CN101993526A - Preparation method for polyester for manufacturing full-dull superfine fiber - Google Patents
Preparation method for polyester for manufacturing full-dull superfine fiber Download PDFInfo
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- CN101993526A CN101993526A CN2009100566441A CN200910056644A CN101993526A CN 101993526 A CN101993526 A CN 101993526A CN 2009100566441 A CN2009100566441 A CN 2009100566441A CN 200910056644 A CN200910056644 A CN 200910056644A CN 101993526 A CN101993526 A CN 101993526A
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- titanium dioxide
- slurries
- polyester
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- matting agent
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Abstract
The invention provides a preparation method for polyester for manufacturing a full-dull superfine fiber, which sequentially comprises the following steps of: carrying out esterification reaction on phthalic acid and glycol to generate bis-hydroxyethyl terephthalatel; carrying out pre-polycondensation reaction on the bis-hydroxyethyl terephthalatel to generate oligopolymers; and carrying out polycondensation reaction on the oligopolymers to generate ethylene glycol terephthalate. Glycol based titanium dioxide flatting agent slurry is added into reaction raw materials of the pre-polycondensation and consists of anatase titanium dioxide powdery particles for chemical fiber extinction with the average particle diameter between 0.2 and 0.8 mu, dispersing stabilizing agent and the balance of glycol, wherein at least 50wt% of the anatase titanium dioxide powdery particles have the particle diameter not more than 0.5mu m, the content of the titanium dioxide powdery particle in the slurry is between 8 and 30wt%, the dispersing stabilizing agent is low polymer of aluminum/barium bimetallic organic complex compounds and has the polymerization degree between 60 and 120, the content of the dispersing stabilizing agent in the slurry is between 0.03 and 1.00wt%.
Description
Technical field
The present invention relates to a kind of manufacture method of polyethylene terephthalate, particularly be used to make the manufacture method of the polyethylene terephthalate of full-dull ultra-fine fibre.
Background technology
Generally, the fiber that filament number is lower than 0.55dtex is called as ultra-fine fibre, and wherein topmost is polyester superfine fibre.The appearance of fabrics style of polyester superfine fibre and feel are all very special, bulk, soft, smooth, and absorbing sweat is not and next to the shin, and after sand washing, napping arrangement, the surface can form the fine hair of similar peach skin, is usually used in making artificial suede.Polyester superfine fibre is very soft, makes cleaning and is furnished with fabulous scrubbing effect.In addition, the polyester superfine fibre fabric also can be used for multiple fields such as health care, labour protection.
As the trevira of common specification, when the polyester superfine fibre fabric was used to take or decorates, the delustring of fiber was normally necessary.The delustring trevira divides half delustring and full-dull two classes, and half delustring dacron fabric surface luster is still apparent in view, and the cured texture of fiber is also stronger, is difficult to use in expensive goods, and the polyester of therefore making the full-dull ultra-fine fibre has the bigger market requirement.
The chemical fibre matting agent is most at present to use titanium dioxide (to be commonly called as: powdered granule titanium dioxide), titanium dioxide has higher specific refractory power, whiteness is good, opacifying power is big, and has better chemical stability, the aftertreatment of chemical fibre and post-treatment process are difficult for changing, do not influence the dyeing of fiber, and can improve the photostabilization and the weathering resistance of fiber.The diameter of polyester superfine fibre is minimum, the TITANIUM DIOXIDE DELUSTRANT addition of whole extinction polyester fiber is 8～10 times of half delustring in addition, this just not only requires titanium dioxide granule that enough little particle diameter is arranged, and fabulous dispersiveness is arranged, otherwise very easily make filament spinning component stop up in the spinning process, even cause fibre breakage in spinning or drafting process.Yet the titanium dioxide solid particles surface that particle diameter is so little can be very big, very easily reunites.In the prior art, in order to guarantee that titanium dioxide can be scattered in the polyester equably, titanium dioxide granule needs to mix with ethylene glycol earlier, again through stirring to pulp, shear mill, titanium dioxide matting agent slurries that a series of processing treatment such as filtration is deployed into ethylene glycol, then before the production process polyester of polyester generates in the adding reaction system.Although the matting agent slurries are to allocate according to the demand of production of polyester is instant usually, but in fact, allotment finishes until adding the reaction system that polyester is made, and produces aggregated particle thereby still have the regular hour to make in the matting agent slurries part titanium dioxide granule take place to reunite.Trevira for conventional fiber number is made; the aggregated particle of these quantity is not sufficient to cause the post-treatment of fiber tangible production problem to occur in using in the polyester slice; but far different for the manufacturing of polyester superfine fibre, can show usually that the spinning end breakage rate obviously improves the full-rolling rate of the continuous yarn spinning (reduce), filament spinning component stops up and makes life cycle reduce.
Summary of the invention
The invention provides a kind of preparation method who is used to make the polyester of full-dull ultra-fine fibre, it is by the improvement to the titanium dioxide matting agent slurry formula that adds in the polyester manufacturing processed, can make the agglomeration basically eliminate of titanium dioxide granule, dispersiveness and the homogenizing degree of titanium dioxide in polyester product improves greatly, when polyester slice is used to make the full-dull polyester superfine fibre, end breakage rate greatly reduces, and the life cycle of filament spinning component obviously improves.
Below be the concrete technical scheme of the present invention:
A kind of preparation method who is used to make the polyester of full-dull ultra-fine fibre, this method comprise that successively terephthalic acid and ethylene glycol carry out esterification and generates bishydroxyethyl terephthalate; Bishydroxyethyl terephthalate carries out prepolymerization reaction and generates oligopolymer; Oligopolymer carries out polycondensation and generates polyethylene terephthalate.
It is characterized in that adding in the reaction raw materials of prepolymerization reaction the titanium dioxide matting agent slurries of ethylene glycol, it consists of:
1) chemical fibre delustring anatase titanium dioxide powdered granule, its median size is 0.2～0.8 μ, the grain diameter of at least 50 weight %≤0.5 μ wherein, titanium dioxide powdery particulate content is 8～30wt% in the slurries;
2) dispersion stabilizer is the oligopolymer of aluminium/barium bimetal organic complex, and its polymerization degree is 60～120, and the content of dispersion stabilizer is 0.03～1.00wt% in the slurries;
3) ethylene glycol, the surplus in the slurries except that titanium dioxide powdery particle and dispersion stabilizer are ethylene glycol.
In the above-mentioned titanium dioxide matting agent slurries, titanium dioxide powdery particulate content is preferably 10～25wt%; The content of dispersion stabilizer is preferably 0.06～0.70wt%.
The add-on of titanium dioxide matting agent slurries is a benchmark with the amount of oligopolymer in the reaction raw materials in the reaction raw materials of above-mentioned polycondensation, and in the amount of titanium dioxide in the slurries, is generally 1.85～3.50wt%, is preferably 2.50～3.00wt%.
In technical scheme provided by the invention, its key is to have added a kind of oligopolymer of bimetal organic complex as dispersion stabilizer in titanium dioxide matting agent slurries, it and titanium dioxide granule have very strong bonding force, with ethylene glycol good intermiscibility are arranged again simultaneously.The contriver found through experiments, after dissolving in this dispersion stabilizer in right amount in the ethylene glycol, the dispersibility of titanium dioxide granule greatly strengthens, and can keep the suspended state of high dispersing for a long time, solved titanium dioxide granule effectively and secondary agglomeration easily takes place produced this technical problem of aggregated particle.Adopt that the titanium dioxide matting agent has the dispersiveness of height in the polyester that this titanium dioxide matting agent slurries make.Application test is the result show, (life cycle of filament spinning component obviously improves in the process of filament number≤0.55dtex), and the full-rolling rate of long filament also can be brought up to more than 95% from being lower than 90% making full-dull polyester microfilament.Compared with prior art, positively effect of the present invention is very remarkable.
Below will the invention will be further described by specific embodiment.
In order to estimate positively effect of the present invention, it is the ultra-fine DTY of full-dull polyester of 56dtex/144F that the polyester slice that each embodiment is made adopts the polyester filament spinning experimental installation at single position to make specification, and investigates its full-rolling rate.
Embodiment
[embodiment 1～7]
In esterifying kettle, terephthalic acid and ethylene glycol are carried out esterification generation bishydroxyethyl terephthalate, in the precondensation still, bishydroxyethyl terephthalate is carried out prepolymerization reaction then and generate oligopolymer; In whole polycondensation vessel, oligopolymer is carried out polycondensation then and generate the polyethylene terephthalate section.
Add the titanium dioxide matting agent slurries of ethylene glycol in the reaction raw materials of prepolymerization reaction, the component of matting agent slurries is:
1) chemical fibre delustring anatase titanium dioxide powdered granule, its median size is 0.2～0.8 μ, wherein the grain diameter of at least 50 weight %≤0.5 μ;
2) dispersion stabilizer, this dispersion stabilizer are the oligopolymer of aluminium/barium bimetal organic complex, and its polymerization degree is 60～120;
3) ethylene glycol.
Among each embodiment, each components contents of matting agent slurries sees Table 1, and the amount of ethylene glycol is the surplus except that titanium dioxide powdery particle and dispersion stabilizer in the slurries.The add-on of matting agent slurries is a benchmark with the amount of oligopolymer in the polycondensation raw material, and in the amount of titanium dioxide in the slurries, concrete data see Table 1.
[comparative example]
Do not have dispersion stabilizer in the component of matting agent slurries, all the other are with embodiment 1～7.
It is the ultra-fine DTY of full-dull polyester of 56dtex/144F that the polyester slice that each embodiment and comparative example make adopts the polyester filament spinning experimental installation at 6 positions to make specification, and investigates its full-rolling rate.The results are shown in Table 1.
Table 1.
Claims (5)
1. preparation method who is used to make the polyester of full-dull ultra-fine fibre, this method comprises that successively terephthalic acid and ethylene glycol carry out esterification and generates bishydroxyethyl terephthalate; Bishydroxyethyl terephthalate carries out prepolymerization reaction and generates oligopolymer; Oligopolymer carries out polycondensation and generates polyethylene terephthalate,
It is characterized in that adding in the reaction raw materials of prepolymerization reaction the titanium dioxide matting agent slurries of ethylene glycol, it consists of:
1) chemical fibre delustring anatase titanium dioxide powdered granule, its median size is 0.2～0.8 μ, the grain diameter of at least 50 weight %≤0.5 μ wherein, titanium dioxide powdery particulate content is 8～30wt% in the slurries;
2) dispersion stabilizer is the oligopolymer of aluminium/barium bimetal organic complex, and its polymerization degree is 60～120, and the content of dispersion stabilizer is 0.03～1.00wt% in the slurries;
3) ethylene glycol, the surplus in the slurries except that titanium dioxide powdery particle and dispersion stabilizer are ethylene glycol.
2. the preparation method of polyester according to claim 1 is characterized in that in the described titanium dioxide matting agent slurries, titanium dioxide powdery particulate content is 10～25wt%.
3. the preparation method of polyester according to claim 1 is characterized in that the content of dispersion stabilizer is 0.06～0.70wt% in the described titanium dioxide matting agent slurries.
4. the preparation method of polyester according to claim 1, the add-on that it is characterized in that titanium dioxide matting agent slurries in the reaction raw materials of described polycondensation is a benchmark with the amount of oligopolymer in the reaction raw materials, and, be 1.85～3.50wt% in the amount of titanium dioxide in the slurries.
5. the preparation method of polyester according to claim 4, the add-on that it is characterized in that titanium dioxide matting agent slurries in the reaction raw materials of described polycondensation is a benchmark with the amount of oligopolymer in the reaction raw materials, and, be 2.50～3.00wt% in the amount of titanium dioxide in the slurries.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100566441A CN101993526A (en) | 2009-08-19 | 2009-08-19 | Preparation method for polyester for manufacturing full-dull superfine fiber |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100566441A CN101993526A (en) | 2009-08-19 | 2009-08-19 | Preparation method for polyester for manufacturing full-dull superfine fiber |
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| CN101993526A true CN101993526A (en) | 2011-03-30 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103756368A (en) * | 2014-01-07 | 2014-04-30 | 江苏长乐纤维科技有限公司 | Preparation method of matting agent product |
| CN108026385A (en) * | 2015-10-30 | 2018-05-11 | 克洛诺斯国际有限公司 | Delustering agent and its production method |
| CN109338496A (en) * | 2018-10-15 | 2019-02-15 | 龙游龙纤新材料有限公司 | A kind of preparation method of delustring ultra high molecular weight polyethylene fiber |
| CN109943892A (en) * | 2019-03-01 | 2019-06-28 | 江苏三联新材料有限公司 | A kind of super fine denier directly spins the production technology of full-dull polyester filament |
| CN111411410A (en) * | 2020-05-21 | 2020-07-14 | 沪本新材料科技（上海）有限公司 | Liquid titanium dioxide for synthetic delustering polyester fiber |
-
2009
- 2009-08-19 CN CN2009100566441A patent/CN101993526A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103756368A (en) * | 2014-01-07 | 2014-04-30 | 江苏长乐纤维科技有限公司 | Preparation method of matting agent product |
| CN108026385A (en) * | 2015-10-30 | 2018-05-11 | 克洛诺斯国际有限公司 | Delustering agent and its production method |
| CN109338496A (en) * | 2018-10-15 | 2019-02-15 | 龙游龙纤新材料有限公司 | A kind of preparation method of delustring ultra high molecular weight polyethylene fiber |
| CN109338496B (en) * | 2018-10-15 | 2021-04-13 | 龙游龙纤新材料有限公司 | Preparation method of extinction ultrahigh molecular weight polyethylene fiber |
| CN109943892A (en) * | 2019-03-01 | 2019-06-28 | 江苏三联新材料有限公司 | A kind of super fine denier directly spins the production technology of full-dull polyester filament |
| CN111411410A (en) * | 2020-05-21 | 2020-07-14 | 沪本新材料科技（上海）有限公司 | Liquid titanium dioxide for synthetic delustering polyester fiber |
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Application publication date: 20110330 |