CN102504217A - 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 the physical strength height, the similar characteristics of engineering plastics such as mechanical property such as tensile strength, Young's modulus and polyoxymethylene, nylon can be widely used in industries such as electronic apparatus, automobile, weaving and optical cable.Domestic each PBT fiber production producer all adopts common PBT or modified PBT to carry out spinning at present.But common PBT carry out spinning exist to be prone to fracture of wire, painted inhomogeneous, from problem such as loose.Domestic have 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; Be used to carry out spinning then, for example patented technology of Jiangsu Xing Hai chemical fibre ltd " a kind of compound method of PBT color spinning " and the graduate patented technology of Shanghai Petrochem. General Plant " fiber is with the research of modified PBT resin " all are PBT to be carried out modification carry out spinning then.And it is 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 the special-purpose polybutylene terephthalate preparation method of a kind of high speed spinning, with this method can produce that crystallization velocity is fast, tint permanence good, the spinning that is difficult for fracture of wire uses the PBT resin.The special-purpose polybutylene terephthalate preparation method of this 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, and stabiliser content accounts for the 0.002-0.006% of raw material weight, and 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 skimmer is YSR 3286 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, catalyzer configuration adds the catalyzer batch tank with tetrabutyl titanate, opens and stirs, and catalyzer batch tank chuck heats with liquid heat medium.Add the 1.4-butyleneglycol after being heated to 110-130 ℃, control vacuum tightness is 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 process metering system are with 1: the 1.1-1.3 mol ratio evenly stirs in the adding slurry configured slot continuously; And skimmer, toning agent evenly added in the slurry configured slot by proportioning continuously, quantitatively add esterifier with volume pump after being mixed into uniform sizing material.
3, esterification, slurry and catalyzer add esterifier through 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 accomplished is quantitatively transferred to the preshrunk reactor drum by the esterifier discharging pump.
4, precondensation, the two hydroxyl butyl esters (BHBT) of terephthalic acid that come from esterifier get into Prepolycondensating reactor, evenly add toughner and stablizer more continuously.The operational condition of Prepolycondensating reactor is 243～245 ℃ of temperature, vacuum tightness 15～20mbr, reaction times 30-45min.After pressurizeing with the prepolymer charge pump, product gets into final polycondensation reactor through the filtration of prepolymer strainer and after passing through prepolymer conveying water cooler attemperation.
5, final minification gathers, and is sent into final polycondensation reactor continuously from the material that Prepolycondensating reactor comes.The final polycondensation reactor operational condition is 242～248 ℃ of temperature, vacuum tightness 1-3mbar, reaction times 2-3h.Reaction product is through 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 the special-purpose polybutylene terephthalate preparation method of high speed spinning to obtain is to have snappiness; Low temperature dyeing property, the PBT resin is used in the spinning that crystallization velocity is fast, tint permanence good, be difficult for fracture of wire, is particularly useful for 100% pure fabric; Be used for tSportswear and swimsuit, also can with other fiber blends.
Description of drawings: Fig. 1 is the special-purpose polybutylene terephthalate preparing method's of high speed spinning a process flow diagram.
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 in the reaction process to add some ancillary components, the kind and the proportioning of used various materials are following:
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, and stabiliser content accounts for the 0.002-0.006% of raw material weight, and 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 skimmer is YSR 3286 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 high speed spinning special use gathers terephthaldehyde 1.4-butyleneglycol acid butanediol ester preparation method, describes with an embodiment, and its technical process is shown in accompanying drawing.
The tetrabutyl titanate of 100kg is added the catalyzer batch tank, with liquid heat medium heating and stirring.Add 1.4-butyleneglycol 158.9kg after being heated to 110 ℃, control vacuum tightness is 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 skimmer, 0.0007 part of toning agent drops into the slurry configured slot and carries out pulp preparation.Material warp in groove stirs, is mixed into uniform sizing material.
Slurry gets into esterifier through volume pump for 1.2 parts with catalyzer.242 ℃ of esterification reaction temperatures, vacuum tightness 420mbr in esterifier, generates 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.This vacuum system is used for precondensation simultaneously and final minification gathers.Material stops 110min in esterifier, carry out esterification, and esterification yield can reach 99.5%.The by product of separating in the esterification process reclaims through rectifying tower.
Two hydroxyl butyl esters (BHBT) of esterification products terephthalic acid and 0.044 part of stablizer, 8 parts of toughner get into 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.After pressurizeing with the prepolymer charge pump, product gets into final polycondensation reactor through the filtration of prepolymer strainer and after passing through prepolymer conveying water cooler attemperation.
The precondensation product gets into final polycondensation reactor, and the disk that rotates has been installed in the final polycondensation reactor, and these disks can drive polymkeric substance and form the surface of rotating, and help 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 through 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.After 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. the special-purpose polybutylene terephthalate preparation method of high speed spinning; Comprise operations such as joining slurry, esterification, polycondensation, pelletizing; It is characterized in that: this preparation method adopts following proportioning raw materials: pure terephthalic acid (PTA) 56-65%, and 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, and 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; This preparation method adopts following operation steps ,+
1., catalyzer configuration, tetrabutyl titanate is added the catalyzer batch tank, open and stir, catalyzer batch tank chuck heats with liquid heat medium.Add the 1.4-butyleneglycol after being heated to 110-130 ℃, control vacuum tightness is 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 evenly stir in the adding slurry configured slot with mol ratio 1: 1.1-1.3 through metering system continuously; And skimmer, toning agent evenly added in the slurry configured slot by proportioning continuously, quantitatively add esterifier with volume pump after being mixed into uniform sizing material;
3., esterification, slurry and catalyzer add esterifier through volume pump, esterifier heats with 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 accomplished is quantitatively transferred to the preshrunk reactor drum by the esterifier discharging pump;
4., precondensation, the two hydroxyl butyl esters (BHBT) of terephthalic acid that come from esterifier get into Prepolycondensating reactor, evenly add toughner and stablizer more continuously.The operational condition of Prepolycondensating reactor is 243～245 ℃ of temperature, vacuum tightness 15～20mbar, reaction times 30-45min.After pressurizeing with the prepolymer charge pump, product gets into final polycondensation reactor through the filtration of prepolymer strainer and after passing through prepolymer conveying water cooler attemperation;
5., final minification gathers, and sent into final polycondensation reactor continuously from the material that Prepolycondensating reactor comes.The final polycondensation reactor operational condition is 242～248 ℃ of temperature, vacuum tightness 1-3mbar, reaction times 2-3h.Reaction product is through 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.
2. the special-purpose polybutylene terephthalate preparation method of high speed spinning as claimed in claim 1, it is characterized in that: in proportioning raw materials, described skimmer is YSR 3286 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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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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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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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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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 |
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