CN85107888A - The manufacture method of durable anti-static polyester resin and fiber - Google Patents

The manufacture method of durable anti-static polyester resin and fiber Download PDF

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CN85107888A
CN85107888A CN 85107888 CN85107888A CN85107888A CN 85107888 A CN85107888 A CN 85107888A CN 85107888 CN85107888 CN 85107888 CN 85107888 A CN85107888 A CN 85107888A CN 85107888 A CN85107888 A CN 85107888A
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manufacture method
polyester resin
temperature
fiber
polycondensation
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CN 85107888
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曹惠椿
朱玉梅
史秀珍
陈宏生
邵晓敏
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SHANGHAI INST OF SYNTHETIC FIBRE
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SHANGHAI INST OF SYNTHETIC FIBRE
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Abstract

The invention provides the manufacture method of a kind of durable anti-static polyester resin and fiber, it is characterized in that adopting the production technology of composite antistatic agent, the following discontinuous phase of antistatic additive can be evenly distributed on resin and fibrous inside.Therefore can avoid occurring in the fiber circuit high-order resistance and electric current gathering etc. to obtain bigger antistatic effect.The half-life of product is less than 60 seconds, and friction voltage is less than 200 volts, than resistance less than 10 10Ohm-centimetre, constant through 20 standard washings, be applicable to desirable supplementary material in industry manufacturings such as making dust-free clothes, aseptic clothing, anti-blast clothing etc., particularly precision instrument, integrated circuit, computer and the application process.

Description

The manufacture method of durable anti-static polyester resin and fiber
The invention relates to antistatic additive and be added on fibrous inside to make the technology of durable anti-static polyester resin and fiber.
As everyone knows, terylene is hydrophobic organic high molecular compound, and it can not ionization, does not have free electron again, and therefore the very easy electric charge that gathers causes all consequences, has a strong impact on use value.At present, the method for eliminating terylene static mainly contains two kinds, and the one, surface treatment is promptly at the surperficial coated antistatic additive of fiber and fabric thereof; The 2nd, basic modification, promptly add antistatic additive at fibrous inside to give its antistatic property.Obviously, the former is because in processing, dyeing and finishing, washing and use, the fiber surface antistatic additive loses easily, so antistatic effect often can not be lasting.So the trend since the eighties is to adopt the latter to produce persistent anti-electrostatic polyester fiber.
Up to now, most in the past number average adopts the interior adding technology route of single type antistatic additive, with development or production anti-electrostatic polyester long filament.
The antistatic additive that belongs to this single type has poly-aryl to gather propyl sulfonic acid na phosphates, aliphatic alcohol polyoxyvinethene phosphate, 2,4 polyoxyethylene groups, 6 Aminocaproic Acid s-triazine, polystyrene sodium salt (80%) and polystyrene amine salt (20%) etc.Select the product of above-mentioned prescription gained in the market for use, the antistatic effect that has is not good, and the then durability that has is bad.Adopt in the aliphatic alcohol polyoxyvinethene phosphate as Japan Patent JP4736459 system to be added on prepared fiber in the polyester resin, though it antistaticly has a durability, effect is bad, fails to reach the technical indicator of making dust-free clothes and aseptic clothing.
The objective of the invention is to adopt the deficiency of adding antistatic additive in the single type, provide a kind of and can produce the high and durable polyester resin of antistatic efficient and the new technology of fiber thereof in order to overcome.
Main points of the present invention, it comprises the manufacturing and the fibre forming process of anti-electrostatic polyester resin, it is characterized in that adopting polyoxyethylene or polyether compound and alkylsulfonate or phosphate compounds to carry out the polyester resin of compound antistatic compounded technology and the technological process that long filament is produced.Belong to the compound antistatic additive of alkylsulfonate or phosphate and polyoxyethylene compound and be called CA type antistatic additive, polyethers or polyoxyethylene compounds are called CA-1 type antistatic additive, and alkylsulfonate or phosphate one compounds are called CA-2 type antistatic additive.
The proportioning of CA-1 type and CA-2 type has considerable influence to antistatic effect, make that CA-2 is fine to be contained among the CA-1 type, guarantees that the CA-1 type is arranged vertically and definite reasonable distribution ratio is vital.Following table 1 and table 2 are classified the test data of CA-1 type and the different additions of CA-2 type as.
Figure 85107888_IMG1
By above-mentioned two tables as can be seen, when CA-1 type addition surpassed 6%, though antistatic effect increases, the condensate spinnability was poor, processing difficulties.When surpassing 10%, then can't process.
The content of CA-2 type fiber antistatic effect in 6% scope is remarkable, surpasses this and is worth then that antistatic effect does not have significant change, causes many, the processing difficulties of fiber lousiness on the contrary.
As fully visible, the CA-1 type is 3: 1~5: 4 with the ratio of CA-2 type, is preferably 5: 3.
Because the CA-2 type is dissolved in alcohol,,, generally after high vacuum, add more suitable in order to avoid take out of with the evaporation of methyl alcohol or ethylene glycol so the CA-2 type is not suitable for adding before polycondensation finishes.
The adding mode of CA-1 type is distributed with very big influence for it in fiber.Confirm according to the analysis of DDV viscoelastic instrument, reach the preceding adding of polycondensation before the ester exchange copolymerisation has all taken place, after polycondensation, add and then be the blend state.Concrete influence is as shown in the table.
Figure 85107888_IMG2
Antistatic additive after composite can be deposited a period of time, also can composite immediately interpolation, can ester exchange polycondensation process adds or spinning before sneak in the terylene chips.It should be noted that, above-mentioned various adding method must guarantee that antistatic additive evenly distributes, be preferably in when polycondensation finishes and add, the percentage by weight that its consumption is pressed polyester resin or polycondensation material or ester exchange material calculates can be in the scope of 2-8%, be no more than 10% at most, otherwise can influence the mechanical-physical index of product.
In the ester exchange process, add in it in proportion as the additive after compound, then through polycondensation, granulation, drying, spinning, coiling, stretching, twisting, typing, winder, weave, arrangement, soap washing, wherein ester exchange, granulation, twisting, typing, winder, weave, put in order technology routinely.The improvement technical characterictic division of other each operation is as follows:
Polycondensation phase I elder generation's normal pressure 1.5~2.5 hours, 190~250 ℃ of temperature; Second stage low vacuum 2.5 hours, 250~280 ℃ of temperature, vacuum 0-760 torr; Phase III high vacuum 2~3 hours, 280 ℃ of temperature, especially the reaction end temperature is no more than 280 ℃ and is beneficial to antistatic additive and plays one's part to the full, and the vacuum residual voltage is less than 0.05 torr.
Dry is 760 torrs in vacuum, in 100~130 ℃ of scopes of temperature, and 24 hours time.
Spinning moulding processing can be carried out on common extruder type spinning machine, and temperature is 275~295 ℃, and winding speed is more than 600~1000 meters/minute.This is because anti-electrostatic polyester resin falls Jie easily than general terylene, so spinning temperature is unsuitable too high or overstand in spinning equipment.
Because the flowing temperature of anti-electrostatic polyester is lower, so draft temperature is unsuitable too high, generally drawing process is, 3.0~4.5 times of draw ratios, temperature of heat plate are 65~80 ℃, with 70 ℃ for well, hot plate temperature is 110~125 ℃, with 110 ℃ for well.
Arranging vertically in fiber in order to ensure antistatic additive, and be the fento distributions, in case the stop polarity group interferes with each other, bring into play maximum antistatic effect, is necessary so will select rational spinning, drawing process.Spinning silk winding speed height helps orientation in principle, but because CA-1 type flowing temperature is lower, so draft temperature is unsuitable too high, to prevent to be rolled state, generally selects draft temperature lower than ordinary polyester long filament draft temperature.
Fiber after the stretching adopts that normal polyester long filament technology is twisted, typing, winder get final product.
The fabric of fiber weaving of the present invention is soaped and is adopted neutral soap powder, and soap lye concentration is 1 grams per liter, and bath raio is 50: 1, and the time is 6 minutes, and temperature is 40 ℃, wash number 5 times, each 3 minutes.
Because the present invention adopts the technology that is added in the composite antistatic agent in the polyster fibre, so can make antistatic additive in the fiber process process, remain even distribution, be that antistatic additive exists with discontinuous phase, and keep even as far as possible and distance weak point, can avoid occurring in the fiber circuit high-order resistance like this, when the electric current in the entire circuit increased, the also corresponding quickening of electric charge loss had suppressed generation of static electricity and accumulation.Therefore, polyester filament and the fabric thereof produced with the present invention not only have durable antistatic behaviour, can be anti-standard wash more than 20 times, and have good antistatic efficient concurrently.Can discharge electric charge fast, be difficult for again electrifying, static friction voltage is all the time less than 200 volts, and the half-life, resistivity was less than 10 less than 60 seconds 10One centimetre of ohm, fracture strength extend 25 ± 7% greater than 2.7 lis of newton/dtexs.Fabric is not stained with ash, do not send out dirt, acidproof, well-pressed, can satisfy the specific (special) requirements of making dust-free clothes, aseptic clothing, anti-blast clothing, also be industry such as precision instrument, integrated circuit, computer make and application process in desirable supporting fibrous material.
Enforcement of the present invention provides by following example.
Example 1 when 5 kilograms of dimethyl terephthalate (DMT)s and 4 kilograms of ethylene glycol and catalyst stabilizer are put into 28 liter stills and carried out ester exchange, adds 6% CA type antistatic additive.The proportioning of CA-1 type and CA-2 type is 5: 3.The ester exchange parameter is 190 ℃ of temperature, 2.5 hours time, 45 rev/mins of stir speed (S.S.)s.The polycondensation parameter is first normal pressure 1.5 hours, 230 ℃ of temperature; Low vacuum is 2.5 hours again, 270 ℃ of temperature, vacuum 0-760 torr; High vacuum is 3 hours again, 280 ℃ of temperature, and the vacuum residual voltage is less than 0.05 torr.To carry out drying after the prepared polyester resin granulation.
Elder generation's preliminary drying is 8 hours when dry, vacuum 760 torrs, and 100 ℃ of temperature, and then dry 16 hours, vacuum 760 torrs, 125 ℃ of temperature.Dried resin slicer is promptly delivered to and is carried out spinning moulding processing on 30 millimeters extruder type spinning machines of diameter, and spinning machine Shang Ge district temperature is respectively 280 ℃, 290 ℃, 290 ℃, 250 ℃, 285 ℃.Coiling speed is 1000 meters/minute, stretches 4 times 75 ℃ of temperature of heat plate, 110 ℃ of hot plate temperatures then on stretching-machine.With obtained drawn yarn routinely technology through twisting, typing, winder, weave, put in order, soap.Adopt neutral soap lye when soaping, concentration is 1 grams per liter, bath raio 50: 1, and 6 minutes time, 40 ℃ of temperature are cleaned each 3 minutes 5 times.
The semi-finished product terylene of this example gained does not have 2.7 lis of newton/dtexs of brute force of oily drafted fibre, and elongation 20% is than resistance 2.41 * 10 9Ohm-cm, 96 volts of friction voltages; The ratio resistance of gained terylene filament fabric is 8.5 * 10 8Ohm-cm, 18 volts of friction voltages, 2 seconds half-life; The ratio resistance of gained terylene filament fabric after 20 standards are soaped is 4.65 * 10 9Ohm-cm, friction voltage is 28 volts, 8 seconds half-life.
Example 2 adds CA type composite antistatic agent when the polycondensation, and other technical process is with example 1, and the brute force that prepared semi-finished product terylene does not have oily drafted fibre is 3.3 lis of newton/dtexs, and elongation 17.4% is than resistance 1.54 * 10 8Ohm-cm, 37 volts of friction voltages.
Example 3, CA type composite antistatic agent addition counts 4% by the percentage by weight of polycondensation vessel material, and all the other are with example 2.The brute force that prepared semi-finished product terylene does not have oily drafted fibre is 3.5 lis of newton/dtexs, and elongation 18.2% is than resistance 5.24 * 10 9Ohm-cm, 124 volts of friction voltages.

Claims (10)

1, the present invention is the manufacture method of a kind of durable anti-static polyester resin and fiber, it comprises the process of the manufacturing and the fibre forming processing of anti-electrostatic polyester resin, it is characterized in that adopting polyoxyethylene or polyether compound and alkylsulfonate or phosphate compounds to carry out the polyester resin of compound antistatic additive compounded technology and the flow process of fiber production.
2, manufacture method as claimed in claim 1 is characterized in that polyoxyethylene or polyether compound and the composite ratio of alkylsulfonate or phosphate compounds are 3: 1 to 5: 4, is preferably 5: 3.
3, manufacture method as claimed in claim 1 is characterized in that composite antistatic additive adds, or adds when polycondensation when ester exchange, also can sneak into the polyester resin section before spinning, is preferably in when polycondensation finishes to add.
4, manufacture method as claimed in claim 1 is characterized in that composite antistatic additive consumption calculates between the 1-8% by the percentage by weight of polyester resin or polycondensation material or ester exchange material, is no more than 10% at most.
5, manufacture method as claimed in claim 1 is characterized in that having the polyester resin of composite antistatic agent and the flow process of long filament production is polycondensation, drying, spinning silk winding, stretches and soap.
6, manufacture method as claimed in claim 5, the phase I is normal pressure 1.5-2 hour when it is characterized in that polycondensation, temperature is 190-250 ℃, second stage vacuumized 2-3.5 hour, vacuum 0-760 torr, temperature 250-280 ℃, 2-3 hour pumping high vacuum time phase III, residual voltage is less than 0.05 torr, 280 ℃ of temperature.
7, manufacture method as claimed in claim 5 is characterized in that baking temperature is 100-130 ℃, and the time is 20-24 hour, and vacuum is 750 torrs.
8, manufacture method as claimed in claim 5 is characterized in that spinning temperature is 275-295 ℃, winding speed be 600-1000 rice/minute.
9, manufacture method as claimed in claim 5 is characterized in that draw ratio is 3.5-4.5 times, and temperature of heat plate is 65-80 ℃.
10, manufacture method as claimed in claim 5 is characterized in that fabric adopts neutrality to soap.
CN 85107888 1985-10-15 1985-10-15 The manufacture method of durable anti-static polyester resin and fiber Pending CN85107888A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107630266A (en) * 2017-10-08 2018-01-26 安徽三宝棉纺针织投资有限公司 A kind of antistatic treatment technique of resin base polyester fiber
CN108179500A (en) * 2017-12-27 2018-06-19 安徽东锦资源再生科技有限公司 HMLS Polyester fibre spinning and twisting technique
CN108299732A (en) * 2018-01-25 2018-07-20 界首市鑫宇塑业有限公司 Waste and old power battery case modification regeneration technique
CN108365288A (en) * 2018-01-25 2018-08-03 界首市天隆塑业科技有限公司 Waste battery shell is modified enhancing regeneration technology

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107630266A (en) * 2017-10-08 2018-01-26 安徽三宝棉纺针织投资有限公司 A kind of antistatic treatment technique of resin base polyester fiber
CN107630266B (en) * 2017-10-08 2020-05-26 安徽三宝棉纺针织投资有限公司 Antistatic treatment process for resin-based polyester fiber
CN108179500A (en) * 2017-12-27 2018-06-19 安徽东锦资源再生科技有限公司 HMLS Polyester fibre spinning and twisting technique
CN108299732A (en) * 2018-01-25 2018-07-20 界首市鑫宇塑业有限公司 Waste and old power battery case modification regeneration technique
CN108365288A (en) * 2018-01-25 2018-08-03 界首市天隆塑业科技有限公司 Waste battery shell is modified enhancing regeneration technology

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