CN104558560A - A preparing method of low-melting point polyester used for manufacturing terylene sewing threads - Google Patents
A preparing method of low-melting point polyester used for manufacturing terylene sewing threads Download PDFInfo
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- CN104558560A CN104558560A CN201310471710.8A CN201310471710A CN104558560A CN 104558560 A CN104558560 A CN 104558560A CN 201310471710 A CN201310471710 A CN 201310471710A CN 104558560 A CN104558560 A CN 104558560A
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Abstract
The invention relates to a preparing method of low-melting point polyester used for manufacturing terylene sewing threads. The method includes: 1) performing esterification by adopting terephthalic acid, ethylene glycol, isophthalic acid, and a straight-chain monomer having double hydroxyl reaction functional groups except the ethylene glycol; and 2) under the existence of a condensation polymerization catalyst, performing further esterification and pre-condensation polymerization, and performing condensation polymerization under a vacuum condition of 0.1-2 KPa. The melting point and the intrinsic viscosity of a polyester product prepared by the method are lower than that of conventional polyester. Compared with present low-melting point polyester, the intrinsic viscosity and the crystallization property of the product prepared by the method are low, and dissolution performance when the product is used for producing an adhesive used for solvent type bonded threads is good.
Description
Technical field
The present invention relates to a kind of preparation method of low-melting point polyester, particularly a kind of preparation method of the outer tackiness agent low-melting point polyester for the manufacture of polyster fibre sewing thread.
Background technology
Polyster fibre sewing thread is made up of polyester filament or polyester staple fiber, have that intensity is high, wear-resisting, washing shrinkage is low, chemical stability is good, can be used for sewing up various dress materials, footwear, case and bag, toy etc. and other dressing material, is sewing thread with the most use, the most universal at present; Polyster fibre sewing thread has practical and decoration dual-use function, and the quality of its quality not only affects sewing efficiency and tooling cost, also affects the visual appearance of finished product.General polyster fibre sewing thread is by the yarn of more than two or two or long filament and twists with the fingers and form, multiplied yarn in conjunction with tightness degree and bar evenness, determined by twisting process and technology stability.
Along with the development of industry high speed seamer, have higher requirement to the use properties of sewing thread, long filament sewing thread product is just widely used in high-grade clothing with its high strength, non junction and the good performance such as even in the world.In addition, the long filament sewing thread that case and bag, footwear and leatherware also requirement intensity are higher.
Terylene Bandaid sewing thread is a kind ofly especially applicable to the superior in quality sewing thread of high speed sewing machine, high temperature resistant in the process of making, flexible, nondiscoloration, do not break, the performance such as phozy, and there is the characteristic such as waterproof, mildew-resistant.Terylene bandage thread is divided into Nei Bang and foreign countries two kinds: interior nation is that polyester filament (yarn) and thermal fuse high-temp glue are combined, foreign countries are that polyester filament (yarn) crosses glue at skin, because bandage thread is more closely glued together by plurality of threads (yarn) to form, so enhance the pulling force of sewing thread, compare with ordinary sewing line, bandage thread also have that pulling force is high, wear resisting property good, washing shrinkage is little, multiplied yarn in conjunction with tightness degree and bar evenness is high, the advantage of bouncing pilotage and broken string not easily occurs.
The low-melting point polyester that prior art is produced, poor for the production of solubility property during solvent-borne type bandage thread tackiness agent, and the tackiness agent after the dissolving of this low-melting point polyester is coated on polyster fibre sewing thread skin, dry rear sewing thread surface and easily occur whiting, sewing thread is made to occur the phenomenon of uneven color, affect outward appearance, be not therefore suitable for the outer tackiness agent manufacturing terylene foreign countries sewing thread.
Summary of the invention
The technical problem that the present invention solves is to provide a kind of preparation method of low-melting point polyester of the outer tackiness agent for the manufacture of polyster fibre sewing thread, at 80 DEG C ~ 120 DEG C between the polyester product melting zone that the method is obtained, limiting viscosity, between 0.4dl/g ~ 0.6dl/g, is suitable for the outer tackiness agent manufacturing terylene foreign countries sewing thread.
Technical solution of the present invention is as follows:
For the manufacture of a preparation method for the low-melting point polyester of polyster fibre sewing thread, comprising:
1) with following four kinds of components for reaction raw materials:
A: terephthalic acid
B: m-phthalic acid
C: ethylene glycol
D: the linear monomers with two hydroxyl reaction functional group except ethylene glycol;
Above-mentioned reaction raw materials is carried out esterification at 240 ~ 270 DEG C of temperature, esterification pressures 20 ~ 50kPa, react and be not less than 92% to esterification yield, reaction process removes the water of generation;
2) by the esterification products of above-mentioned reaction raw materials, under polycondensation catalyst existence condition, under the condition of negative pressure 2 ~ 10kpa, temperature of reaction is 260 ~ 285 DEG C and carries out further esterification and precondensation, 1.5 ~ 2.5 hours reaction times; Then under negative pressure 0.1 ~ 2KPa condition, polycondensation temperature is 260 ~ 290 DEG C, 2 ~ 3 hours reaction times, obtained low-melting point polyester.
In described step 1), reaction raw materials molar ratio is (terephthalic acid+m-phthalic acid): (linear monomers of the two hydroxyl reaction functional group of ethylene glycol+have)=1: 1.1 ~ 1.8.
In described step 1), the mol ratio of each reaction raw materials is terephthalic acid: m-phthalic acid=1: 0.5 ~ 1; Ethylene glycol: linear monomers=1 with two hydroxyl reaction functional group: 0.05 ~ 0.2.
The monomer with two hydroxyl reaction functional group described in described step 1) is selected from the mixture of one or more in 1,6-hexylene glycol, BDO, 1,3-PD, glycol ether, polyoxyethylene glycol.
Described step 2) in polycondensation catalyst be selected from one in antimony glycol, antimony acetate or antimonous oxide, the theoretical yield weight that the consumption of polycondensation catalyst obtains polyester based on polycondensation is benchmark, counts 180 ~ 300ppm/kg with antimony ion.
At 80 DEG C ~ 120 DEG C between the melting zone of described low-melting point polyester, limiting viscosity is between 0.4dl/g ~ 0.6dl/g.
Key of the present invention is on the basis of normal polyester, add m-phthalic acid and other straight dihydric alcohol class monomers, and control esterification and polycondensation process, obtained low-melting point polyester, the fusing point of this polyester and limiting viscosity are all lower than normal polyester, and compared with existing low-melting point polyester, limiting viscosity and crystal property low, good for the production of solubility property during solvent-borne type bandage thread tackiness agent.
Compared with existing low-melting point polyester production technology, the invention has the advantages that obtained polyester product limiting viscosity is low, crystal property is low, good for the production of solubility property during solvent-borne type bandage thread tackiness agent, the soft resilient film of one deck can be formed on sewing thread surface, film is colourless, smooth, does not affect pliability and the outward appearance of sewing thread.Meanwhile, preparation technology of the present invention is simple, and cost is low, can complete in general-purpose equipment, has good industrial applications prospect.
The low-melting point polyester of system of the present invention, be suitable for the outer tackiness agent manufacturing terylene foreign countries sewing thread, good for the production of solubility property during solvent-borne type bandage thread tackiness agent, tackiness agent after dissolving is coated on polyster fibre sewing thread skin, the soft resilient film of one deck is formed on sewing thread surface after drying, film is colourless, smooth, does not affect pliability and the outward appearance of sewing thread.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1 ~ 3
1) with terephthalic acid, ethylene glycol, m-phthalic acid, and the linear monomers with two hydroxyl reaction functional group except ethylene glycol is reaction raw materials, esterification is carried out at 240 ~ 270 DEG C of temperature, esterification pressures 20 ~ 50kPa, raw material molar ratio is (terephthalic acid+abridged edition dioctyl phthalate): (linear monomers of the two hydroxyl reaction functional group of ethylene glycol+have)=1: 1.1 ~ 1.8, reaction is to esterification yield to being not less than 92%, and reaction process removes the water of generation;
2) esterification products intermediate is under polycondensation catalyst existence condition, under the condition of negative pressure 2 ~ 10kpa, temperature of reaction is 260 ~ 285 DEG C of polyester oligomers carrying out that further esterification and prepolymerization reaction obtain certain polymerization degree, and the reaction times is 1.5 ~ 2.5 hours; Then under negative pressure 0.1 ~ 2KPa vacuum condition, polycondensation temperature is 260 ~ 290 DEG C, 2 ~ 3 hours reaction times, obtained low-melting point polyester.
The reaction raw materials proportioning of embodiment 1 ~ 3 is in table 1.
The esterification reaction tech of embodiment 1 ~ 3: temperature of reaction 255 DEG C, reaction pressure 30kpa, removes the water of generation in reaction process, when reacting esterification yield and reaching 95%, esterification completes.
The precondensation technique of embodiment 1 ~ 3: temperature of reaction 265 DEG C, reaction pressure negative pressure 2kpa, reaction times 2hr.
The polycondensating process of embodiment 1 ~ 3: temperature of reaction 285 DEG C, reaction pressure negative pressure 0.1kpa, reaction times 2hr.
Table 1
* comparative example 1 is normal polyester section
Measure the molecular weight and molecualr weight distribution of embodiment and comparative example low-molecular-weight polyester, and other primary quality measure, data are in table 2.
Table 2
Although preferred embodiment discloses as above by the present invention; so itself and be not used to limit content of the present invention; anyly be familiar with this those skilled in the art; not departing from main spirits of the present invention and context; when doing various change and retouching, the protection domain therefore invented should be as the criterion with the basic right claimed range applied for a patent.
Claims (6)
1. for the manufacture of a preparation method for the low-melting point polyester of polyster fibre sewing thread, it is characterized in that, comprising:
1) with following four kinds of components for reaction raw materials:
A: terephthalic acid
B: m-phthalic acid
C: ethylene glycol
D: the linear monomers with two hydroxyl reaction functional group except ethylene glycol;
Above-mentioned reaction raw materials is carried out esterification at 240 ~ 270 DEG C of temperature, esterification pressures 20 ~ 50kPa, react and be not less than 92% to esterification yield, reaction process removes the water of generation;
2) by the esterification products of above-mentioned reaction raw materials, under polycondensation catalyst existence condition, under the condition of negative pressure 2 ~ 10kpa, temperature of reaction is 260 ~ 285 DEG C and carries out further esterification and precondensation, 1.5 ~ 2.5 hours reaction times; Then under negative pressure 0.1 ~ 2KPa condition, polycondensation temperature is 260 ~ 290 DEG C, 2 ~ 3 hours reaction times, obtained low-melting point polyester.
2. the preparation method of the low-melting point polyester for the manufacture of polyster fibre sewing thread according to claim 1, it is characterized in that, in described step 1), reaction raw materials molar ratio is (terephthalic acid+m-phthalic acid): (linear monomers of the two hydroxyl reaction functional group of ethylene glycol+have)=1: 1.1 ~ 1.8.
3. the preparation method of the low-melting point polyester for the manufacture of polyster fibre sewing thread according to claim 1 and 2, is characterized in that, in described step 1), the mol ratio of each reaction raw materials is terephthalic acid: m-phthalic acid=1: 0.5 ~ 1; Ethylene glycol: linear monomers=1 with two hydroxyl reaction functional group: 0.05 ~ 0.2.
4. the preparation method of the low-melting point polyester for the manufacture of polyster fibre sewing thread according to claim 1, it is characterized in that, the monomer with two hydroxyl reaction functional group described in described step 1) is selected from 1,6-hexylene glycol, 1, the mixture of one or more in 4-butyleneglycol, 1,3-PD, glycol ether, polyoxyethylene glycol.
5. the preparation method of the low-melting point polyester for the manufacture of polyster fibre sewing thread according to claim 1, it is characterized in that, described step 2) in polycondensation catalyst be selected from one in antimony glycol, antimony acetate or antimonous oxide, the theoretical yield weight that the consumption of polycondensation catalyst obtains polyester based on polycondensation is benchmark, counts 180 ~ 300ppm/kg with antimony ion.
6. the preparation method of the low-melting point polyester for the manufacture of polyster fibre sewing thread according to claim 1, is characterized in that, at 80 DEG C ~ 120 DEG C between the melting zone of described low-melting point polyester, limiting viscosity is between 0.4dl/g ~ 0.6dl/g.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310471710.8A CN104558560A (en) | 2013-10-11 | 2013-10-11 | A preparing method of low-melting point polyester used for manufacturing terylene sewing threads |
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| CN201310471710.8A CN104558560A (en) | 2013-10-11 | 2013-10-11 | A preparing method of low-melting point polyester used for manufacturing terylene sewing threads |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106750219A (en) * | 2017-01-10 | 2017-05-31 | 扬州富威尔复合材料有限公司 | A kind of low-melting point polyester and preparation method thereof |
| CN107033334A (en) * | 2017-04-26 | 2017-08-11 | 厦门象屿兴泓特种材料有限公司 | A kind of low-melting point polyester and preparation method thereof |
| TWI650343B (en) * | 2016-08-31 | 2019-02-11 | 匯維仕股份公司 | Polyester fiber with advanced adhesive strength for binders |
| CN109957099A (en) * | 2019-02-28 | 2019-07-02 | 宜兴新乐祺纺织印染有限公司 | A kind of production method of low melting point anionic copolymerization type modified poly ester |
| CN109972408A (en) * | 2019-02-28 | 2019-07-05 | 宜兴新乐祺纺织印染有限公司 | A kind of production method that anion chemical fibre web surface is modified |
| CN110952161A (en) * | 2019-12-16 | 2020-04-03 | 扬州富威尔复合材料有限公司 | Low-melting-point elastic polyester fiber and preparation method thereof |
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2013
- 2013-10-11 CN CN201310471710.8A patent/CN104558560A/en active Pending
Non-Patent Citations (3)
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| 林兵生等: ""低熔点聚酯的合成与性能研究"", 《合成纤维工业》 * |
| 王雁: ""低熔点聚酯的合成及应用研究"", 《石油化工技术与经济》 * |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI650343B (en) * | 2016-08-31 | 2019-02-11 | 匯維仕股份公司 | Polyester fiber with advanced adhesive strength for binders |
| CN106750219A (en) * | 2017-01-10 | 2017-05-31 | 扬州富威尔复合材料有限公司 | A kind of low-melting point polyester and preparation method thereof |
| CN106750219B (en) * | 2017-01-10 | 2018-10-19 | 扬州富威尔复合材料有限公司 | A kind of low-melting point polyester and preparation method thereof |
| CN107033334A (en) * | 2017-04-26 | 2017-08-11 | 厦门象屿兴泓特种材料有限公司 | A kind of low-melting point polyester and preparation method thereof |
| CN109957099A (en) * | 2019-02-28 | 2019-07-02 | 宜兴新乐祺纺织印染有限公司 | A kind of production method of low melting point anionic copolymerization type modified poly ester |
| CN109972408A (en) * | 2019-02-28 | 2019-07-05 | 宜兴新乐祺纺织印染有限公司 | A kind of production method that anion chemical fibre web surface is modified |
| CN110952161A (en) * | 2019-12-16 | 2020-04-03 | 扬州富威尔复合材料有限公司 | Low-melting-point elastic polyester fiber and preparation method thereof |
| CN110952161B (en) * | 2019-12-16 | 2021-06-29 | 扬州富威尔复合材料有限公司 | Low-melting-point elastic polyester fiber and preparation method thereof |
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Application publication date: 20150429 |