solution that be added to 6-9 times of its weight, 70-75%, is added
Enter the gamma-aminopropyl-triethoxy-silane of 3-4 parts by weight, it is 10-29 minutes ultrasonic, obtain silane polypropylene dispersion liquid;
(8) above-mentioned estersil Sol-gel Coated lotion, the mixing of silane polypropylene dispersion liquid are taken, is sent in 65-70 DEG C of water bath with thermostatic control,
Insulated and stirred 16-20 hours discharges, and precipitation is washed in filtering, and it is 0.1-0.2% to be dried at 46-50 DEG C of vacuum to water content,
It is cooled to room temperature, obtains estersil Sol-gel Coated modified polypropene;
(9) above-mentioned estersil Sol-gel Coated modified polypropene is taken, is sent in screw extruder, melting extrusion, extrusion temperature is
270-300 DEG C, melt is subjected to spinning, by receiving silk processing to get the estersil cladded type flame-retardant polypropylene long filament.
2. the preparation method of a kind of estersil cladded type flame-retardant polypropylene long filament according to claim 1, which is characterized in that described
Presoma be ethyl orthosilicate.
3. the preparation method of a kind of estersil cladded type flame-retardant polypropylene long filament according to claim 1, which is characterized in that described
The preparation method of catalyst solution be:
Take the p-methyl benzenesulfonic acid of 1-2 parts by weight, be added in the deionized water of 24-30 times of its weight, stir evenly to get.
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