CN104988733A - Water-soluble polyester slurry for FDY filament sizing water-jet weaving and preparation method thereof - Google Patents
Water-soluble polyester slurry for FDY filament sizing water-jet weaving and preparation method thereof Download PDFInfo
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- CN104988733A CN104988733A CN201510453115.0A CN201510453115A CN104988733A CN 104988733 A CN104988733 A CN 104988733A CN 201510453115 A CN201510453115 A CN 201510453115A CN 104988733 A CN104988733 A CN 104988733A
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- water
- phthalic acid
- jet weaving
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- fdy filament
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- 229920000728 polyester Polymers 0.000 title claims abstract description 35
- 238000009941 weaving Methods 0.000 title claims abstract description 34
- 239000002002 slurry Substances 0.000 title abstract description 19
- 238000002360 preparation method Methods 0.000 title abstract description 18
- 238000004513 sizing Methods 0.000 title abstract description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 105
- 238000000034 method Methods 0.000 claims abstract description 43
- 239000003054 catalyst Substances 0.000 claims abstract description 22
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims abstract description 20
- 150000001298 alcohols Chemical class 0.000 claims abstract description 13
- 238000006136 alcoholysis reaction Methods 0.000 claims abstract description 12
- 229920000570 polyether Polymers 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 238000007334 copolymerization reaction Methods 0.000 claims abstract description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 129
- 238000011084 recovery Methods 0.000 claims description 40
- 238000006243 chemical reaction Methods 0.000 claims description 39
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 38
- 229920002635 polyurethane Polymers 0.000 claims description 29
- 239000004814 polyurethane Substances 0.000 claims description 29
- 239000000463 material Substances 0.000 claims description 28
- 238000009955 starching Methods 0.000 claims description 27
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- 239000011734 sodium Substances 0.000 claims description 21
- 229910052708 sodium Inorganic materials 0.000 claims description 21
- 150000002148 esters Chemical group 0.000 claims description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 238000005194 fractionation Methods 0.000 claims description 16
- 238000006116 polymerization reaction Methods 0.000 claims description 16
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 14
- BDKLKNJTMLIAFE-UHFFFAOYSA-N 2-(3-fluorophenyl)-1,3-oxazole-4-carbaldehyde Chemical compound FC1=CC=CC(C=2OC=C(C=O)N=2)=C1 BDKLKNJTMLIAFE-UHFFFAOYSA-N 0.000 claims description 12
- AIDLAEPHWROGFI-UHFFFAOYSA-N 2-methylbenzene-1,3-dicarboxylic acid Chemical compound CC1=C(C(O)=O)C=CC=C1C(O)=O AIDLAEPHWROGFI-UHFFFAOYSA-N 0.000 claims description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 12
- 235000017281 sodium acetate Nutrition 0.000 claims description 12
- 229940087562 sodium acetate trihydrate Drugs 0.000 claims description 12
- 239000012634 fragment Substances 0.000 claims description 11
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 11
- 230000032050 esterification Effects 0.000 claims description 9
- 238000005886 esterification reaction Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical group [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 8
- 229940040526 anhydrous sodium acetate Drugs 0.000 claims description 8
- 229910052787 antimony Inorganic materials 0.000 claims description 8
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 8
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical group O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 8
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 8
- 230000008018 melting Effects 0.000 claims description 8
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 229920000642 polymer Polymers 0.000 claims description 8
- 230000000630 rising effect Effects 0.000 claims description 8
- 239000011343 solid material Substances 0.000 claims description 8
- 230000003068 static effect Effects 0.000 claims description 8
- 238000012360 testing method Methods 0.000 claims description 8
- 239000004246 zinc acetate Substances 0.000 claims description 8
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical group [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 7
- 239000001639 calcium acetate Substances 0.000 claims description 7
- 235000011092 calcium acetate Nutrition 0.000 claims description 7
- 229960005147 calcium acetate Drugs 0.000 claims description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 239000002685 polymerization catalyst Substances 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 238000013467 fragmentation Methods 0.000 claims description 2
- 238000006062 fragmentation reaction Methods 0.000 claims description 2
- TZBAVQKIEKDGFH-UHFFFAOYSA-N n-[2-(diethylamino)ethyl]-1-benzothiophene-2-carboxamide;hydrochloride Chemical compound [Cl-].C1=CC=C2SC(C(=O)NCC[NH+](CC)CC)=CC2=C1 TZBAVQKIEKDGFH-UHFFFAOYSA-N 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 7
- 238000010521 absorption reaction Methods 0.000 abstract description 5
- 239000000835 fiber Substances 0.000 abstract description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 abstract description 4
- 239000007787 solid Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 230000009477 glass transition Effects 0.000 abstract description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 abstract 1
- 239000004721 Polyphenylene oxide Substances 0.000 abstract 1
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 239000012752 auxiliary agent Substances 0.000 abstract 1
- 238000003912 environmental pollution Methods 0.000 abstract 1
- 230000007062 hydrolysis Effects 0.000 abstract 1
- 238000006460 hydrolysis reaction Methods 0.000 abstract 1
- 230000002209 hydrophobic effect Effects 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 24
- 239000002699 waste material Substances 0.000 description 21
- 229920003023 plastic Polymers 0.000 description 19
- 239000004033 plastic Substances 0.000 description 19
- 239000007788 liquid Substances 0.000 description 7
- 238000006068 polycondensation reaction Methods 0.000 description 7
- 238000004017 vitrification Methods 0.000 description 7
- 206010009866 Cold sweat Diseases 0.000 description 6
- 239000004698 Polyethylene Substances 0.000 description 6
- 238000013461 design Methods 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 239000004744 fabric Substances 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 3
- HTXMGVTWXZBZNC-UHFFFAOYSA-N 3,5-bis(methoxycarbonyl)benzenesulfonic acid Chemical compound COC(=O)C1=CC(C(=O)OC)=CC(S(O)(=O)=O)=C1 HTXMGVTWXZBZNC-UHFFFAOYSA-N 0.000 description 2
- 229920001634 Copolyester Polymers 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920000151 polyglycol Polymers 0.000 description 2
- 239000010695 polyglycol Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 230000002087 whitening effect Effects 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- QPKOBORKPHRBPS-UHFFFAOYSA-N bis(2-hydroxyethyl) terephthalate Chemical compound OCCOC(=O)C1=CC=C(C(=O)OCCO)C=C1 QPKOBORKPHRBPS-UHFFFAOYSA-N 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- FYIBGDKNYYMMAG-UHFFFAOYSA-N ethane-1,2-diol;terephthalic acid Chemical compound OCCO.OC(=O)C1=CC=C(C(O)=O)C=C1 FYIBGDKNYYMMAG-UHFFFAOYSA-N 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000008233 hard water Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 239000002195 soluble material Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
Landscapes
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The invention discloses a water-soluble polyester slurry for FDY filament sizing water-jet weaving and a preparation method thereof, belongs to the technical field of water-soluble polyester slurry, and is used for mainly solving the problems that a conventional acrylic acid slurry has the product solid content of only about 30% and is high in transport costs, severe in environmental pollution, serious in moisture absorption and rebonding, low in adhesive power with hydrophobic polyester fibers and the like. The water-soluble polyester slurry is mainly characterized in that the water-soluble polyester slurry is prepared by alcoholysis, copolymerization, cooling and crushing of recycled polyester, ethylene glycol, m-phthalic acid-5-sulfonate or derivatives thereof, m-phthalic acid, other dihydric alcohols, a catalyst, an inorganic auxiliary agent and polyether with the weight-average molecular weight of 600-10000. The water-soluble polyester slurry has the characteristics of improving the product glass transition temperature, being excellent in chemical stability, hydrolysis resistance and thermal stability, being convenient to store and transport and having no addition and release of ammonia gas in the process of using, and is mainly used for preparation of the water-soluble polyester slurry for FDY filament sizing water-jet weaving.
Description
Technical field
The invention belongs to water-soluble polyurethane technical field, be specifically related to a kind of water-soluble environment protective polyester pulp for FDY filament starching water-jet weaving and preparation method thereof.
Background technology
Water jet looms is woven technically brings good economy, as a kind of shuttleless loom of high speed, in contemporary textile industry, shows vigorous vitality.Meanwhile, also expedited the emergence of the development of Water-Jet Weaving Size, Water-Jet Weaving Size is different from conventional slurry, and it will meet following characteristics: soluble in water when sizing mixing, when weaving, serous coat is water-fast, and during destarch, slurry is easy to remove again.
Water-Jet Weaving Size conventional is at present acrylic size, and this kind of slurry is that acrylicacidandesters is adopted polymerisation in solution under initator effect, then by carboxyl saponification in copolyesters, slurry is had water-soluble.When with ammoniacal liquor thickening, ammonia volatile feature when high temperature can be utilized, make the requirements of weaving process of resistance to water.During destarch, use alkali lye boiling-off, serous coat becomes acrylates that can be water-soluble, thus completes destarch.
Acrylic size is being produced, storing and transporting and is being had the following disadvantages in post processing: use a large amount of ammonia environment and human body being had to considerable influence in 1, producing; 2, product solid content only has about 30%, and to having time limit requirement, cost of transportation is high; 3, destarch waste liquid is difficult to biodegradation; 4, the adhesion of Acrylates to hydrophobicity polyster fibre is little.
Chinese patent CN1333792 " sulfonic polyester based on terephthalate " relates to the water dispersible sulfonic polyester comprising difunctional sulfomonomer and polyethylene glycol and is used as slurry.CN1834131 " water-soluable sizing material polyester and preparation method " proposes to add inorganic salts when preparing water-soluable sizing material polyester, and the polyester pulp of preparation can use in hard water.CN101955581A " water-soluble polyurethane prepared by waste and old polyester plastics and preparation method thereof " proposes waste and old polyester fragment, 1,2-propylene glycol, diglycol, water system polyester improver, compound stabilizer and catalyst to prepare water-soluble polyurethane in same reactor one-step method.CN102161751A " a kind of production method of polyester pulp " directly prepares polyester pulp with reaction material ethylene glycol terephthalate BHET, M-phthalic acid-5-sodium sulfonate SIPA, diglycol DEG etc.CN101967225A " preparation method of water-soluble sulfo-copolyester " proposes not use expensive polyethylene glycols raw material when producing polyester, adopts the mol ratio of lower dihydroxylic alcohols and binary acid (1: 1.3 ~ 1: 1.8) simultaneously) be suitable for storing to obtain higher glass transition temperature.
In prior art, acrylic size is described above, and clearly, slurry with water dissolubility polyester still exists following problem to shortcoming in addition: (1) product still has any moisture absorption viscosity again, affect water-jet weaving, product can be caused time serious to glue also; (2) for preventing moisture absorption adhesion again, needing the content reducing hydrophilic radical, the water-soluble of product may be affected, destarch may be caused time serious not thorough, affect fabric quality.
Summary of the invention
The object of the invention is for above-mentioned deficiency, a kind of preparation method of FDY filament starching water-jet weaving water-soluble polyurethane is provided, prepared water-soluble polyurethane has and both meets water-soluble requirement, depositing and leasing of silk is starched under can meeting again hot conditions, chemical stability is excellent, convenient storing, the feature of meet the requirement of environmental protection.
The technical solution of water-soluble polyurethane of the present invention is: a kind of FDY filament starching water-jet weaving water-soluble polyurethane, is characterized in that: be by Pillar recovery, the ethylene glycol accounting for Pillar recovery weight ratio 5 ~ 10% and following component
A, account for Pillar recovery weight ratio 10 ~ 20% M-phthalic acid-5-sulfonate or derivatives thereof,
B, account for Pillar recovery weight ratio 3 ~ 15% M-phthalic acid,
C, account for Pillar recovery weight ratio 5 ~ 10% other dihydroxylic alcohols,
D, account for Pillar recovery weight ratio 0.03 ~ 0.15% catalyst,
E, account for Pillar recovery weight ratio 0.02 ~ 0.1% inorganic assistant,
F, account for the polyethers of the weight average molecular weight 600 ~ 10000 of Pillar recovery weight ratio 0 ~ 5%,
Obtain through alcoholysis, copolymerization, cooling, fragmentation.
M-phthalic acid-5-sulfonate or derivatives thereof described in technical solution of the present invention is selected from M-phthalic acid-5-sodium sulfonate (SSIPA), dimethyl isophthalate-5-sodium sulfonate or M-phthalic acid binaryglycol ester-5-sodium sulfonate (SIPE).
Other dihydroxylic alcohols except ethylene glycol described in technical solution of the present invention is selected from diglycol, 2-methyl isophthalic acid, 3 propylene glycol, 2,2-dimethyl-1,3 propylene glycol.
Catalyst described in technical solution of the present invention comprises polyester catalyst and/or ester exchange catalyst, and polyester catalyst is selected from antimonous oxide or antimony glycol, and ester exchange catalyst is selected from zinc acetate or calcium acetate; Described inorganic assistant adopts anti-ether agent, and anti-ether agent is selected from anhydrous sodium acetate or Sodium acetate trihydrate.
Polyethers described in technical solution of the present invention is Macrogol 4000.
The technical solution that the present invention prepares above-mentioned water-soluble polyurethane method is: a kind of preparation method of FDY filament starching water-jet weaving water-soluble polyurethane, it is characterized in that comprising following four steps:
(1) Pillar recovery is made fragment, in proportion by Pillar recovery fragment, ethylene glycol, M-phthalic acid-5-sulfonate or derivatives thereof, M-phthalic acid, other dihydroxylic alcohols, put in fritting still after catalyst and inorganic assistant mixing, static normal pressure heats up, this process fritting still fractionation capital temperature incipient stage controls below 130 DEG C, between preferably 105 DEG C ± 3 DEG C, when in reaction, temperature reaches 235 DEG C ± 5 DEG C, the complete melting of material, distillate moisture or methyl alcohol when about reaching 90 ~ 100% of theoretical quantity of distillate, can judge that early stage has reacted, this process mainly carries out alcoholysis, ester exchange, esterification, in further rising, temperature is to 250-260 DEG C, improves fractionation capital temperature to about 180 DEG C, is distilled by unnecessary ethylene glycol moieties,
(2) according to reaction condition, after above fritting reaction terminates, material is imported terminal polymerization kettle, add polyethers simultaneously, progressively temperature in the kettle is improved from 235 DEG C of beginnings, stop heating when interior temperature reaches 265 DEG C, while intensification, slowly progressively improve vacuum in still and finally reach below absolute pressure 133Pa; Because polycondensation reaction belongs to exothermic reaction, and agitating friction heat-dissipating, reaction temperature can continue to raise; Interior temperature reaches 275 ± 2 DEG C, is polymerized under power of agitator 10KW condition, and the excessive ethylene glycol of residue removes by this process further, and then obtains the water-soluble polyurethane melt of FDY filament starching water-jet weaving;
(3) stop stirring, stop vacuumizing, with high pure nitrogen releasing vacuum is carried out to terminal polymerization kettle and pressurising to about 0.2MPa, open bottom valve, polymer be released in hopper and be cooled to solid material block;
(4) with strong crusher material block is broken into Powdered after, test, measure, pack, finished product.
The present invention's inorganic assistant prepared in the method for FDY filament starching water-jet weaving water-soluble polyurethane in (1) step is anti-ether agent.
M-phthalic acid-5-sulfonate the or derivatives thereof that the present invention is prepared in the method for FDY filament starching water-jet weaving water-soluble polyurethane described in (1) step is selected from M-phthalic acid-5-sodium sulfonate (SSIPA), dimethyl isophthalate-5-sodium sulfonate or M-phthalic acid-5-sodium sulfonate glycol ester (SIPE); Other described dihydroxylic alcohols is selected from diglycol, 2-methyl isophthalic acid, 3 propylene glycol, 2,2-dimethyl-1,3 propylene glycol; Described catalyst comprises polymerization catalyst and/or ester exchange catalyst, and polymerization catalyst is selected from antimonous oxide or antimony glycol, and ester exchange catalyst is selected from zinc acetate or calcium acetate; Described anti-ether agent adopts anhydrous sodium acetate or Sodium acetate trihydrate; Polyethers described in (2) step is selected from polyethylene glycol.
The dihydroxylic alcohols that the present invention adopts steric hindrance larger is as comonomer, have the following advantages: the vitrification point that 1, improve product on the basis of not reducing water-soluble monomer, make product both meet water-soluble requirement, under hot conditions can be met again, starch depositing and leasing of silk; 2, due to the special construction of the larger dihydroxylic alcohols of steric hindrance, provide the chemical stability of product fine, hydrolytic resistance and heat endurance, further guarantee the water resistance of slurry silk in water-jet weaving process; 3, adopt thermoplastic polyester solid, water soluble material, convenient storing, does not have wrap pages to be reclaimed, reduces storing cost and integrated cost; 4, in use, there is no adding and disengage, meet the requirement of environmental protection of ammonia, reduce the actual bodily harm to operative employee.
The present invention is mainly used in the preparation of FDY filament starching water-jet weaving water-soluble polyurethane.
Detailed description of the invention
Below by embodiment, the present invention will be further described.
Embodiment 1:
Component comprises:
Within waste and old Pillar recovery plastics 825kg(moisture content 6%),
Ethylene glycol 320kg(excessive more than 200%),
M-phthalic acid 50kg,
5-sodium sulfo isophthalate 125kg,
2,2-dimethyl-1,3 propylene glycol 50kg,
Anhydrous sodium acetate 1kg,
Sb
2O
3120g。
Preparation method:
(1) waste and old Pillar recovery plastics are made fragment, in proportion by waste and old Pillar recovery plastic flakes, ethylene glycol, 5-sodium sulfo isophthalate, M-phthalic acid, 2,2-dimethyl-1,3 propylene glycol, anhydrous sodium acetate, Sb
2o
3put in fritting still after mixing, static normal pressure heats up, this process fritting still fractionation capital temperature incipient stage controls below 130 DEG C, between preferably 105 DEG C ± 3 DEG C, when in reaction, temperature reaches 235 DEG C ± 5 DEG C, the complete melting of material, distillate moisture or methyl alcohol when about reaching 90 ~ 100% of theoretical quantity of distillate, can judge that early stage has reacted, this process mainly carries out alcoholysis, ester exchange, esterification; In further rising, temperature is to 250-260 DEG C, improves fractionation capital temperature to about 180 DEG C, is distilled by unnecessary ethylene glycol moieties;
(2) according to reaction condition, after above fritting reaction terminates, material is imported terminal polymerization kettle, progressively temperature in the kettle is improved from 235 DEG C of beginnings, stop heating when interior temperature reaches 265 DEG C, while intensification, slowly progressively improve vacuum in still and finally reach below absolute pressure 133Pa.Because polycondensation reaction belongs to exothermic reaction, and agitating friction heat-dissipating, reaction temperature can continue to raise.Interior temperature reaches 275 ± 2 DEG C, is polymerized under power of agitator 10KW condition, and the excessive ethylene glycol of residue removes by this process further, and then obtains the water-soluble polyurethane melt of FDY filament starching water-jet weaving;
(3) stop stirring, stop vacuumizing, with high pure nitrogen releasing vacuum is carried out to terminal polymerization kettle and pressurising to about 0.2MPa, open bottom valve, polymer be released in hopper and be cooled to solid material block;
(4) with strong crusher by material block be broken into diameter be less than 3mm Powdered after, test, measure, pack, finished product.
Adopt product prepared by above-mentioned technical process, vitrification point Tg is 61.5 DEG C, and powder does not stick together, and product appearance is faint yellow particle, solubility 27g, caused by the moisture content 0.17%(moisture absorption, lower same).
Get 15g product, together add in 500ml flask with 85ml running water and be heated to 95 DEG C and stir 30min, all dissolve, without insoluble matter, solution clarifies good brightness, and solution PH is 6.Gained polyester liquid (about 15%wt) viscosity (25 DEG C) is 6 ± 1mPa.S, 15% solution viscosity (95 DEG C) is 2 ± 0.5mPa.S, by the mass percent of having dissolved be 15% pulp solution be laid on PE film, be produce serous coat in the drying box of 80 DEG C at design temperature, the serous coat thickness produced is about 0.5mm, long 10cm, wide about 5cm, makes that serous coat elasticity after serous coat is strong, good film-forming property, is soaked in non-whitening in 60 DEG C of hot water, pliability is strong, is not clamminess.
Embodiment 2:
Component comprises:
Within waste and old Pillar recovery plastics 825kg(moisture content 6%),
Ethylene glycol 300kg(excessive more than 160%),
M-phthalic acid 50kg,
Dimethyl isophthalate-5-sodium sulfonate 150kg,
2,2-dimethyl-1,3 propylene glycol 50kg,
Polyglycol ether 4000 25kg,
Sodium acetate trihydrate 1kg,
Sb
2O
3150g，
Calcium acetate 500g.
Preparation method:
(1) waste and old Pillar recovery plastics are made fragment, in proportion by waste and old Pillar recovery plastic flakes, ethylene glycol, dimethyl isophthalate-5-sodium sulfonate, M-phthalic acid, 2,2-dimethyl-1,3 propylene glycol, Sb
2o
3, calcium acetate, Sodium acetate trihydrate mixing after put in fritting still, static normal pressure heats up, this process fritting still fractionation capital temperature incipient stage controls below 130 DEG C, between preferably 105 DEG C ± 3 DEG C, when in reaction, temperature reaches 235 DEG C ± 5 DEG C, the complete melting of material, distillate moisture or methyl alcohol when about reaching 90 ~ 100% of theoretical quantity of distillate, can judge that early stage has reacted, this process mainly carries out alcoholysis, ester exchange, esterification; In further rising, temperature is to 250-260 DEG C, improves fractionation capital temperature to about 180 DEG C, is distilled by unnecessary ethylene glycol moieties;
(2) according to reaction condition, after above fritting reaction terminates, material is imported terminal polymerization kettle, add polyglycol ether 4000 simultaneously, progressively temperature in the kettle is improved from 235 DEG C of beginnings, stop heating when interior temperature reaches 265 DEG C, while intensification, slowly progressively improve vacuum in still and finally reach below absolute pressure 133Pa.Because polycondensation reaction belongs to exothermic reaction, and agitating friction heat-dissipating, reaction temperature can continue to raise.Interior temperature reaches 275 ± 2 DEG C, is polymerized under power of agitator 10KW condition, and the excessive ethylene glycol of residue removes by this process further, and then obtains the water-soluble polyurethane melt of FDY filament starching water-jet weaving;
(3) stop stirring, stop vacuumizing, with high pure nitrogen releasing vacuum is carried out to terminal polymerization kettle and pressurising to about 0.2MPa, open bottom valve, polymer be released in hopper and be cooled to solid material block;
(4) with strong crusher by material block be broken into diameter be less than 3mm Powdered after, test, measure, pack, finished product.
Adopt product prepared by above-mentioned technical process, vitrification point Tg is 57.3 DEG C, and powder does not stick together, and product appearance is faint yellow particle, solubility 29g, moisture content 0.21%.
Get 15g product, together add in 500ml flask with 85ml running water and be heated to 95 DEG C and stir 30min, all dissolve, without insoluble matter, solution clarifies good brightness, and solution PH is 6.Gained polyester liquid (about 15%wt) viscosity (25 DEG C) is 6 ± 1mPa.S, 15% solution viscosity (95 DEG C) is 2 ± 0.5mPa.S, by the mass percent of having dissolved be 15% pulp solution be laid on PE film, be produce serous coat in the drying box of 80 DEG C at design temperature, the serous coat thickness produced is about 0.5mm, long 10cm, wide about 5cm, makes that serous coat elasticity after serous coat is strong, good film-forming property, is soaked in non-whitening in 60 DEG C of hot water, pliability is strong, is not clamminess.
Embodiment 3:
Component comprises:
Within waste and old Pillar recovery plastics 825kg(moisture content 6%),
Ethylene glycol 300kg(excessive more than 160%),
M-phthalic acid 40kg,
Sodium Dimethyl Isophthalate-5-sulfonate 125kg,
2-methyl isophthalic acid, 3 propylene glycol 60kg,
Anhydrous sodium acetate 1kg,
Sb
2O
330g，
Calcium acetate 500g.
Preparation method:
(1) waste and old Pillar recovery plastics are made fragment, in proportion by waste and old Pillar recovery plastic flakes, ethylene glycol, dimethyl isophthalate-5-sodium sulfonate, M-phthalic acid, 2-methyl isophthalic acid, 3 propylene glycol, Sb
2o
3, calcium acetate, anhydrous sodium acetate mixing after put in fritting still, static normal pressure heats up, this process fritting still fractionation capital temperature incipient stage controls below 130 DEG C, between preferably 105 DEG C ± 3 DEG C, when in reaction, temperature reaches 235 DEG C ± 5 DEG C, the complete melting of material, distillate moisture or methyl alcohol when about reaching 90 ~ 100% of theoretical quantity of distillate, can judge that early stage has reacted, this process mainly carries out alcoholysis, ester exchange, esterification; In further rising, temperature is to 250-260 DEG C, improves fractionation capital temperature to about 180 DEG C, is distilled by unnecessary ethylene glycol moieties;
(2) according to reaction condition, after above fritting reaction terminates, material is imported terminal polymerization kettle, progressively temperature in the kettle is improved from 235 DEG C of beginnings, stop heating when interior temperature reaches 265 DEG C, while intensification, slowly progressively improve vacuum in still and finally reach below absolute pressure 133Pa.Because polycondensation reaction belongs to exothermic reaction, and agitating friction heat-dissipating, reaction temperature can continue to raise.Interior temperature reaches 275 ± 2 DEG C, is polymerized under power of agitator 10KW condition, and the excessive ethylene glycol of residue removes by this process further, and then obtains the water-soluble polyurethane melt of FDY filament starching water-jet weaving;
(3) stop stirring, stop vacuumizing, with high pure nitrogen releasing vacuum is carried out to terminal polymerization kettle and pressurising to about 0.2MPa, open bottom valve, polymer be released in hopper and be cooled to solid material block;
(4) with strong crusher by material block be broken into diameter be less than 3mm Powdered after, test, measure, pack, finished product.
Adopt product prepared by above-mentioned technical process, vitrification point Tg is 59.1 DEG C, and powder does not stick together, and product appearance is faint yellow particle, solubility 26g, moisture content 0.16%.
Get 15g product, together add in 500ml flask with 85ml running water and be heated to 95 DEG C and stir 30min, all dissolve, without insoluble matter, solution clarifies good brightness, and solution PH is 6.Gained polyester liquid (about 15%wt) viscosity (25 DEG C) is 6 ± 1mPa.S, 15% solution viscosity (95 DEG C) is 2 ± 0.5mPa.S, by the mass percent of having dissolved be 15% pulp solution be laid on PE film, be produce serous coat in the drying box of 80 DEG C at design temperature, serous coat thickness about 0. 5mm produced, long 10cm, wide about 5cm, makes that serous coat elasticity after serous coat is strong, good film-forming property, is soaked in 60 DEG C of hot water and slightly turns white, pliability is strong, is not clamminess.
Embodiment 4:
Component comprises:
Within waste and old Pillar recovery plastics 825kg(moisture content 6%),
Ethylene glycol 280kg(excessive more than 130%),
M-phthalic acid 50kg,
5-sodium sulfo isophthalate 125kg,
2-methyl isophthalic acid, 3 propylene glycol 60kg,
Sb
2O
330g，
Sodium acetate trihydrate 500g,
Diglycol 50kg.
Preparation method:
(1) waste and old Pillar recovery plastics are made fragment, in proportion by waste and old Pillar recovery plastic flakes, ethylene glycol, 5-sodium sulfo isophthalate, M-phthalic acid, 2-methyl isophthalic acid, 3 propylene glycol, diglycol, Sb
2o
3, Sodium acetate trihydrate mixing after put in fritting still, static normal pressure heats up, this process fritting still fractionation capital temperature incipient stage controls below 130 DEG C, between preferably 105 DEG C ± 3 DEG C, when in reaction, temperature reaches 235 DEG C ± 5 DEG C, the complete melting of material, distillate moisture or methyl alcohol when about reaching 90 ~ 100% of theoretical quantity of distillate, can judge that early stage has reacted, this process mainly carries out alcoholysis, ester exchange, esterification; In further rising, temperature is to 250-260 DEG C, improves fractionation capital temperature to about 180 DEG C, is distilled by unnecessary ethylene glycol moieties;
(2) according to reaction condition, after above fritting reaction terminates, material is imported terminal polymerization kettle, progressively temperature in the kettle is improved from 235 DEG C of beginnings, stop heating when interior temperature reaches 265 DEG C, while intensification, slowly progressively improve vacuum in still and finally reach below absolute pressure 133Pa.Because polycondensation reaction belongs to exothermic reaction, and agitating friction heat-dissipating, reaction temperature can continue to raise.Interior temperature reaches 275 ± 2 DEG C, is polymerized under power of agitator 10KW condition, and the excessive ethylene glycol of residue removes by this process further, and then obtains the water-soluble polyurethane melt of FDY filament starching water-jet weaving;
(3) stop stirring, stop vacuumizing, with high pure nitrogen releasing vacuum is carried out to terminal polymerization kettle and pressurising to about 0.2MPa, open bottom valve, polymer be released in hopper and be cooled to solid material block;
(4) with strong crusher by material block be broken into diameter be less than 3mm Powdered after, test, measure, pack, finished product.
Adopt product prepared by above-mentioned technical process, vitrification point Tg is 56.7 DEG C, and powder does not stick together, and product appearance is faint yellow particle, solubility 28g, moisture content 0.19%.
Get 15g product, together add in 500ml flask with 85ml running water and be heated to 95 DEG C and stir 30min, all dissolve, without insoluble matter, solution clarifies good brightness, and solution PH is 6.Gained polyester liquid (about 15%wt) viscosity (25 DEG C) is 6 ± 1mPa.S, 15% solution viscosity (95 DEG C) is 2 ± 0.5mPa.S, by the mass percent of having dissolved be 15% pulp solution be laid on PE film, be produce serous coat in the drying box of 80 DEG C at design temperature, serous coat thickness about 0. 5mm produced, long 10cm, wide about 5cm, makes that serous coat elasticity after serous coat is strong, good film-forming property, is soaked in 60 DEG C of hot water and slightly turns white, pliability is strong, is not clamminess.
Embodiment 5:
Component comprises:
Within waste and old Pillar recovery plastics 825kg(moisture content 6%),
Ethylene glycol 280kg(excessive more than 130%),
M-phthalic acid 50kg,
Sodium Dimethyl Isophthalate-5-sulfonate 125kg,
2-methyl isophthalic acid, 3 propylene glycol 60kg,
Antimony glycol 60g,
Sodium acetate trihydrate 500g,
Zinc acetate 600g,
Diglycol 50kg.
Preparation method:
(1) waste and old Pillar recovery plastics are made fragment, in proportion by waste and old Pillar recovery plastic flakes, ethylene glycol, dimethyl isophthalate-5-sodium sulfonate, M-phthalic acid, 2-methyl isophthalic acid, 3 propylene glycol, diglycol, antimony glycol, zinc acetate, put in fritting still after Sodium acetate trihydrate mixing, static normal pressure heats up, this process fritting still fractionation capital temperature incipient stage controls below 130 DEG C, between preferably 105 DEG C ± 3 DEG C, when in reaction, temperature reaches 235 DEG C ± 5 DEG C, the complete melting of material, distillate moisture or methyl alcohol when about reaching 90 ~ 100% of theoretical quantity of distillate, can judge that early stage has reacted, this process mainly carries out alcoholysis, ester exchange, esterification, in further rising, temperature is to 250-260 DEG C, improves fractionation capital temperature to about 180 DEG C, is distilled by unnecessary ethylene glycol moieties,
(2) according to reaction condition, after above fritting reaction terminates, material is imported terminal polymerization kettle, progressively temperature in the kettle is improved from 235 DEG C of beginnings, stop heating when interior temperature reaches 265 DEG C, while intensification, slowly progressively improve vacuum in still and finally reach below absolute pressure 133Pa.Because polycondensation reaction belongs to exothermic reaction, and agitating friction heat-dissipating, reaction temperature can continue to raise.Interior temperature reaches 275 ± 2 DEG C, is polymerized under power of agitator 10KW condition, and the excessive ethylene glycol of residue removes by this process further, and then obtains the water-soluble polyurethane melt of FDY filament starching water-jet weaving;
(3) stop stirring, stop vacuumizing, with high pure nitrogen releasing vacuum is carried out to terminal polymerization kettle and pressurising to about 0.2MPa, open bottom valve, polymer be released in hopper and be cooled to solid material block;
(4) with strong crusher by material block be broken into diameter be less than 3mm Powdered after, test, measure, pack, finished product.
Adopt product prepared by above-mentioned technical process, vitrification point Tg is 58.5 DEG C, and powder does not stick together, and product appearance is faint yellow particle, solubility 29g, moisture content 0.16%.
Get 15g product, together add in 500ml flask with 85ml running water and be heated to 95 DEG C and stir 30min, all dissolve, without insoluble matter, solution clarifies good brightness, and solution PH is 6.Gained polyester liquid (about 15%wt) viscosity (25 DEG C) is 6 ± 1mPa.S, 15% solution viscosity (95 DEG C) is 2 ± 0.5mPa.S, by the mass percent of having dissolved be 15% pulp solution be laid on PE film, be produce serous coat in the drying box of 80 DEG C at design temperature, serous coat thickness about 0. 5mm produced, long 10cm, wide about 5cm, makes that serous coat elasticity after serous coat is strong, good film-forming property, is soaked in 60 DEG C of hot water and slightly turns white, pliability is strong, is not clamminess.
Embodiment 6:
Component comprises:
Within waste and old Pillar recovery plastics 825kg(moisture content 6%),
Ethylene glycol 280kg(excessive more than 130%),
M-phthalic acid 50kg,
M-phthalic acid binaryglycol ester-5-sodium sulfonate 125kg,
2-methyl isophthalic acid, 3 propylene glycol 60kg,
Antimony glycol 60g,
Sodium acetate trihydrate 500g,
Zinc acetate 600g,
Diglycol 50kg.
Preparation method:
(1) waste and old Pillar recovery plastics are made fragment, in proportion by waste and old Pillar recovery plastic flakes, ethylene glycol, M-phthalic acid binaryglycol ester-5-sodium sulfonate, M-phthalic acid, 2-methyl isophthalic acid, 3 propylene glycol, diglycol, antimony glycol, zinc acetate, put in fritting still after Sodium acetate trihydrate mixing, static normal pressure heats up, this process fritting still fractionation capital temperature incipient stage controls below 130 DEG C, between preferably 105 DEG C ± 3 DEG C, when in reaction, temperature reaches 235 DEG C ± 5 DEG C, the complete melting of material, distillate moisture or methyl alcohol when about reaching 90 ~ 100% of theoretical quantity of distillate, can judge that early stage has reacted, this process mainly carries out alcoholysis, ester exchange, esterification, in further rising, temperature is to 250-260 DEG C, improves fractionation capital temperature to about 180 DEG C, is distilled by unnecessary ethylene glycol moieties,
(2) according to reaction condition, after above fritting reaction terminates, material is imported terminal polymerization kettle, progressively temperature in the kettle is improved from 235 DEG C of beginnings, stop heating when interior temperature reaches 265 DEG C, while intensification, slowly progressively improve vacuum in still and finally reach below absolute pressure 133Pa.Because polycondensation reaction belongs to exothermic reaction, and agitating friction heat-dissipating, reaction temperature can continue to raise.Interior temperature reaches 275 ± 2 DEG C, is polymerized under power of agitator 10KW condition, and the excessive ethylene glycol of residue removes by this process further, and then obtains the water-soluble polyurethane melt of FDY filament starching water-jet weaving;
(3) stop stirring, stop vacuumizing, with high pure nitrogen releasing vacuum is carried out to terminal polymerization kettle and pressurising to about 0.2MPa, open bottom valve, polymer be released in hopper and be cooled to solid material block;
(4) with strong crusher by material block be broken into diameter be less than 3mm Powdered after, test, measure, pack, finished product.
Adopt product prepared by above-mentioned technical process, vitrification point Tg is 58.5 DEG C, and powder does not stick together, and product appearance is faint yellow particle, solubility 29g, moisture content 0.16%.
Get 15g product, together add in 500ml flask with 85ml running water and be heated to 95 DEG C and stir 30min, all dissolve, without insoluble matter, solution clarifies good brightness, and solution PH is 6.Gained polyester liquid (about 15%wt) viscosity (25 DEG C) is 6 ± 1mPa.S, 15% solution viscosity (95 DEG C) is 2 ± 0.5mPa.S, by the mass percent of having dissolved be 15% pulp solution be laid on PE film, be produce serous coat in the drying box of 80 DEG C at design temperature, serous coat thickness about 0. 5mm produced, long 10cm, wide about 5cm, makes that serous coat elasticity after serous coat is strong, good film-forming property, is soaked in 60 DEG C of hot water and slightly turns white, pliability is strong, is not clamminess.
FDY fiber is the synthetic fiber filament adopting spin-drawing one step obtained, and fiber is fully orientation stretching sizing, can be directly used in textile process.Feature: the smooth softness of feel, twist with the fingers point few, yarn, between monofilament, cohesive force is little, is similar to parastate, and gloss is dazzle the eyes, and is the kind that in polyster fibre, output is maximum, is often used in and weaves silk-like fabric.According to this feature, in weaving process, yarn breakage causes stopping, and starching makes mutual obvolvent between yarn monofilament, according to the principle of " similar mix ", can reach better cohesive force with polyester material.Water jet looms relies on water stream to complete wefting insertion in addition, water stream can cause organizine and the Fabric wettability of shed open near region, if slurry is not water-fast or moisture absorption is glued again, grey cloth flaw or degradation will be caused, the good water solubility when slurry synthesized by the present invention can perfect reach with slurry, can the requirement of thorough destarch when water-fast heatproof, destarch when weaving.
Key point of the present invention is: 1), adopt Pillar recovery to prepare the water-soluble environment protective polyester pulp of FDY filament starching water-jet weaving; 2), alcoholysis, ester exchange, esterification one step complete; 3), adopt other dihydroxylic alcohols, reach FDY starching, weave, move back dye links particular/special requirement.
The present invention adopts Pillar recovery one-step method to prepare FDY filament slurry, and while reducing costs, production efficiency also significantly improves.
Claims (8)
1. a FDY filament starching water-jet weaving water-soluble polyurethane, is characterized in that: be by Pillar recovery, the ethylene glycol accounting for Pillar recovery weight ratio 5 ~ 10% and following component
A, account for Pillar recovery weight ratio 10 ~ 20% M-phthalic acid-5-sulfonate or derivatives thereof,
B, account for Pillar recovery weight ratio 3 ~ 15% M-phthalic acid,
C, account for Pillar recovery weight ratio 5 ~ 10% other dihydroxylic alcohols,
D, account for Pillar recovery weight ratio 0.03 ~ 0.15% catalyst,
E, account for Pillar recovery weight ratio 0.02 ~ 0.1% inorganic assistant,
F, account for the polyethers of the weight average molecular weight 600 ~ 10000 of Pillar recovery weight ratio 0 ~ 5%,
Obtain through alcoholysis, copolymerization, cooling, fragmentation.
2. a kind of FDY filament starching water-jet weaving water-soluble polyurethane according to claim 1, is characterized in that: described M-phthalic acid-5-sulfonate or derivatives thereof is selected from M-phthalic acid-5-sodium sulfonate (SSIPA), dimethyl isophthalate-5-sodium sulfonate or M-phthalic acid-5-sodium sulfonate glycol ester (SIPE).
3. a kind of FDY filament starching water-jet weaving water-soluble polyurethane according to claim 1 and 2, is characterized in that: other described dihydroxylic alcohols is selected from diglycol, 2-methyl isophthalic acid, 3 propylene glycol, 2,2-dimethyl-1,3 propylene glycol.
4. a kind of FDY filament starching water-jet weaving water-soluble polyurethane according to claim 1 and 2, it is characterized in that: described catalyst comprises polyester catalyst and/or ester exchange catalyst, polyester catalyst is selected from antimonous oxide or antimony glycol, and ester exchange catalyst is selected from zinc acetate or calcium acetate; Described inorganic assistant adopts anti-ether agent, and anti-ether agent is selected from anhydrous sodium acetate or Sodium acetate trihydrate.
5. a kind of FDY filament starching water-jet weaving water-soluble polyurethane according to claim 1 and 2, is characterized in that: described polyethers is Macrogol 4000.
6. prepare a method for FDY filament starching water-jet weaving water-soluble polyurethane described in claim 1, it is characterized in that comprising following four steps:
(1) Pillar recovery is made fragment, in proportion by Pillar recovery fragment, ethylene glycol, M-phthalic acid-5-sulfonate or derivatives thereof, M-phthalic acid, other dihydroxylic alcohols, put in fritting still after catalyst and inorganic assistant mixing, static normal pressure heats up, this process fritting still fractionation capital temperature incipient stage controls below 130 DEG C, between preferably 105 DEG C ± 3 DEG C, when in reaction, temperature reaches 235 DEG C ± 5 DEG C, the complete melting of material, distillate moisture or methyl alcohol when about reaching 90 ~ 100% of theoretical quantity of distillate, can judge that early stage has reacted, this process mainly carries out alcoholysis, ester exchange, esterification, in further rising, temperature is to 250-260 DEG C, improves fractionation capital temperature to about 180 DEG C, is distilled by unnecessary ethylene glycol moieties,
(2) according to reaction condition, after above fritting reaction terminates, material is imported terminal polymerization kettle, add polyethers simultaneously, progressively temperature in the kettle is improved from 235 DEG C of beginnings, stop heating when interior temperature reaches 265 DEG C, while intensification, slowly progressively improve vacuum in still and finally reach below absolute pressure 133Pa; Interior temperature reaches 275 ± 2 DEG C, is polymerized under power of agitator 10KW condition, and the excessive ethylene glycol of residue removes by this process further, and then obtains the water-soluble polyurethane melt of FDY filament starching water-jet weaving;
(3) stop stirring, stop vacuumizing, with high pure nitrogen releasing vacuum is carried out to terminal polymerization kettle and pressurising to about 0.2MPa, open bottom valve, polymer be released in hopper and be cooled to solid material block;
(4) with strong crusher material block is broken into Powdered after, test, measure, pack, finished product.
7. a kind of method preparing FDY filament starching water-jet weaving water-soluble polyurethane described in claim 1 according to claim 6, is characterized in that: the inorganic assistant in (1) described step is anti-ether agent.
8. a kind of method preparing FDY filament starching water-jet weaving water-soluble polyurethane described in claim 1 according to claim 7, is characterized in that: the described M-phthalic acid-5-sulfonate or derivatives thereof described in (1) step is selected from M-phthalic acid-5-sodium sulfonate (SSIPA), dimethyl isophthalate-5-sodium sulfonate or M-phthalic acid-5-sodium sulfonate glycol ester (SIPE); Other described dihydroxylic alcohols is selected from diglycol, 2-methyl isophthalic acid, 3 propylene glycol, 2,2-dimethyl-1,3 propylene glycol; Described catalyst comprises polymerization catalyst and/or ester exchange catalyst, and polymerization catalyst is selected from antimonous oxide or antimony glycol, and ester exchange catalyst is selected from zinc acetate or calcium acetate; Described anti-ether agent adopts anhydrous sodium acetate or Sodium acetate trihydrate; Polyethers described in (2) step is selected from polyethylene glycol.
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| CN112812284A (en) * | 2020-12-30 | 2021-05-18 | 湖北山特莱新材料有限公司 | Water-soluble slurry capable of being desized quickly |
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| CN113045740A (en) * | 2021-03-18 | 2021-06-29 | 湖北山特莱新材料有限公司 | Preparation method of cyclic regeneration type water-soluble polyester chip |
| CN113174035A (en) * | 2021-05-08 | 2021-07-27 | 湖北山特莱新材料有限公司 | Multifunctional water-soluble polyester slurry |
| CN114481413A (en) * | 2021-12-23 | 2022-05-13 | 吴江余宏织造有限公司 | Weaving method of high-bulkiness chemical fiber cloth and high-bulkiness chemical fiber cloth |
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| CN114481413A (en) * | 2021-12-23 | 2022-05-13 | 吴江余宏织造有限公司 | Weaving method of high-bulkiness chemical fiber cloth and high-bulkiness chemical fiber cloth |
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| CN104988733B (en) | 2017-07-14 |
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Denomination of invention: FDY filament sizing and water jet weaving water-soluble polyester size and its preparation method Effective date of registration: 20230404 Granted publication date: 20170714 Pledgee: Industrial Bank Co.,Ltd. Xiangyang Branch Pledgor: Hubei Santak New Material Co.,Ltd. Registration number: Y2023420000147 |