CN1020736C - Manufacturing method of polyesteramide thermosol for fabric - Google Patents
Manufacturing method of polyesteramide thermosol for fabric Download PDFInfo
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- CN1020736C CN1020736C CN 89100675 CN89100675A CN1020736C CN 1020736 C CN1020736 C CN 1020736C CN 89100675 CN89100675 CN 89100675 CN 89100675 A CN89100675 A CN 89100675A CN 1020736 C CN1020736 C CN 1020736C
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- acid
- hot melt
- polycondensation
- diamine
- melt adhesive
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Abstract
The present invention relates to a manufacturing method for polyesteramide thermosol for fabric, which comprises that firstly, terylene type polyester is mixed with dihydric alcohol, and the mixture is heated and stirred under the action of a catalyst to alcoholize the terylene type polyester; then, dicarboxylic acid, diamine, the catalyst and an antioxidant are added to be heated and stirred under the protection of nitrogen gas, and a polycondensation reaction is carried out to manufacture the polyesteramide thermosol. The method has the advantages of abundant raw material, cheapness, easy acquirement, low cost, high efficiency, easy control of a production process and no generation of three waste. An adhesive lining manufactured by the polyesteramide thermosol has the advantages of high strength retention, dry cleaning resistance and favorable performance of water washing.
Description
The present invention relates to the manufacture method that a kind of fabric sticks with glue agent.
A kind of manufacture method of polyesteramide thermosol for fabric is disclosed in JP-59-140226, US-4604449, US-4345064, US-4254254 patent document.They all are to adopt different di-carboxylic acid (or its ester), dibasic alcohol or diamine, and under the effect of catalyzer, heated and stirred is carried out transesterify, at high temperature carry out polycondensation then and make.The weak point of this method is: the cost height; Price costlinesses such as normally used raw material such as laurolactam, 11 lactan, dimethyl isophthalate 1,6-hexylene glycol, thereby the cost of polyester amide hot melt adhesive is also improved greatly; Generate toxic substance methyl alcohol in the reaction of above-mentioned raw materials, be unfavorable for operation and environment protection.
The manufacture method that the objective of the invention is to overcome weak point of the prior art and a kind of polyester amide hot melt adhesive is provided.
Purpose of the present invention can reach by following measure:
The manufacturing technology steps of polyester amide hot melt adhesive is:
1. alcoholysis: with terylene resin and C
2-6Dibasic alcohol mix, under the effect of catalyst acetic acid zinc, heating, stir, carry out alcoholysis;
2. esterification and amidate action: add C in the solution after alcoholysis
6-10Di-carboxylic acid and C
6-10Diamine, and drip the oxidation inhibitor triphenyl phosphite, under protection of nitrogen gas, heating, stir, in the time of 190 ℃～206 ℃, finish esterification and amidate action;
3. polycondensation: add The catalytic antimony trioxide in the system behind esterification and amidate action, under protection of nitrogen gas, heating, stirring, connect vacuum pump then, continue heating, dealcoholysis, temperature rises to 235 ℃～240 ℃ gradually, overbottom pressure is 0.4-0.5mmHg in the maintenance system, continue the polycondensation dealcoholysis, along with the carrying out of polycondensation, the viscosity in the system increases gradually, when " pole-climbing " phenomenon occurring, polycondensation is finished;
4. feeding nitrogen is removed vacuum, melt polymers is strip pours in the cold water, promptly obtains flexible polyester acid amides hot melt adhesive tape.
The consumption of terylene resin accounts for the mole fraction 0.5～0.6 of diprotic acid in the present invention, and the mol ratio of dibasic alcohol and diamine is 1.02: 0.15～0.94: 0.22, and the consumption of alcohol, amine is 1.2 times of acid amount.
Used C among the present invention
2-6Dibasic alcohol be: ethylene glycol, butyleneglycol, a condensed ethandiol, hexylene glycol.
Used C among the present invention
6-10Di-carboxylic acid be: terephthalic acid (ester), m-phthalic acid (ester), sebacic acid, hexanodioic acid.
Used C among the present invention
6-10Diamine be: hexanediamine, decamethylene diamine.
Be described in further detail below in conjunction with specific embodiment.
Embodiment 1:
Alcoholysis: take by weighing the polyester resin particle of 115.2g, the ethylene glycol of 71.9g adds in the there-necked flask, adds catalyst acetic acid zinc 0.12g again, heating, and the alcoholysis that under agitation refluxes.The efflorescence gradually of polyester resin particle, until dissolving fully, the reaction system is transparent homogeneous phase, and alcoholysis reaction is finished.
Esterification and amidate action: the hexanediamine that adds hexanodioic acid 58.4g and 23.2g in the there-necked flask after alcoholysis is finished; and dropping oxidation inhibitor triphenyl phosphite 0.3ml; under protection of nitrogen gas, heat temperature raising is when temperature reaches 100 ℃; material begins fusing; and start stirring, during to liquid temperature rise to the 190 ℃ left and right sides, begin to occur drop; gas phase temperature is at 98～105 ℃ at this moment, and esterification and amidate action begin.The water that generates in the reaction is steamed, and along with the carrying out of reaction, aquifer yield constantly increases, and when aquifer yield was slightly larger than the aquifer yield of Theoretical Calculation, esterification and acid amides reaction were finished.At this moment, the liquid temperature is about 204～206 ℃.
Polycondensation: in above-mentioned there-necked flask, add the 0.17g The catalytic antimony trioxide again.Logical nitrogen heating behind material melting, is slowly started stirring, when temperature rises to 210 ℃, begin to have distillate ethylene glycol to be steamed, when slack-off, system is connected water jet pump to the speed of distillating, it is 10～15mmHg that vacuum tightness reaches overbottom pressure gradually, and temperature rises to 220～230 ℃, keeps about 1 hour.When distillate seldom the time, system is connected high vacuum, make overbottom pressure reach 0.4～0.5mmHg, temperature rises to 246 ℃ gradually.Along with steaming of ethylene glycol, the viscosity of system increases gradually, and power of agitator also increases gradually thereupon, and when slight " pole-climbing " phenomenon occurring, polycondensation is finished.Logical then nitrogen is removed vacuum, melt polymers is strip pours in the cold water, promptly obtains yellowish flexible adhesive tape, is cut into micelle.The fusing point of this glue (mp) is 116～121 ℃, and melting index (MI) is 38.5, logarithmic specific concentration viscosity (Ln
C) be 0.634, with this polyesteramide in apparatus,Soxhlet's with continuous molten the getting 8 hours of trieline, its rate of weight loss only is 0.11%.
Embodiment
Alcoholysis: the polyester resin particle of 115.2g, the ethylene glycol of 92.4g and the zinc acetate of 0.12g are added in the there-necked flask.Heating, alcoholysis under agitation refluxes.The efflorescence gradually of terylene particle, until dissolving fully, the reaction system is transparent homogeneous phase, and alcoholysis reaction is finished.
Esterification and amidate action: in finishing the there-necked flask of alcoholysis reaction, add the hexanodioic acid of 87.6g and the decamethylene diamine of 42.2g, and drip the oxidation inhibitor triphenyl phosphite of 0.3mL.Under nitrogen protection, heat temperature raising, when temperature reached 100 ℃, material began to dissolve, and started stirring.During to liquid temperature rise to the 190 ℃ left and right sides, begin to occur drop, this moment gas phase temperature at 98～105 ℃, esterification at this moment and amidate action begin.The water that generates in the reaction is steamed, and along with the carrying out of reaction, aquifer yield constantly increases, and when aquifer yield was slightly larger than the aquifer yield of Theoretical Calculation, esterification and amidate action were finished, and this moment, the liquid temperature was 204～206 ℃.
Polycondensation: the antimonous oxide that in above-mentioned there-necked flask, adds 0.20g.Stirring is slowly started in logical nitrogen, heating behind material melting, temperature begins to have distillate ethylene glycol to be steamed when rising to 210 ℃, when slack-off, system is connected water jet pump to the speed of distillating, it is 10～15mmHg that vacuum tightness reaches overbottom pressure gradually, temperature rises to 220～230 ℃, keeps about 1 hour.Distillate is connected high vacuum with system seldom the time, makes overbottom pressure reach 0.4～0.5mmHg, and temperature rises to 235 ℃ gradually.Along with steaming of ethylene glycol, the viscosity of system increases gradually, and power of agitator also increases thereupon, and when slight " pole-climbing " phenomenon occurring, polycondensation is finished.Logical then nitrogen is removed vacuum, melt polymers is strip pours in the cold water, promptly obtains yellowish flexible adhesive tape, is cut into micelle, and the fusing point of this glue (mp) is 115～127 ℃, and melting index (MI) is 28.This polymkeric substance is put into apparatus,Soxhlet's got 8 hours with trieline is molten, rate of weight loss only is 0.12%.
The polyesteramide micelle that example 1,2 makes is made rubber powder by the method for CN85105052 patent.It is 60～100 purpose rubber powders that sieve is got granularity, presses 25g/m
2The dusting amount, be spread on terylene non-woven fabric or the woven textile cloth.Under 150～160 ℃ temperature, baked 40～50 seconds, the rubber powder fusing, and adhere on the base cloth, promptly make adhesive lining.
Get above-mentioned adhesive lining and different linings, use pressing machine at 150 ℃, 2.5kg/cm
2Pressure under, press to scald 10 seconds, promptly make the sample after compound.
Get the sample after compound, by the state specified standards washing methods, washing is four times in 40 ℃ water, finds to bubble and the phenomenon of coming unglued, and with the stripping strength of not washing sample relatively, its strength retention is 82～83%.Anti-dry-cleaning test is sample to be soaked take out after 48 hours in trieline, after drying, measures that stripping strength is same does not wash the sample ratio, and strength retention is 72～80%.
The present invention compared with prior art has following advantage:
1. the terylene type polyester that uses of the present invention mainly is the offal that utilizes in polyester resin production and the processing, thus the raw material abundance, cheap, be easy to get, thereby the cost of polyester amide hot melt adhesive is reduced greatly.
2. use terylene type polyester to make raw material, not only production process is easy to control, and has not generated Poisonous substance matter is such as methyl alcohol. Do not produce the three wastes, be conducive to environmental protection.
3. the polyester amide hot melt adhesive of producing in this way, the viscosity height. The adhesive lining strength retention height that Cheng Fenhou makes, anti-dry-cleaning, wash durability are good.
Claims (5)
1, a kind of manufacture method of polyesteramide thermosol for fabric, its technology is to use di-carboxylic acid (or its ester), dibasic alcohol and diamine under the effect of catalyzer, and polycondensation is carried out in heating, stirring, produce polyester amide hot melt adhesive, it is characterized in that: processing step is:
1. alcoholysis: with terylene resin and C
2-6Dibasic alcohol mix, under the effect of catalyst acetic acid zinc, heating, stir, carry out alcoholysis;
2. esterification and amidate action: add C in the solution after alcoholysis
6-10Di-carboxylic acid and C
6-10Diamine, and drip the oxidation inhibitor triphenyl phosphite, under protection of nitrogen gas, heating, stir, in the time of 190 ℃-206 ℃, finish esterification and amidate action;
3. polycondensation: add The catalytic antimony trioxide in the system behind esterification and amidate action, under protection of nitrogen gas, heating, stirring, connect vacuum pump then, continue heating, dealcoholysis, temperature rises to 235-240 ℃ gradually, overbottom pressure is 0.4-0.5mmHg in the maintenance system, continue the polycondensation dealcoholysis, along with the carrying out of polycondensation, the viscosity in the system increases gradually, when " pole-climbing " phenomenon occurring, polycondensation is finished;
4. feed nitrogen, remove vacuum, melt polymers is strip pours in the cold water, promptly obtain flexible polyester acid amides hot melt adhesive tape.
2, according to the manufacture method of the said polyester amide hot melt adhesive of claim 1, it is characterized in that: the consumption of terylene resin accounts for the mole fraction 0.5-0.6 of diprotic acid, the mol ratio of dibasic alcohol and diamine is 1.02: 0.15-0.94: 0.22, and the consumption of hydramine is 1.2 times of acid amount.
3, according to the manufacture method of the said polyester amide hot melt adhesive of claim 1, it is characterized in that: used C in the alcoholysis reaction
2-6Dibasic alcohol be: ethylene glycol, butyleneglycol, a condensed ethandiol, hexylene glycol.
4, according to the manufacture method of the said polyester amide hot melt adhesive of claim 1, it is characterized in that: used C in esterification and the amidate action
6-10Di-carboxylic acid be: terephthalic acid (ester), m-phthalic acid (ester), sebacic acid, hexanodioic acid.
5, according to the manufacture method of the said polyester amide hot melt adhesive of claim 1, it is characterized in that: used C in esterification and the amidate action
6-10Diamine be: hexanediamine, decamethylene diamine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89100675 CN1020736C (en) | 1989-02-01 | 1989-02-01 | Manufacturing method of polyesteramide thermosol for fabric |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89100675 CN1020736C (en) | 1989-02-01 | 1989-02-01 | Manufacturing method of polyesteramide thermosol for fabric |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1044664A CN1044664A (en) | 1990-08-15 |
| CN1020736C true CN1020736C (en) | 1993-05-19 |
Family
ID=4853971
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 89100675 Expired - Fee Related CN1020736C (en) | 1989-02-01 | 1989-02-01 | Manufacturing method of polyesteramide thermosol for fabric |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1020736C (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1102169C (en) * | 1999-09-29 | 2003-02-26 | 郑州大学 | Petroleum fermented nylon 1212 not-fusible colloid and its preparing process |
| CN102382614A (en) * | 2011-09-13 | 2012-03-21 | 烟台德邦电子材料有限公司 | Polyamide hot melt adhesive for adhering nonpolar materials and preparation method thereof |
| CN102408867B (en) * | 2011-09-13 | 2013-08-21 | 浙江速固德科技有限公司 | Process for preparing high temperature-resistant polyester hot melt adhesive powder |
| CN104892932B (en) * | 2014-03-04 | 2022-06-28 | 上海凯赛生物技术股份有限公司 | Polyester amide, preparation method thereof and product fiber thereof |
| CN106520056B (en) * | 2016-10-09 | 2019-08-06 | 浙江大学 | A kind of PET overlay film aluminium sheet and preparation method thereof |
| CN109867779B (en) * | 2017-12-05 | 2021-12-07 | 上海凯赛生物技术股份有限公司 | Preparation method of polyesteramide and product thereof |
| CN110591086B (en) * | 2019-09-12 | 2021-12-14 | 江苏景宏新材料科技有限公司 | Biodegradable polyesteramide and preparation method thereof |
-
1989
- 1989-02-01 CN CN 89100675 patent/CN1020736C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1044664A (en) | 1990-08-15 |
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