CN104988733B - FDY filament starching water-jet weaving water-soluble polyurethane and preparation method thereof - Google Patents
FDY filament starching water-jet weaving water-soluble polyurethane and preparation method thereof Download PDFInfo
- Publication number
- CN104988733B CN104988733B CN201510453115.0A CN201510453115A CN104988733B CN 104988733 B CN104988733 B CN 104988733B CN 201510453115 A CN201510453115 A CN 201510453115A CN 104988733 B CN104988733 B CN 104988733B
- Authority
- CN
- China
- Prior art keywords
- water
- kettle
- ethylene glycol
- phthalic acid
- soluble polyurethane
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 238000009941 weaving Methods 0.000 title claims abstract description 41
- 229920002635 polyurethane Polymers 0.000 title claims abstract description 38
- 239000004814 polyurethane Substances 0.000 title claims abstract description 38
- 238000009955 starching Methods 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title abstract description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 150
- 238000011084 recovery Methods 0.000 claims abstract description 52
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229920000728 polyester Polymers 0.000 claims abstract description 31
- 239000003054 catalyst Substances 0.000 claims abstract description 23
- 238000006136 alcoholysis reaction Methods 0.000 claims abstract description 19
- 150000001298 alcohols Chemical class 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 238000007334 copolymerization reaction Methods 0.000 claims abstract description 10
- 229920000570 polyether Polymers 0.000 claims abstract description 10
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 144
- 238000006243 chemical reaction Methods 0.000 claims description 57
- 238000000034 method Methods 0.000 claims description 48
- 238000006116 polymerization reaction Methods 0.000 claims description 36
- 238000010438 heat treatment Methods 0.000 claims description 34
- 239000011734 sodium Substances 0.000 claims description 30
- 229910052708 sodium Inorganic materials 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 29
- 229920003023 plastic Polymers 0.000 claims description 28
- 239000004033 plastic Substances 0.000 claims description 28
- 239000002699 waste material Substances 0.000 claims description 28
- 150000002148 esters Chemical class 0.000 claims description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- 238000005194 fractionation Methods 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 19
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 claims description 18
- AIDLAEPHWROGFI-UHFFFAOYSA-N 2-methylbenzene-1,3-dicarboxylic acid Chemical class CC1=C(C(O)=O)C=CC=C1C(O)=O AIDLAEPHWROGFI-UHFFFAOYSA-N 0.000 claims description 17
- 239000012634 fragment Substances 0.000 claims description 16
- 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 15
- 235000017281 sodium acetate Nutrition 0.000 claims description 15
- 229940087562 sodium acetate trihydrate Drugs 0.000 claims description 15
- 239000002002 slurry Substances 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 229920000642 polymer Polymers 0.000 claims description 12
- 239000011343 solid material Substances 0.000 claims description 12
- 230000003068 static effect Effects 0.000 claims description 12
- 229940040526 anhydrous sodium acetate Drugs 0.000 claims description 10
- 229910052787 antimony Inorganic materials 0.000 claims description 10
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical group [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 10
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical class OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 claims description 10
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 9
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical group [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 8
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical group [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 8
- 239000001639 calcium acetate Substances 0.000 claims description 8
- 235000011092 calcium acetate Nutrition 0.000 claims description 8
- 229960005147 calcium acetate Drugs 0.000 claims description 8
- 238000012360 testing method Methods 0.000 claims description 8
- 239000004246 zinc acetate Substances 0.000 claims description 8
- 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 claims description 7
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Inorganic materials O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 7
- 230000032050 esterification Effects 0.000 claims description 7
- 238000005886 esterification reaction Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 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 claims description 5
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 229910000410 antimony oxide Inorganic materials 0.000 claims description 4
- 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 4
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical group [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 claims description 4
- 239000002685 polymerization catalyst Substances 0.000 claims description 4
- NEOGGGHDLGYATP-UHFFFAOYSA-N 1,6-dimethylimidazo[4,5-b]pyridin-2-amine Chemical compound CC1=CN=C2N=C(N)N(C)C2=C1 NEOGGGHDLGYATP-UHFFFAOYSA-N 0.000 claims description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- HFNUUHLSQPLBQI-UHFFFAOYSA-N acetic acid;calcium Chemical compound [Ca].CC(O)=O HFNUUHLSQPLBQI-UHFFFAOYSA-N 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- YEAUATLBSVJFOY-UHFFFAOYSA-N tetraantimony hexaoxide Chemical compound O1[Sb](O2)O[Sb]3O[Sb]1O[Sb]2O3 YEAUATLBSVJFOY-UHFFFAOYSA-N 0.000 claims description 2
- 239000000052 vinegar Substances 0.000 claims description 2
- 235000021419 vinegar Nutrition 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- LZDKZFUFMNSQCJ-UHFFFAOYSA-N 1,2-diethoxyethane Chemical compound CCOCCOCC LZDKZFUFMNSQCJ-UHFFFAOYSA-N 0.000 claims 2
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims 1
- 238000002844 melting Methods 0.000 claims 1
- 230000008018 melting Effects 0.000 claims 1
- 230000009477 glass transition Effects 0.000 abstract description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 8
- 238000010521 absorption reaction Methods 0.000 abstract description 5
- 239000000835 fiber Substances 0.000 abstract description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 abstract description 4
- 229910021529 ammonia Inorganic materials 0.000 abstract description 4
- 239000007787 solid Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 abstract description 3
- 230000003301 hydrolyzing effect Effects 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 26
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 18
- 238000006068 polycondensation reaction Methods 0.000 description 7
- 239000004698 Polyethylene Substances 0.000 description 6
- 238000013461 design Methods 0.000 description 6
- 238000009990 desizing Methods 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 238000009738 saturating Methods 0.000 description 6
- 230000000630 rising effect Effects 0.000 description 5
- 239000004744 fabric Substances 0.000 description 4
- 238000004513 sizing Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 229920001634 Copolyester Polymers 0.000 description 2
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture 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
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical class CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- KQNKJJBFUFKYFX-UHFFFAOYSA-N acetic acid;trihydrate Chemical compound O.O.O.CC(O)=O KQNKJJBFUFKYFX-UHFFFAOYSA-N 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
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000001934 delay Effects 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
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000008233 hard water Substances 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- 229920000151 polyglycol Polymers 0.000 description 1
- 239000010695 polyglycol Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 235000013772 propylene glycol Nutrition 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 239000002195 soluble material Substances 0.000 description 1
- 239000007921 spray 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
- 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
Landscapes
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
Entitled FDY filament starching water-jet weaving water-soluble polyurethane of the present invention and preparation method thereof.Belong to water-soluble polyurethane technical field.It is mainly the existing acrylic size of solution there are problems that product solid content there was only that 30% or so, cost of transportation is high, environmental pollution is big, moisture absorption stick again it is serious, to the adhesion of hydrophobicity polyester fiber.It is mainly characterized by：Be by Pillar recovery, ethylene glycol, the sulfonate of M-phthalic acid 5 or derivatives thereof, M-phthalic acid, other dihydric alcohols, catalyst, inorganic assistant, weight average molecular weight 600~10000 polyethers through alcoholysis, copolymerization, cooling, broken be made.The present invention, which has, improves product glass transition temperature, and excellent chemical stability, hydrolytic resistance and heat endurance, convenient storing do not have the characteristics of ammonia is added and disengaged, is mainly used in the preparation of FDY filament starching water-jet weaving water-soluble polyurethane during use.
Description
Technical field
The invention belongs to water-soluble polyurethane technical field, and in particular to one kind is used for FDY filament starching water-jet weaving
Water-soluble environment protective polyester pulp and preparation method thereof.
Background technology
Water-jet loom it is woven it is technical bring preferable economy, as a kind of shuttleless loom of high speed, in the present age
Vigorous vitality is shown in textile industry.At the same time, the development of Water-Jet Weaving Size, Water-Jet Weaving Size have also been expedited the emergence of
Different from conventional slurry, it will meet following characteristics：Soluble in water when sizing mixing, serous coat is water-fast during weaving, and slurry is again during desizing
It is easily removed.
Conventional Water-Jet Weaving Size is acrylic size at present, and this kind of slurry is in initiator by acrylicacidandesters
Polymerisation in solution is used under effect, then by carboxyl saponification in copolyesters, makes slurry that there is water solubility., can when being thickened with ammoniacal liquor
Using ammonia in high temperature volatile feature, the requirements of weaving process of water resistance is made.During desizing, alkali lye boiling-off is used, serous coat becomes can
Water-soluble acrylates, so as to complete desizing.
Acrylic size has the following disadvantages in production, storing and post processing：1st, used in producing a large amount of to environment
And human body has the ammonia of considerable influence；2nd, product solid content only has 30% or so, and to storing limited requirement, cost of transportation is high；3rd, move back
Pulp waste is difficult to biodegradation；4th, Acrylates are little to the adhesion of hydrophobicity polyester fiber.
Chinese patent CN1333792 " sulfonic polyester based on terephthalate " is related to comprising difunctional sulfomonomer
It is used as slurry with the water dispersible sulfonic polyester of polyethylene glycol.CN1834131 " water-soluable sizing material polyester and preparation method " is proposed
Inorganic salts are added when preparing water-soluable sizing material polyester, the polyester pulp of preparation can be used in hard water.CN101955581A
" waste and old polyester plastics prepare water-soluble polyurethane and preparation method thereof " propose by waste and old polyester fragment, 1,2- propane diols,
Diglycol, water system polyester improver, compound stabilizer and catalyst prepare water-soluble poly in same reactor one-step method
Ester slurry.CN102161751A " a kind of production method of polyester pulp " directly uses reaction material ethylene glycol terephthalate
BHET, M-phthalic acid -5- sodium sulfonates SIPA, diglycol DEG etc. prepare polyester pulp.CN101967225A " water
The preparation method of dissolubility sulfo-copolyester " proposes the polyethylene glycols raw material without using costliness when producing polyester, while using
Relatively low dihydric alcohol and the mol ratio of binary acid（1: 1.3~1: 1.8)）It is suitable to deposit to obtain higher glass transition temperature
Storage.
In the prior art acrylic size as described above, shortcoming clearly, slurry with water dissolubility polyester is still deposited in addition
In problems with：（1）Product still has the moisture absorption of any sticky again, influences water-jet weaving, can cause product viscous simultaneously when serious；
(2), may when serious to prevent that adhesion, it is necessary to reduce the content of hydrophilic radical, may influence the water solubility of product again for moisture absorption
Desizing can be caused not thorough, fabric quality is influenceed.
The content of the invention
The purpose of the present invention is to be starched for above-mentioned deficiency there is provided a kind of FDY filament starching water-jet weaving with water-soluble polyester
The preparation method of material, prepared water-soluble polyurethane, which has, both meets water-soluble requirement, disclosure satisfy that again under hot conditions
Storage and the leasing of silk are starched, chemical stability is excellent, the characteristics of facilitating storing, 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 is water-soluble
Polyester pulp, it is characterised in that：It is by Pillar recovery, accounts for ethylene glycol of the Pillar recovery weight than 5~10% and following components
A, account for the M-phthalic acid -5- sulfonate of Pillar recovery weight than 10~20% or derivatives thereof,
B, account for M-phthalic acid of the Pillar recovery weight than 3~15%,
C, account for other dihydric alcohols of the Pillar recovery weight than 5~10%,
D, account for catalyst of the Pillar recovery weight than 0.03~0.15%,
E, account for inorganic assistant of the Pillar recovery weight than 0.02~0.1%,
F, the polyethers for accounting for weight average molecular weight 600~10000 of the Pillar recovery weight than 0~5%,
Through alcoholysis, copolymerization, cooling, broken it is made.
M-phthalic acid -5- sulfonate described in the technical solution of the present invention or derivatives thereof is selected from isophthalic two
Formic acid -5- sodium sulfonates（SSIPA）, DMIP -5- sodium sulfonates or M-phthalic acid binaryglycol ester -5- sulfonic acid
Sodium（SIPE）.
The present invention technical solution described in other dihydric alcohols in addition to ethylene glycol be selected from diglycol,
2- methyl isophthalic acids, 3 propane diols, 2,2- dimethyl -1,3 propane diols.
Catalyst described in the technical solution of the present invention includes polyester catalyst and/or ester exchange catalyst, gathers
Ester catalyst is selected from antimony oxide or antimony glycol, and ester exchange catalyst is selected from zinc acetate or calcium acetate；It is described without machine aided
Agent uses anti-ether agent, and anti-ether agent is selected from anhydrous sodium acetate or Sodium acetate trihydrate.
Polyethers described in the technical solution of the present invention is Macrogol 4000.
The present invention prepares the technical solution of above-mentioned water-soluble polyurethane method：A kind of FDY filament starching water spray
The preparation method of weaving water-soluble polyurethane, it is characterised in that including following four step：
（1）Fragment is made in Pillar recovery, in proportion by Pillar recovery fragment, ethylene glycol, M-phthalic acid -5- sulfonate
Or derivatives thereof, put into fritting kettle after M-phthalic acid, other dihydric alcohols, catalyst and inorganic assistant mixing, it is static often
Pressure heating, the fractionation capital temperature incipient stage control of this process fritting kettle is below 130 DEG C, between preferably 105 DEG C ± 3 DEG C, when
Temperature reaches 235 DEG C ± 5 DEG C in reaction, and material is melted completely, distillates moisture or methanol about reach theoretical quantity of distillate 90~100%
When, early stage reaction completion is can determine whether, this process is substantially carried out alcoholysis, ester exchange, esterification；Further temperature arrives 250- in rise
260 DEG C, fractionation capital temperature is improved to 180 DEG C or so, unnecessary ethylene glycol moieties are distilled；
（2）According to reaction condition, after above fritting reaction terminates, material is imported into terminal polymerization kettle, while polyethers is added, from
235 DEG C start to step up temperature in the kettle, stop heating when interior temperature reaches 265 DEG C, while heating, slowly step up
Vacuum and below absolute pressure 133Pa is finally reached in kettle；Because polycondensation reaction belongs to exothermic reaction, and agitating friction is given birth to
Heat, reaction temperature may proceed to rise；Interior temperature reaches polymerization under the conditions of 275 ± 2 DEG C, power of agitator 10KW, and this process is by remaining mistake
The ethylene glycol of amount is further removed, and then obtains the water-soluble polyurethane melt of FDY filament starching water-jet weaving；
（3）Stop stirring, stop vacuumizing, terminal polymerization kettle is carried out releasing vacuum with high pure nitrogen and pressurising is left to 0.2MPa
The right side, opens bottom valve, polymer is released in hopper and is cooled to solid material block；
（4）With strong crusher will expect block crush it is powdered after, test, measure, pack, finished product.
The present invention is prepared the in the method for FDY filament starching water-jet weaving water-soluble polyurethane（1）Nothing in step
Machine aided agent is anti-ether agent.
The present invention is prepared the in the method for FDY filament starching water-jet weaving water-soluble polyurethane（1）Described in step
M-phthalic acid -5- sulfonate or derivatives thereof be selected from M-phthalic acid -5- sodium sulfonates（SSIPA）, M-phthalic acid two
Methyl esters -5- sodium sulfonates or M-phthalic acid -5- sodium sulfonates glycol ester (SIPE)；Described other dihydric alcohols are selected from a contracting two
Ethylene glycol, 2- methyl isophthalic acids, 3 propane diols, 2,2- dimethyl -1,3 propane diols；Described catalyst include polymerization catalyst and/or
Ester exchange catalyst, polymerization catalyst is selected from antimony oxide or antimony glycol, and ester exchange catalyst is selected from zinc acetate or acetic acid
Calcium；Described anti-ether agent uses anhydrous sodium acetate or Sodium acetate trihydrate；The（2）Polyethers described in step is selected from polyethylene glycol.
The present invention uses the larger dihydric alcohol of steric hindrance as comonomer, with advantages below：1st, water-soluble list is not being reduced
The glass transition temperature of product is improved on the basis of body, product had both been met water-soluble requirement, disclosure satisfy that again under hot conditions
Starch storage and the leasing of silk；2nd, because the special construction of the larger dihydric alcohol of steric hindrance is there is provided the chemical stability of product fine,
Hydrolytic resistance and heat endurance, further ensure that water resistance of the slurry silk during water-jet weaving；3rd, using thermoplastic poly
Ester solid, water soluble material, convenient storing, without wrap pages to be reclaimed, reduces storing cost and integrated cost；4th, using
Cheng Zhong, addition without ammonia and disengages, meet the requirement of environmental protection, reduces the actual bodily harm to operating employee.
Present invention is mainly used for the preparation of FDY filament starching water-jet weaving water-soluble polyurethane.
Embodiment
Below by embodiment, the present invention will be further described.
Embodiment 1：
Component includes：
Waste and old Pillar recovery plastics 825kg（Within moisture content 6%）、
Ethylene glycol 320kg（Excessive more than 200%）、
M-phthalic acid 50kg,
5-sodium sulfo isophthalate 125kg,
2,2- dimethyl -1,3 propane diols 50kg,
Anhydrous sodium acetate 1kg,
Sb2O3 120g。
Preparation method：
（1）Fragment is made in waste and old Pillar recovery plastics, in proportion by waste and old Pillar recovery plastic flakes, ethylene glycol,
Phthalic acid -5- sodium sulfonates, M-phthalic acid, 2,2- dimethyl -1,3 propane diols, anhydrous sodium acetate, Sb2O3Put into after mixing
In fritting kettle, static normal pressure heating, the fractionation capital temperature incipient stage control of this process fritting kettle is below 130 DEG C, and preferably 105
Between DEG C ± 3 DEG C, when temperature reaches 235 DEG C ± 5 DEG C in reaction, material is melted completely, is distillated moisture or methanol and is about reached that theory evaporates
Output 90~100% when, can determine whether early stage reaction completion, this process is substantially carried out alcoholysis, ester exchange, esterification；Further
Temperature arrives 250-260 DEG C in rise, improves fractionation capital temperature to 180 DEG C or so, unnecessary ethylene glycol moieties are distilled；
（2）According to reaction condition, after above fritting reaction terminates, material is imported into terminal polymerization kettle, progressively carried since 235 DEG C
High temperature in the kettle, stops heating when interior temperature reaches 265 DEG C, while heating, slowly steps up in kettle vacuum and most
Below absolute pressure 133Pa is reached eventually.Because polycondensation reaction belongs to exothermic reaction, and agitating friction heat, reaction temperature can be after
Height of continuing rising.Interior temperature reaches polymerization under the conditions of 275 ± 2 DEG C, power of agitator 10KW, and this process is further by remaining excessive ethylene glycol
Removing, and then obtain the water-soluble polyurethane melt of FDY filament starching water-jet weaving；
（3）Stop stirring, stop vacuumizing, terminal polymerization kettle is carried out releasing vacuum with high pure nitrogen and pressurising is left to 0.2MPa
The right side, opens bottom valve, polymer is released in hopper and is cooled to solid material block；
（4）With strong crusher by expect block be broken into diameter less than 3mm it is powdered after, test, measure, pack,
Finished product.
The product prepared using above-mentioned technical process, glass transition temperature Tg is 61.5 DEG C, and powder does not stick together, outside product
See as yellowish coloured particles, solubility 27g, moisture content 0.17%（Caused by the moisture absorption, similarly hereinafter）.
15g products are taken, is together added with 85ml running water and 95 DEG C of stirring 30min is heated in 500ml flasks, whole is molten
Solution, no insoluble matter, solution clarifies saturating good brightness, and solution PH is 6.Gained polyester liquid（About 15%wt）Viscosity（25℃）For 6 ±
1mPa.S, 15% solution viscosity（95℃）For 2 ± 0.5mPa.S, the mass percent dissolved is tiled for 15% pulp solution
On PE films, serous coat is produced in design temperature is 80 DEG C of drying box, serous coat thickness about 0.5mm, the long 10cm produced is wide
About 5cm, is made the elastic strong, good film-forming property of serous coat after serous coat, is soaked in non-whitening in 60 DEG C of hot water, pliability is strong, not tacky.
Embodiment 2：
Component includes：
Waste and old Pillar recovery plastics 825kg（Within moisture content 6%）,
Ethylene glycol 300kg（Excessive more than 160%）,
M-phthalic acid 50kg,
DMIP -5- sodium sulfonate 150kg,
2,2- dimethyl -1,3 propane diols 50kg,
The 25kg of polyglycol ether 4000,
Sodium acetate trihydrate 1kg,
Sb2O3150g,
Calcium acetate 500g.
Preparation method：
（1）Fragment is made in waste and old Pillar recovery plastics, in proportion by waste and old Pillar recovery plastic flakes, ethylene glycol,
Rutgers -5- sodium sulfonates, M-phthalic acid, 2,2- dimethyl -1,3 propane diols, Sb2O3, calcium acetate, acetate trihydrate
Put into after sodium mixing in fritting kettle, static normal pressure heating, the fractionation capital temperature incipient stage control of this process fritting kettle is at 130 DEG C
Hereinafter, between preferably 105 DEG C ± 3 DEG C, when temperature reaches 235 DEG C ± 5 DEG C in reaction, material is melted completely, distillates moisture or first
When alcohol about reaches the 90~100% of theoretical quantity of distillate, can determine whether early stage reaction completion, this process be substantially carried out alcoholysis, ester exchange,
Esterification；Further temperature arrives 250-260 DEG C in rise, fractionation capital temperature is improved to 180 DEG C or so, by unnecessary ethylene glycol portion
Divide and distill；
（2）According to reaction condition, after above fritting reaction terminates, material is imported into terminal polymerization kettle, while adding polyethylene glycol
Ether 4000, steps up temperature in the kettle since 235 DEG C, stops heating when interior temperature reaches 265 DEG C, while heating, delays
It is slow to step up in kettle vacuum and be finally reached below absolute pressure 133Pa.Because polycondensation reaction belongs to exothermic reaction, and stir
Frictional heat is mixed, reaction temperature may proceed to rise.Interior temperature reaches polymerization, this process under the conditions of 275 ± 2 DEG C, power of agitator 10KW
Remaining excessive ethylene glycol is further removed, and then obtains the water-soluble polyurethane melt of FDY filament starching water-jet weaving；
（3）Stop stirring, stop vacuumizing, terminal polymerization kettle is carried out releasing vacuum with high pure nitrogen and pressurising is left to 0.2MPa
The right side, opens bottom valve, polymer is released in hopper and is cooled to solid material block；
（4）With strong crusher by expect block be broken into diameter less than 3mm it is powdered after, test, measure, pack,
Finished product.
The product prepared using above-mentioned technical process, glass transition temperature Tg is 57.3 DEG C, and powder does not stick together, outside product
See as yellowish coloured particles, solubility 29g, moisture content 0.21%.
15g products are taken, is together added with 85ml running water and 95 DEG C of stirring 30min is heated in 500ml flasks, whole is molten
Solution, no insoluble matter, solution clarifies saturating good brightness, and solution PH is 6.Gained polyester liquid（About 15%wt）Viscosity（25℃）For 6 ±
1mPa.S, 15% solution viscosity（95℃）For 2 ± 0.5mPa.S, the mass percent dissolved is tiled for 15% pulp solution
On PE films, serous coat is produced in design temperature is 80 DEG C of drying box, serous coat thickness about 0.5mm, the long 10cm produced is wide
About 5cm, is made the elastic strong, good film-forming property of serous coat after serous coat, is soaked in non-whitening in 60 DEG C of hot water, pliability is strong, not tacky.
Embodiment 3：
Component includes：
Waste and old Pillar recovery plastics 825kg（Within moisture content 6%）,
Ethylene glycol 300kg（Excessive more than 160%）,
M-phthalic acid 40kg,
Sodium Dimethyl Isophthalate-5-sulfonate 125kg,
2- methyl isophthalic acids, 3 propane diols 60kg,
Anhydrous sodium acetate 1kg,
Sb2O330g,
Calcium acetate 500g.
Preparation method：
（1）Fragment is made in waste and old Pillar recovery plastics, in proportion by waste and old Pillar recovery plastic flakes, ethylene glycol,
Rutgers -5- sodium sulfonates, M-phthalic acid, 2- methyl isophthalic acids, 3 propane diols, Sb2O3, calcium acetate, anhydrous sodium acetate mix
Put into after conjunction in fritting kettle, the heating of static normal pressure, this process fritting kettle fractionation capital temperature incipient stage control 130 DEG C with
Under, between preferably 105 DEG C ± 3 DEG C, when temperature reaches 235 DEG C ± 5 DEG C in reaction, material is melted completely, distillates moisture or methanol
When about reaching the 90~100% of theoretical quantity of distillate, early stage reaction completion is can determine whether, this process is substantially carried out alcoholysis, ester exchange, ester
Change reaction；Further temperature arrives 250-260 DEG C in rise, fractionation capital temperature is improved to 180 DEG C or so, by unnecessary ethylene glycol moieties
Distill；
（2）According to reaction condition, after above fritting reaction terminates, material is imported into terminal polymerization kettle, progressively carried since 235 DEG C
High temperature in the kettle, stops heating when interior temperature reaches 265 DEG C, while heating, slowly steps up in kettle vacuum and most
Below absolute pressure 133Pa is reached eventually.Because polycondensation reaction belongs to exothermic reaction, and agitating friction heat, reaction temperature can be after
Height of continuing rising.Interior temperature reaches polymerization under the conditions of 275 ± 2 DEG C, power of agitator 10KW, and this process is further by remaining excessive ethylene glycol
Removing, and then obtain the water-soluble polyurethane melt of FDY filament starching water-jet weaving；
（3）Stop stirring, stop vacuumizing, terminal polymerization kettle is carried out releasing vacuum with high pure nitrogen and pressurising is left to 0.2MPa
The right side, opens bottom valve, polymer is released in hopper and is cooled to solid material block；
（4）With strong crusher by expect block be broken into diameter less than 3mm it is powdered after, test, measure, pack,
Finished product.
The product prepared using above-mentioned technical process, glass transition temperature Tg is 59.1 DEG C, and powder does not stick together, outside product
See as yellowish coloured particles, solubility 26g, moisture content 0.16%.
15g products are taken, is together added with 85ml running water and 95 DEG C of stirring 30min is heated in 500ml flasks, whole is molten
Solution, no insoluble matter, solution clarifies saturating good brightness, and solution PH is 6.Gained polyester liquid（About 15%wt）Viscosity（25℃）For 6 ±
1mPa.S, 15% solution viscosity（95℃）For 2 ± 0.5mPa.S, the mass percent dissolved is tiled for 15% pulp solution
On PE films, serous coat is produced in design temperature is 80 DEG C of drying box, serous coat thickness about 0. 5mm, the long 10cm produced,
Width about 5cm, is made the elastic strong, good film-forming property of serous coat after serous coat, is soaked in 60 DEG C of hot water and turns white slightly, pliability is strong, does not send out
It is viscous.
Embodiment 4：
Component includes：
Waste and old Pillar recovery plastics 825kg（Within moisture content 6%）,
Ethylene glycol 280kg（Excessive more than 130%）,
M-phthalic acid 50kg,
5-sodium sulfo isophthalate 125kg,
2- methyl isophthalic acids, 3 propane diols 60kg,
Sb2O330g,
Sodium acetate trihydrate 500g,
Diglycol 50kg.
Preparation method：
（1）Fragment is made in waste and old Pillar recovery plastics, in proportion by waste and old Pillar recovery plastic flakes, ethylene glycol,
Phthalic acid -5- sodium sulfonates, M-phthalic acid, 2- methyl isophthalic acids, 3 propane diols, diglycol, Sb2O3, Sodium acetate trihydrate mix
Put into after conjunction in fritting kettle, the heating of static normal pressure, this process fritting kettle fractionation capital temperature incipient stage control 130 DEG C with
Under, between preferably 105 DEG C ± 3 DEG C, when temperature reaches 235 DEG C ± 5 DEG C in reaction, material is melted completely, distillates moisture or methanol
When about reaching the 90~100% of theoretical quantity of distillate, early stage reaction completion is can determine whether, this process is substantially carried out alcoholysis, ester exchange, ester
Change reaction；Further temperature arrives 250-260 DEG C in rise, fractionation capital temperature is improved to 180 DEG C or so, by unnecessary ethylene glycol moieties
Distill；
（2）According to reaction condition, after above fritting reaction terminates, material is imported into terminal polymerization kettle, progressively carried since 235 DEG C
High temperature in the kettle, stops heating when interior temperature reaches 265 DEG C, while heating, slowly steps up in kettle vacuum and most
Below absolute pressure 133Pa is reached eventually.Because polycondensation reaction belongs to exothermic reaction, and agitating friction heat, reaction temperature can be after
Height of continuing rising.Interior temperature reaches polymerization under the conditions of 275 ± 2 DEG C, power of agitator 10KW, and this process is further by remaining excessive ethylene glycol
Removing, and then obtain the water-soluble polyurethane melt of FDY filament starching water-jet weaving；
（3）Stop stirring, stop vacuumizing, terminal polymerization kettle is carried out releasing vacuum with high pure nitrogen and pressurising is left to 0.2MPa
The right side, opens bottom valve, polymer is released in hopper and is cooled to solid material block；
（4）With strong crusher by expect block be broken into diameter less than 3mm it is powdered after, test, measure, pack,
Finished product.
The product prepared using above-mentioned technical process, glass transition temperature Tg is 56.7 DEG C, and powder does not stick together, outside product
See as yellowish coloured particles, solubility 28g, moisture content 0.19%.
15g products are taken, is together added with 85ml running water and 95 DEG C of stirring 30min is heated in 500ml flasks, whole is molten
Solution, no insoluble matter, solution clarifies saturating good brightness, and solution PH is 6.Gained polyester liquid（About 15%wt）Viscosity（25℃）For 6 ±
1mPa.S, 15% solution viscosity（95℃）For 2 ± 0.5mPa.S, the mass percent dissolved is tiled for 15% pulp solution
On PE films, serous coat is produced in design temperature is 80 DEG C of drying box, serous coat thickness about 0. 5mm, the long 10cm produced,
Width about 5cm, is made the elastic strong, good film-forming property of serous coat after serous coat, is soaked in 60 DEG C of hot water and turns white slightly, pliability is strong, does not send out
It is viscous.
Embodiment 5：
Component includes：
Waste and old Pillar recovery plastics 825kg（Within moisture content 6%）,
Ethylene glycol 280kg（Excessive more than 130%）,
M-phthalic acid 50kg,
Sodium Dimethyl Isophthalate-5-sulfonate 125kg,
2- methyl isophthalic acids, 3 propane diols 60kg,
Antimony glycol 60g,
Sodium acetate trihydrate 500g,
Zinc acetate 600g,
Diglycol 50kg.
Preparation method：
（1）Fragment is made in waste and old Pillar recovery plastics, in proportion by waste and old Pillar recovery plastic flakes, ethylene glycol,
Rutgers -5- sodium sulfonates, M-phthalic acid, 2- methyl isophthalic acids, 3 propane diols, diglycol, antimony glycol, vinegar
Put into after sour zinc, Sodium acetate trihydrate mixing in fritting kettle, static normal pressure heating, this process fritting kettle fractionation capital temperature starts rank
Section control is below 130 DEG C, between preferably 105 DEG C ± 3 DEG C, and when temperature reaches 235 DEG C ± 5 DEG C in reaction, material is melted completely,
When distillating moisture or methanol and about reaching the 90~100% of theoretical quantity of distillate, early stage reaction completion is can determine whether, this process is substantially carried out
Alcoholysis, ester exchange, esterification；Further temperature arrives 250-260 DEG C in rise, improves fractionation capital temperature to 180 DEG C or so, will be many
Remaining ethylene glycol moieties are distilled；
（2）According to reaction condition, after above fritting reaction terminates, material is imported into terminal polymerization kettle, progressively carried since 235 DEG C
High temperature in the kettle, stops heating when interior temperature reaches 265 DEG C, while heating, slowly steps up in kettle vacuum and most
Below absolute pressure 133Pa is reached eventually.Because polycondensation reaction belongs to exothermic reaction, and agitating friction heat, reaction temperature can be after
Height of continuing rising.Interior temperature reaches polymerization under the conditions of 275 ± 2 DEG C, power of agitator 10KW, and this process is further by remaining excessive ethylene glycol
Removing, and then obtain the water-soluble polyurethane melt of FDY filament starching water-jet weaving；
（3）Stop stirring, stop vacuumizing, terminal polymerization kettle is carried out releasing vacuum with high pure nitrogen and pressurising is left to 0.2MPa
The right side, opens bottom valve, polymer is released in hopper and is cooled to solid material block；
（4）With strong crusher by expect block be broken into diameter less than 3mm it is powdered after, test, measure, pack,
Finished product.
The product prepared using above-mentioned technical process, glass transition temperature Tg is 58.5 DEG C, and powder does not stick together, outside product
See as yellowish coloured particles, solubility 29g, moisture content 0.16%.
15g products are taken, is together added with 85ml running water and 95 DEG C of stirring 30min is heated in 500ml flasks, whole is molten
Solution, no insoluble matter, solution clarifies saturating good brightness, and solution PH is 6.Gained polyester liquid（About 15%wt）Viscosity（25℃）For 6 ±
1mPa.S, 15% solution viscosity（95℃）For 2 ± 0.5mPa.S, the mass percent dissolved is tiled for 15% pulp solution
On PE films, serous coat is produced in design temperature is 80 DEG C of drying box, serous coat thickness about 0. 5mm, the long 10cm produced,
Width about 5cm, is made the elastic strong, good film-forming property of serous coat after serous coat, is soaked in 60 DEG C of hot water and turns white slightly, pliability is strong, does not send out
It is viscous.
Embodiment 6：
Component includes：
Waste and old Pillar recovery plastics 825kg（Within 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 acids, 3 propane diols 60kg,
Antimony glycol 60g,
Sodium acetate trihydrate 500g,
Zinc acetate 600g,
Diglycol 50kg.
Preparation method：
（1）Fragment is made in waste and old Pillar recovery plastics, in proportion by waste and old Pillar recovery plastic flakes, ethylene glycol,
Phthalic acid binaryglycol ester -5- sodium sulfonates, M-phthalic acid, 2- methyl isophthalic acids, 3 propane diols, diglycol, ethylene glycol
Put into after antimony, zinc acetate, Sodium acetate trihydrate mixing in fritting kettle, static normal pressure heating, this process fritting kettle fractionation capital temperature
Incipient stage is controlled below 130 DEG C, between preferably 105 DEG C ± 3 DEG C, and when temperature reaches 235 DEG C ± 5 DEG C in reaction, material is complete
Full-fusing, when distillating moisture or methanol and about reaching the 90~100% of theoretical quantity of distillate, can determine whether early stage reaction completion, this process master
Carry out alcoholysis, ester exchange, esterification；Further temperature arrives 250-260 DEG C in rise, improves fractionation capital temperature to 180 DEG C of left sides
The right side, unnecessary ethylene glycol moieties are distilled；
（2）According to reaction condition, after above fritting reaction terminates, material is imported into terminal polymerization kettle, progressively carried since 235 DEG C
High temperature in the kettle, stops heating when interior temperature reaches 265 DEG C, while heating, slowly steps up in kettle vacuum and most
Below absolute pressure 133Pa is reached eventually.Because polycondensation reaction belongs to exothermic reaction, and agitating friction heat, reaction temperature can be after
Height of continuing rising.Interior temperature reaches polymerization under the conditions of 275 ± 2 DEG C, power of agitator 10KW, and this process is further by remaining excessive ethylene glycol
Removing, and then obtain the water-soluble polyurethane melt of FDY filament starching water-jet weaving；
（3）Stop stirring, stop vacuumizing, terminal polymerization kettle is carried out releasing vacuum with high pure nitrogen and pressurising is left to 0.2MPa
The right side, opens bottom valve, polymer is released in hopper and is cooled to solid material block；
（4）With strong crusher by expect block be broken into diameter less than 3mm it is powdered after, test, measure, pack,
Finished product.
The product prepared using above-mentioned technical process, glass transition temperature Tg is 58.5 DEG C, and powder does not stick together, outside product
See as yellowish coloured particles, solubility 29g, moisture content 0.16%.
15g products are taken, is together added with 85ml running water and 95 DEG C of stirring 30min is heated in 500ml flasks, whole is molten
Solution, no insoluble matter, solution clarifies saturating good brightness, and solution PH is 6.Gained polyester liquid（About 15%wt）Viscosity（25℃）For 6 ±
1mPa.S, 15% solution viscosity（95℃）For 2 ± 0.5mPa.S, the mass percent dissolved is tiled for 15% pulp solution
On PE films, serous coat is produced in design temperature is 80 DEG C of drying box, serous coat thickness about 0. 5mm, the long 10cm produced,
Width about 5cm, is made the elastic strong, good film-forming property of serous coat after serous coat, is soaked in 60 DEG C of hot water and turns white slightly, pliability is strong, does not send out
It is viscous.
FDY fiber is to use filament of synthetic fibre made from the step of spin-drawing one, fiber abundant orientation stretching sizing,
It is used directly for textile process.Feature：The smooth softness of feel, twists with the fingers point less, yarn, and cohesive force is small between monofilament, is similar to put down
Row state, gloss is dazzle the eyes, and is a kind of yield maximum in polyester fiber, is often used in weaving silk-like fabric.According to
This feature, in order to avoid yarn breakage causes parking in weaving process, starching makes obvolvent mutually between yarn monofilament, according to " phase
Patibhaga-nimitta is molten " principle, can reach more preferable cohesive force with polyester material.Other water-jet loom completes wefting insertion by water stream,
Water stream can cause the organizine and Fabric wettability of shed open near region, if slurry is not water-fast or moisture absorption is glued again, will result in the fabric flaw
Defect or degradation, slurry synthesized by the present invention can perfection can be thorough when water-fast heatproof, desizing when good water solubility, weaving when reaching with slurry
The requirement of bottom desizing.
The present invention key point be：1）, using Pillar recovery prepare FDY filament starching water-jet weaving water-soluble environment protective gather
Ester slurry；2）, alcoholysis, ester exchange, the step of esterification one complete；3）, using other dihydric alcohols, reach FDY starchings, weave, move back
Contaminate links particular/special requirement.
The present invention prepares FDY filament slurry using Pillar recovery one-step method, and while cost is reduced, production efficiency is also bright
It is aobvious to improve.
Claims (10)
1. a kind of FDY filament starching water-jet weaving water-soluble polyurethane, it is characterised in that：It is by Pillar recovery, accounts for recovery
Ethylene glycol of the weight polyester than 5~10% and following components
A, account for the M-phthalic acid -5- sulfonate of Pillar recovery weight than 10~20% or derivatives thereof,
B, account for M-phthalic acid of the Pillar recovery weight than 3~15%,
C, account for other dihydric alcohols of the Pillar recovery weight than 5~10%, other dihydric alcohols are 2- methyl isophthalic acids, 3 propane diols and/or 2,
2- dimethyl -1,3 propane diols,
D, account for catalyst of the Pillar recovery weight than 0.03~0.15%,
E, account for inorganic assistant of the Pillar recovery weight than 0.02~0.1%,
F, the polyethers for accounting for weight average molecular weight 600~10000 of the Pillar recovery weight than 0~5%,
Through alcoholysis, copolymerization, cooling, broken it is made；
Alcoholysis includes Pillar recovery fragment is made, in proportion by Pillar recovery fragment, ethylene glycol, M-phthalic acid -5- sulfonic acid
Put into after salt or derivatives thereof, M-phthalic acid, other dihydric alcohols, catalyst and inorganic assistant mixing in fritting kettle, it is static
Normal pressure heats up, and the fractionation capital temperature incipient stage control of this process fritting kettle is below 130 DEG C, when temperature reaches 235 DEG C ± 5 in reaction
DEG C, material is melted completely, when distillating moisture and reaching the 90~100% of theoretical quantity of distillate, and further temperature arrives 250-260 DEG C in rise,
Fractionation capital temperature is improved to 180 DEG C, unnecessary ethylene glycol moieties are distilled；
Copolymerization includes after above fritting reaction terminates, material being imported into terminal polymerization kettle, while adding polyethers, since 235 DEG C progressively
Temperature in the kettle is improved, stops heating when interior temperature reaches 265 DEG C, while heating, vacuum is slowly stepped up in kettle simultaneously
It is finally reached below absolute pressure 133Pa；Interior temperature reaches polymerization under the conditions of 275 ± 2 DEG C, power of agitator 10kW, and this process will be surplus
Remaining excessive ethylene glycol is further removed, and then obtains the water-soluble polyurethane melt of FDY filament starching water-jet weaving；
Cooling includes stopping stirring, stops vacuumizing, and terminal polymerization kettle is carried out releasing vacuum with high pure nitrogen and pressurising is to 0.2MPa,
Bottom valve is opened, polymer is released in hopper and is cooled to solid material block；
It is broken powdered including that will expect that block is crushed with strong crusher.
2. a kind of FDY filament starching water-jet weaving water-soluble polyurethane according to claim 1, it is characterised in that：
Described M-phthalic acid -5- sulfonate or derivatives thereof is selected from M-phthalic acid -5- sodium sulfonates, M-phthalic acid diformazan
Ester -5- sodium sulfonates or M-phthalic acid -5- sodium sulfonate glycol esters.
3. a kind of FDY filament starching water-jet weaving water-soluble polyurethane according to claim 1 or 2, its feature exists
In：Removed in described c components outside 2- methyl isophthalic acids, 3 propane diols and/or 2,2- dimethyl -1,3 propane diols and be additionally added a contracting diethyl
Glycol.
4. a kind of FDY filament starching water-jet weaving water-soluble polyurethane according to claim 1 or 2, its feature exists
In：Described catalyst includes polyester catalyst and/or ester exchange catalyst, and polyester catalyst is selected from antimony oxide or second two
Alcohol antimony, ester exchange catalyst is selected from zinc acetate or calcium acetate；Described inorganic assistant uses anti-ether agent, and described 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 or 2, its feature exists
In：Described polyethers is Macrogol 4000.
6. a kind of method for preparing FDY filament starching water-jet weaving water-soluble polyurethane described in claim 1, its feature exists
In including following four step：
（1）Fragment is made in Pillar recovery, in proportion by Pillar recovery fragment, ethylene glycol, M-phthalic acid -5- sulfonate or its
Put into after derivative, M-phthalic acid, other dihydric alcohols, catalyst and inorganic assistant mixing in fritting kettle, static normal pressure liter
Temperature, the fractionation capital temperature incipient stage control of this process fritting kettle is below 130 DEG C, when temperature reaches 235 DEG C ± 5 DEG C, thing in reaction
Material melting completely, when distillating moisture and reaching the 90~100% of theoretical quantity of distillate, can determine whether early stage reaction completion, this process is mainly entered
Row alcoholysis, ester exchange, esterification；Further temperature arrives 250-260 DEG C in rise, improves fractionation capital temperature to 180 DEG C, will be unnecessary
Ethylene glycol moieties distill；
（2）According to reaction condition, after above fritting reaction terminates, material is imported into terminal polymerization kettle, while polyethers is added, from 235 DEG C
Start to step up temperature in the kettle, stop heating when interior temperature reaches 265 DEG C, while heating, slowly step up in kettle
Vacuum is simultaneously finally reached below absolute pressure 133Pa；Interior temperature reaches polymerization under the conditions of 275 ± 2 DEG C, power of agitator 10kW, this
Process further removes remaining excessive ethylene glycol, and then obtains the water-soluble polyurethane of FDY filament starching water-jet weaving
Melt；
（3）Stop stirring, stop vacuumizing, terminal polymerization kettle is carried out releasing vacuum with high pure nitrogen and pressurising is to 0.2MPa, is opened
Bottom valve, polymer is released in hopper and is cooled to solid material block；
（4）With strong crusher will expect block crush it is powdered after, test, measure, pack, finished product.
7. one kind according to claim 6 prepares FDY filament starching water-jet weaving water-soluble polyester described in claim 1
The method of slurry, it is characterised in that：Described（1）M-phthalic acid -5- sulfonate described in step or derivatives thereof is selected
From M-phthalic acid -5- sodium sulfonates, DMIP -5- sodium sulfonates or M-phthalic acid -5- sodium sulfonate ethylene glycol
Ester；Removed in described c components outside 2- methyl isophthalic acids, 3 propane diols and/or 2,2- dimethyl -1,3 propane diols and be additionally added a contracting diethyl
Glycol；Described catalyst includes polymerization catalyst and/or ester exchange catalyst, and polymerization catalyst is selected from antimony oxide or second
Glycol antimony, ester exchange catalyst is selected from zinc acetate or calcium acetate；Described inorganic assistant is anti-ether agent, and described anti-ether agent is used
Anhydrous sodium acetate or Sodium acetate trihydrate；The（2）Polyethers described in step is selected from polyethylene glycol.
8. a kind of FDY filament starching water-jet weaving water-soluble polyurethane, it is characterised in that：The water-soluble polyurethane is
By waste and old Pillar recovery plastics 825kg, ethylene glycol 300kg, Sodium Dimethyl Isophthalate-5-sulfonate 150kg, M-phthalic acid
The propane diols 50kg of 50kg, 2,2- dimethyl -1,3, Macrogol 4000 25kg, Sodium acetate trihydrate 1kg, Sb2O3150g, acetic acid
Calcium 500g, through alcoholysis, copolymerization, cooling, broken is made；
Alcoholysis includes Pillar recovery plastics fragment is made, in proportion by Pillar recovery plastic flakes, ethylene glycol, M-phthalic acid
Dimethyl ester -5- sodium sulfonates, M-phthalic acid, 2,2- dimethyl -1,3 propane diols, Sb2O3, calcium acetate, Sodium acetate trihydrate mixing after
Put into fritting kettle, static normal pressure heating, this process fritting kettle fractionation capital temperature incipient stage is controlled below 130 DEG C, when
Temperature reaches 235 DEG C ± 5 DEG C in reaction, and material is melted completely, when distillating moisture and reaching the 90~100% of theoretical quantity of distillate, further
Temperature arrives 250-260 DEG C in rise, improves fractionation capital temperature to 180 DEG C, unnecessary ethylene glycol moieties are distilled；
After copolymerization terminates including above fritting reaction, material is imported into terminal polymerization kettle, while Macrogol 4000 is added, from 235 DEG C
Start to step up temperature in the kettle, stop heating when interior temperature reaches 265 DEG C, while heating, slowly step up in kettle
Vacuum is simultaneously finally reached below absolute pressure 133Pa；Interior temperature reaches polymerization under the conditions of 275 ± 2 DEG C, power of agitator 10kW, this
Process further removes remaining excessive ethylene glycol, and then obtains the water-soluble polyurethane of FDY filament starching water-jet weaving
Melt；
Cooling includes stopping stirring, stops vacuumizing, and terminal polymerization kettle is carried out releasing vacuum with high pure nitrogen and pressurising is to 0.2MPa,
Bottom valve is opened, polymer is released in hopper and is cooled to solid material block；
It is broken powdered including that will expect that block is crushed with strong crusher.
9. a kind of FDY filament starching water-jet weaving water-soluble polyurethane, it is characterised in that：The water-soluble polyurethane is
By waste and old Pillar recovery plastics 825kg, ethylene glycol 300kg, Sodium Dimethyl Isophthalate-5-sulfonate 125kg, M-phthalic acid
40kg, 2- methyl isophthalic acid, 3 propane diols 60kg, anhydrous sodium acetate 1kg, Sb2O3 30g, calcium acetate 500g, through alcoholysis, copolymerization, cooling,
It is broken to be made；
Alcoholysis include fragment is made in waste and old Pillar recovery plastics, in proportion by waste and old Pillar recovery plastic flakes, ethylene glycol,
Rutgers -5- sodium sulfonates, M-phthalic acid, 2- methyl isophthalic acids, 3 propane diols, Sb2O3, calcium acetate, anhydrous sodium acetate mix
Put into after conjunction in fritting kettle, the heating of static normal pressure, this process fritting kettle fractionation capital temperature incipient stage control 130 DEG C with
Under, when temperature reaches 235 DEG C ± 5 DEG C in reaction, material is melted completely, when distillating moisture and reaching the 90~100% of theoretical quantity of distillate,
Further temperature arrives 250-260 DEG C in rise, improves fractionation capital temperature to 180 DEG C, unnecessary ethylene glycol moieties are distilled；
Copolymerization includes after above fritting reaction terminates, material being imported into terminal polymerization kettle, temperature in the kettle is stepped up since 235 DEG C,
Stop heating when interior temperature reaches 265 DEG C, while heating, slowly step up in kettle vacuum and be finally reached absolute pressure
Below power 133Pa；Interior temperature reaches polymerization under the conditions of 275 ± 2 DEG C, power of agitator 10kW, and this process is by remaining excessive ethylene glycol
Further removing, and then obtain the water-soluble polyurethane melt of FDY filament starching water-jet weaving；
Cooling includes stopping stirring, stops vacuumizing, and terminal polymerization kettle is carried out releasing vacuum with high pure nitrogen and pressurising is to 0.2MPa,
Bottom valve is opened, polymer is released in hopper and is cooled to solid material block；
It is broken powdered including that will expect that block is crushed with strong crusher.
10. a kind of FDY filament starching water-jet weaving water-soluble polyurethane, it is characterised in that：The water-soluble polyurethane
It is by waste and old Pillar recovery plastics 825kg, ethylene glycol 280kg, Sodium Dimethyl Isophthalate-5-sulfonate 125kg, isophthalic diformazan
Sour 50kg, 2- methyl isophthalic acid, 3 propane diols 60kg, antimony glycol 60g, zinc acetate 600g, Sodium acetate trihydrate 500g, a contracting diethyl two
Alcohol 50kg, through alcoholysis, copolymerization, cooling, broken is made；
Alcoholysis include fragment is made in waste and old Pillar recovery plastics, in proportion by waste and old Pillar recovery plastic flakes, ethylene glycol,
Rutgers -5- sodium sulfonates, M-phthalic acid, 2- methyl isophthalic acids, 3 propane diols, diglycol, antimony glycol, vinegar
Put into after sour zinc, Sodium acetate trihydrate mixing in fritting kettle, static normal pressure heating, this process fritting kettle fractionation capital temperature starts rank
Section control is below 130 DEG C, and when temperature reaches 235 DEG C ± 5 DEG C in reaction, material is melted completely, is distillated moisture and is reached that theory is distillated
Amount 90~100% when, further rise in temperature arrive 250-260 DEG C, improve fractionation capital temperature to 180 DEG C, by unnecessary ethylene glycol
Part is distilled；
Copolymerization includes after above fritting reaction terminates, material being imported into terminal polymerization kettle, temperature in the kettle is stepped up since 235 DEG C,
Stop heating when interior temperature reaches 265 DEG C, while heating, slowly step up in kettle vacuum and be finally reached absolute pressure
Below power 133Pa；Interior temperature reaches polymerization under the conditions of 275 ± 2 DEG C, power of agitator 10kW, and this process is by remaining excessive ethylene glycol
Further removing, and then obtain the water-soluble polyurethane melt of FDY filament starching water-jet weaving；
Cooling includes stopping stirring, stops vacuumizing, and terminal polymerization kettle is carried out releasing vacuum with high pure nitrogen and pressurising is to 0.2MPa,
Bottom valve is opened, polymer is released in hopper and is cooled to solid material block；
It is broken powdered including that will expect that block is crushed with strong crusher.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510453115.0A CN104988733B (en) | 2015-07-29 | 2015-07-29 | FDY filament starching water-jet weaving water-soluble polyurethane and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510453115.0A CN104988733B (en) | 2015-07-29 | 2015-07-29 | FDY filament starching water-jet weaving water-soluble polyurethane and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104988733A CN104988733A (en) | 2015-10-21 |
| CN104988733B true CN104988733B (en) | 2017-07-14 |
Family
ID=54300616
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510453115.0A Active CN104988733B (en) | 2015-07-29 | 2015-07-29 | FDY filament starching water-jet weaving water-soluble polyurethane and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104988733B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105949448A (en) * | 2016-06-17 | 2016-09-21 | 吴江市恒茂环保科技有限公司 | Process for preparing water-soluble polyester chip through regenerated bottle-grade chips and production system thereof |
| CN112812284B (en) * | 2020-12-30 | 2022-05-24 | 湖北山特莱新材料有限公司 | Water-soluble slurry capable of being desized quickly |
| CN112852117B (en) * | 2021-03-11 | 2022-05-24 | 湖北山特莱新材料有限公司 | High-temperature-resistant water-soluble polyester slurry |
| CN113045740B (en) * | 2021-03-18 | 2022-07-26 | 湖北山特莱新材料有限公司 | Preparation method of cyclic regeneration type water-soluble polyester chip |
| CN113174035B (en) * | 2021-05-08 | 2022-12-02 | 湖北山特莱新材料有限公司 | Multifunctional water-soluble polyester slurry |
| CN114481413B (en) * | 2021-12-23 | 2023-07-18 | 吴江余宏织造有限公司 | Weaving method of high-bulking chemical fiber cloth and high-bulking chemical fiber cloth |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4977191A (en) * | 1989-06-27 | 1990-12-11 | The Seydel Companies, Inc. | Water-soluble or water-dispersible polyester sizing compositions |
| CN101798482A (en) * | 2009-02-10 | 2010-08-11 | 上海诺科化工新材料有限公司 | Environment-friendly aqueous adhesive for shoes |
| CN102604062A (en) * | 2012-04-11 | 2012-07-25 | 山东巨业精细化工有限公司 | Water-soluble polyester for textile size and preparation method of water-soluble polyester |
| CN103572605A (en) * | 2012-08-11 | 2014-02-12 | 嘉兴瀚天纺织新材料有限公司 | Mixed size prepared from waste PET (polyethylene terephthalate) and used for filament spinning and preparation method of mixed size |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05214678A (en) * | 1992-01-31 | 1993-08-24 | Yushiro Chem Ind Co Ltd | Warp-sizing agent |
-
2015
- 2015-07-29 CN CN201510453115.0A patent/CN104988733B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4977191A (en) * | 1989-06-27 | 1990-12-11 | The Seydel Companies, Inc. | Water-soluble or water-dispersible polyester sizing compositions |
| CN101798482A (en) * | 2009-02-10 | 2010-08-11 | 上海诺科化工新材料有限公司 | Environment-friendly aqueous adhesive for shoes |
| CN102604062A (en) * | 2012-04-11 | 2012-07-25 | 山东巨业精细化工有限公司 | Water-soluble polyester for textile size and preparation method of water-soluble polyester |
| CN103572605A (en) * | 2012-08-11 | 2014-02-12 | 嘉兴瀚天纺织新材料有限公司 | Mixed size prepared from waste PET (polyethylene terephthalate) and used for filament spinning and preparation method of mixed size |
Non-Patent Citations (1)
| Title |
|---|
| 乙二醇醇解法回收涤纶废丝制备聚酯浆料的研究;李准准;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20090315;第11、22-25页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104988733A (en) | 2015-10-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104988733B (en) | FDY filament starching water-jet weaving water-soluble polyurethane and preparation method thereof | |
| CN105064028B (en) | DTY low elastic polyester filament starching water-soluble polyurethanes and preparation method thereof | |
| JP3205620B2 (en) | Water-soluble or water-dispersible sulfonated polyester resin composition | |
| CN102604062B (en) | Water-soluble polyester for textile size and preparation method of water-soluble polyester | |
| US4158083A (en) | Fibrous article sized with a branched water-dispersible polyester | |
| CN109485839A (en) | A method of water-soluble polyester is prepared using three monomer production technology Waste water concentrating material | |
| CN1980977B (en) | Sulfonated copolyetherester compositions from hydroxyalkanoic acids and shaped articles produced therefrom | |
| CN100558784C (en) | The sulfonated aliphatic-aromatic copolyether ester | |
| KR20000057356A (en) | Sulfoaryl modified water-soluble or water-dispersible resins from polyethylene terephthalate or terephthalates | |
| PT1327648E (en) | Polymerization catalyst for polyester, polyester produced with the same, and process for producing polyester | |
| KR20150144336A (en) | Paper and nonwoven articles comprising synthetic microfiber binders | |
| CN111808272B (en) | Impact-resistant heat-resistant flame-retardant polyester, polyester product, and preparation method and application thereof | |
| CN115651371A (en) | Polymer composition for making thermoformed articles | |
| CN102617839A (en) | Method for preparing water-soluble polyesters for composite fibers by waste polyesters | |
| CN105111423A (en) | Polymer waterborne polyester and preparation method thereof | |
| CN102352027A (en) | Cationic dye dyeable polyester and superfine fibers thereof | |
| CN107417897A (en) | A kind of degradation of ethylene glycol discards the method that polyester fabric prepares water-soluble polyester | |
| CN105002588A (en) | Preparation method for imitating cotton polyester-PET/PA6 copolymer fiber | |
| KR101551638B1 (en) | Flame Retardancy Copolymer Polyester Using Chemical Recycling Process and Process of Preparation Thereof | |
| CN107163892B (en) | Preparation method for producing polyester hot melt adhesive by using PET waste material | |
| CN116288804B (en) | High-shrinkage polyester sea-island fiber and preparation method and application thereof | |
| KR20200059241A (en) | Thermoplastic polyester with many 1,4: 3,6-dianhydro-L-iditol units mixed | |
| JP2009275319A (en) | Flame-retardant polyester composite staple fiber | |
| KR960006301B1 (en) | Method for manufacturing polyester | |
| CN111777753B (en) | Heat-resistant flame-retardant polyester, polyester product, preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information |
Address after: 441403 Lei Road, Lei Da Industrial Park, Lei Town, Xiangyang City, Hubei, Yicheng Applicant after: HUBEI JIATE WEAVING SLURRY CO.,LTD. Address before: 441403 Lei Road, Lei Da Industrial Park, Lei Town, Xiangfan City, Hubei, Yicheng Applicant before: HUBEI JIATE WEAVING SLURRY Co.,Ltd. |
|
| CB02 | Change of applicant information | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CB03 | Change of inventor or designer information |
Inventor after: Chen Chunhua Inventor after: Zhou Zhongxu Inventor before: Wei Jinhong Inventor before: Chen Chunhua Inventor before: Zhou Zhongxu Inventor before: Sun Jinglun |
|
| CB03 | Change of inventor or designer information | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20171225 Address after: 441403 Lei Yan Avenue in Lehe Town, Yicheng, Xiangyang, Hubei Patentee after: Hubei Santak New Material Co.,Ltd. Address before: 441403 Lei Road, Lei Da Industrial Park, Lei Town, Xiangyang City, Hubei, Yicheng Patentee before: HUBEI JIATE WEAVING SLURRY CO.,LTD. |
|
| TR01 | Transfer of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
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 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right |