CN102504217B - Method for preparing special polybutylene terephthalate for high-speed spinning - Google Patents
Method for preparing special polybutylene terephthalate for high-speed spinning Download PDFInfo
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Abstract
The invention discloses a method for preparing a special raw material for high-speed spinning and belongs to the technical field of synthetic fiber production. The special raw material for the high-speed spinning is prepared from the following materials: purified terephthalic acid, an antifoaming agent, a stabilizer, a flexibilizer, a catalyst and a toner. The method for preparing polybutylene terephthalate from the raw material comprises the following steps of: 1, preparing the catalyst; 2, preparing slurry; 3, carrying out esterification; 4, carrying out pre-polycondensation; and 5, carrying out final polycondensation and finally feeding the obtained product to a dicing workshop section to carry out dicing. Currently, no special PBT (polybutylece terephthalate) product for spinning is provided in China. The product obtained by adopting the method for preparing the special polybutylece terephthalate for high-speed spinning has high elasticity and low temperature chromaticity. PBT resin for spinning, which has high crystallization rate and good dyeing property and of which yarns are difficult to break, is particularly suitable for 100 percent pure fiber fabrics, is used for sports wears and swimsuits and can also be blended with other fibers.
Description
Technical field: patent of the present invention relates to a kind of preparation method of high speed spinning special raw material, belongs to the synthon production technical field.
Background technology: polybutylene terephthalate (PBT) is to be made through chemical reaction by terephthalic acid (PTA) and 1.4-butyleneglycol (BDO).Have physical strength high, the characteristics that the engineering plastics such as the mechanical property such as tensile strength, Young's modulus and polyoxymethylene, nylon are similar can be widely used in the industries such as electronic apparatus, automobile, weaving and optical cable.At present domestic each PBT fiber production producer all adopts common PBT or modified PBT to carry out spinning.But common PBT carry out spinning exist easy fracture of wire, painted inhomogeneous, from the problem such as loose.Domestic have the producers such as Yizheng Fiber Optical plant setting about the research of spinning PBT resin at present; but mainly still concentrate on common PBT is carried out modification; then be used for carrying out spinning, for example the patented technology " a kind of synthetic method of PBT color spinning " of Jiangsu Xing Hai chemical fibre company limited and the graduate patented technology of Shanghai Petrochem. General Plant " fiber with the research of modified PBT resin " are all PBT to be carried out modification then carry out spinning.And domestic at present also not about the relevant criterion of spinning with the PBT resin.
Summary of the invention: the purpose of this invention is to provide a kind of special polybutylene terephthalate for high-speed spinning, can produce that crystallization velocity is fast, tint permanence good, be difficult for the spinning PBT resin of fracture of wire with this method.This special polybutylene terephthalate for high-speed spinning adopts following proportioning raw materials: pure terephthalic acid (PTA) 56-65%, 1.4-butyleneglycol (BDO) 35-44%, antifoam content accounts for the 0.0001-0.0005% of raw material weight, stabiliser content accounts for the 0.002-0.006% of raw material weight, toughner content accounts for the 0.5-2.0% of raw material weight, catalyst content accounts for the 0.05-0.2% of raw material weight, and toner content accounts for the 0.0006-0.003% of raw material weight.
Described defoamer is polydimethylsiloxane or silicon ether grafts; Described stablizer is phosphoric acid or dimethyl phosphate; Described toughner is phthalein white powder or talcum powder; Described catalyzer is phthalandione four butyl ester compounds; Described toning agent is the purple agent that food adds.
Utilize above-mentioned raw materials to produce polybutylene terephthalate, comprise the following steps:
1, catalyst arrangement adds the catalyst arrangement tank with tetrabutyl titanate, opens and stirs, and catalyst arrangement tank chuck heats with liquid heat medium.Add the 1.4-butyleneglycol after being heated to 110-130 ℃, control vacuum tightness and be warming up to 170-190 ℃ of reaction 2-3h under 180-220mbar.The catalyzer that configures quantitatively adds esterifier with toothed gear pump.
2, the configuration of slurry, liquid butyleneglycol and solid pure terephthalic acid through metering system with 1: 1.1-1.3 mol ratio continuous uniform adds in the slurry configured slot and stirs, and defoamer, toning agent are added in the slurry configured slot by the proportioning continuous uniform, quantitatively add esterifier with volume pump after being mixed into uniform sizing material.
3, esterification, slurry and catalyzer add esterifier by volume pump, and esterifier heats with heating agent biphenyl.Esterification reaction temperature 242-246 ℃, vacuum tightness 400～430mbar.Material generates the two hydroxyl butyl esters (BHBT) of terephthalic acid at esterifier lactonization reaction 110-120min, and the material after esterification is completed is quantitatively transferred to the preshrunk reactor by the esterifier discharging pump.
4, precondensation, the two hydroxyl butyl esters (BHBT) of terephthalic acid that come from esterifier enter Prepolycondensating reactor, then continuous uniform adds toughner and stablizer.The operational condition of Prepolycondensating reactor is 243～245 ℃ of temperature, vacuum tightness 15～20mbr, reaction times 30-45min.Filter and pass through through the prepolymer strainer after product pressurizes with the prepolymer charge pump and enter final polycondensation reactor after prepolymer carries water cooler to regulate temperature.
5, final minification is poly-, and the material that comes from Prepolycondensating reactor is continuously fed into final polycondensation reactor.The final polycondensation reactor operational condition is 242～248 ℃ of temperature, vacuum tightness 1-3mbar, reaction times 2-3h.Reaction product is by the pressurization of polymkeric substance discharging pump, through the in-line viscometer monitoring viscosity.Product is sent to the pelletizing of pelletizing workshop section after polymer filter filters.
The present domestic PBT product that also is not specifically designed to spinning, the product that adopts special polybutylene terephthalate for high-speed spinning to obtain is to have snappiness, low temperature dyeing, crystallization velocity is fast, tint permanence good, be difficult for the spinning PBT resin of fracture of wire, be particularly useful for 100% pure fabric, be used for Sportswear and swimsuit, also can with other fiber blends.
Description of drawings: Fig. 1 is the process flow diagram of special polybutylene terephthalate for high-speed spinning.
Embodiment: be further described below in conjunction with accompanying drawing.
Polybutylene terephthalate (PBT) is to be made through chemical reaction by terephthalic acid (PTA) and 1.4-butyleneglycol (BDO).Need add some ancillary components in reaction process, kind and the proportioning of various materials used are as follows:
Pure terephthalic acid (PTA) 56-65%, 1.4-butyleneglycol (BDO) 35-44%, antifoam content accounts for the 0.0001-0.0005% of raw material weight, stabiliser content accounts for the 0.002-0.006% of raw material weight, toughner content accounts for the 0.5-2.0% of raw material weight, catalyst content accounts for the 0.05-0.2% of raw material weight, and toner content accounts for the 0.0006-0.003% of raw material weight.
Described defoamer is polydimethylsiloxane or silicon ether grafts; Described stablizer is phosphoric acid or dimethyl phosphate; Described toughner is phthalein white powder or talcum powder; Described catalyzer is phthalandione four butyl ester compounds; Described toning agent is the purple agent that food adds.
The special-purpose poly-terephthaldehyde 1.4-butyleneglycol acid butanediol ester preparation method of high speed spinning describes with an embodiment, and its technical process as shown in drawings.
The tetrabutyl titanate of 100kg is added the catalyst arrangement tank, heat and stir with liquid heat medium.Add 1.4-butyleneglycol 158.9kg after being heated to 110 ℃, control vacuum tightness and be warming up to 180 ℃ of reaction 3h under 200mbar, be configured to catalyzer.
Get 758 parts of pure terephthalic acids, 496 parts of 1.4-butyleneglycols, 0.002 part of defoamer, 0.0007 part of toning agent drops into the slurry configured slot and carries out the slurry preparation.Material in groove through stirring, be mixed into uniform sizing material.
Slurry enters esterifier together with 1.2 parts of volume pump and catalyzer.242 ℃ of esterification reaction temperatures, vacuum tightness 420mbr in esterifier, generates the two hydroxyl butyl esters (BHBT) of terephthalic acid and more high molecular oligopolymer after terephthalic acid and the water outlet of butyleneglycol Reaction Separation.The vacuum of reaction needed is produced by central vacuum system.It is poly-that this vacuum system is used for precondensation and final minification simultaneously.Material stops 110min in esterifier, carry out esterification, and esterification yield can reach 99.5%.The by product of separating in esterification process reclaims by rectifying tower.
The two hydroxyl butyl esters (BHBT) of esterification products terephthalic acid and 0.044 part of stablizer, 8 parts of toughner enter Prepolycondensating reactor together, and the operational condition of Prepolycondensating reactor is 243 ℃ of temperature, vacuum tightness 18mbr, reaction times 45min.。Obtain low molecule PBT through prepolymerization reaction.Filter and pass through through the prepolymer strainer after product pressurizes with the prepolymer charge pump and enter final polycondensation reactor after prepolymer carries water cooler to regulate temperature.
The precondensation product enters final polycondensation reactor, and the disk that rotates has been installed in final polycondensation reactor, and these disks can drive polymkeric substance and form the surface of rotating, and are conducive to the discharge of low molecule by product.The final polycondensation reactor operational condition is 245 ℃ of temperature, vacuum tightness 1mbr, reaction times 3h.Reaction product is by the pressurization of polymkeric substance discharging pump, through the in-line viscometer monitoring viscosity.Product is sent to pelletizing workshop section after polymer filter filters.
Temperature, pressure and reaction times in each reaction process of choose reasonable can obtain high-quality polymeric articles.Finally by pelletizing, be packaged to finished product.
Final polymer should satisfy following key index: limiting viscosity is that 1.006 ± 0.015dl/g carboxyl is that 17 ± 2mol/t aggregated particle is that 55 ± 5MPa elongation at break is 〉=250% for≤1/mg tensile strength.
Claims (2)
1. special polybutylene terephthalate for high-speed spinning, comprise the with slurry material, esterification, polycondensation, the operations such as pelletizing, it is characterized in that: this preparation method adopts following proportioning raw materials: pure terephthalic acid (PTA) 56-65%, 1.4-butyleneglycol (BDO) 35-44%, antifoam content accounts for the 0.0001-0.0005% of raw material weight, stabiliser content accounts for the 0.002-0.006% of raw material weight, toughner content accounts for the 0.5-2.0% of raw material weight, catalyst content accounts for the 0.05-0.2% of raw material weight, toner content accounts for the 0.0006-0.003% of raw material weight, this preparation method adopts following operation steps,
1., catalyst arrangement, tetrabutyl titanate is added the catalyst arrangement tank, open and stir, catalyst arrangement tank chuck heats with liquid heat medium, add the 1.4-butyleneglycol after being heated to 110-130 ℃, control vacuum tightness and be warming up to 170-190 ℃ of reaction 2-3h under 180-220mbar, the catalyzer that configures adds the catalyzer feed pot, after quantitatively add esterifier with toothed gear pump again;
2., the configuration of slurry, liquid butyleneglycol and solid pure terephthalic acid through metering system with mol ratio 1: the 1.1-1.3 continuous uniform adds in the slurry configured slot and stirs, and defoamer, toning agent are added in the slurry configured slot by the proportioning continuous uniform, quantitatively add esterifier with volume pump after being mixed into uniform sizing material;
3., esterification, slurry and catalyzer add esterifier by volume pump, esterifier is with the heating of heating agent biphenyl, esterification reaction temperature 242-246 ℃, vacuum tightness 400～430mbar; Material is at esterifier lactonization reaction 110-120min, and the material after esterification is completed is quantitatively transferred to the preshrunk reactor by the esterifier discharging pump;
4., precondensation, the two hydroxyl butyl esters (BHBT) of terephthalic acid that come from esterifier enter Prepolycondensating reactor, then continuous uniform adds toughner and stablizer; The operational condition of Prepolycondensating reactor is 243～245 ℃ of temperature, vacuum tightness 15～20mbar, filter and pass through through the prepolymer strainer after reaction times 30-45min, product pressurize with the prepolymer charge pump and enter final polycondensation reactor after prepolymer carries water cooler to regulate temperature;
5., final minification is poly-, the material that comes from Prepolycondensating reactor is continuously fed into final polycondensation reactor; The final polycondensation reactor operational condition is 242～248 ℃ of temperature, vacuum tightness 1-3mbar, reaction times 2-3h; Reaction product is by polymkeric substance discharging pump pressurization, and through the in-line viscometer monitoring viscosity, product is sent to the pelletizing of pelletizing workshop section after polymer filter filters.
2. special polybutylene terephthalate for high-speed spinning as claimed in claim 1, it is characterized in that: in proportioning raw materials, described defoamer is polydimethylsiloxane or silicon ether grafts; Described stablizer is phosphoric acid or dimethyl phosphate; Described toughner is phthalein white powder or talcum powder; Described catalyzer is phthalandione four butyl ester compounds; Described toning agent is the purple agent that food adds.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103642012A (en) * | 2013-10-30 | 2014-03-19 | 新疆蓝山屯河聚酯有限公司 | Method for preparing high-flow and high-modulus polybutylene terephthalate |
| CN104195653A (en) * | 2014-07-29 | 2014-12-10 | 中国石油化工股份有限公司 | PBT fiber manufacturing method based on high speed one-step method |
| CN105088383A (en) * | 2015-09-02 | 2015-11-25 | 太仓市宏亿化纤有限公司 | PBT (polybutylene terephthalate) fiber production technology |
| CN106008939A (en) * | 2016-07-28 | 2016-10-12 | 中国纺织科学研究院 | Black PET as well as preparation method and device thereof and black PET fiber as well as preparation method, device and application thereof |
| CN106519196A (en) * | 2016-10-27 | 2017-03-22 | 南通星辰合成材料有限公司 | Method for manufacturing high-quality PBT basic resin applied to nano injection molding |
| CN107955992A (en) * | 2017-10-19 | 2018-04-24 | 无锡市兴盛新材料科技有限公司 | A kind of short fine and its fused mass directly spinning preparation methods of high-quality PBT |
| CN108484890A (en) * | 2018-02-02 | 2018-09-04 | 桐昆集团股份有限公司 | A kind of production technology and production system producing multifunctional different PBT polyester |
| CN109206597A (en) * | 2018-08-29 | 2019-01-15 | 江苏鑫博高分子材料有限公司 | Polybutylene terephthalate (PBT) resin and preparation method thereof |
| CN109232873A (en) * | 2018-08-29 | 2019-01-18 | 江苏鑫博高分子材料有限公司 | The preparation facilities of polybutylene terephthalate (PBT) resin |
| CN109529753A (en) * | 2019-01-14 | 2019-03-29 | 扬州惠通化工科技股份有限公司 | A kind of PBT esterification system |
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| CN101824143A (en) * | 2010-03-08 | 2010-09-08 | 江阴和时利工程塑胶科技发展有限公司 | Preparation method of high crystallization thermoplastics type polybutylene terephthalate slice |
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| CN101824143A (en) * | 2010-03-08 | 2010-09-08 | 江阴和时利工程塑胶科技发展有限公司 | Preparation method of high crystallization thermoplastics type polybutylene terephthalate slice |
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Denomination of invention: Preparation of high speed spinning special polybutylene terephthalate Effective date of registration: 20201116 Granted publication date: 20130522 Pledgee: Agricultural Development Bank of China Changji Hui Autonomous Prefecture Branch Business Department Pledgor: XINJIANG BLUE RIDGE TUNHE POLYESTER Co.,Ltd. Registration number: Y2020990001352 |