CN112342645A - Method for producing high-strength high-modulus polyethylene fiber by using tetrachloroethylene as second solvent through gel method - Google Patents

Method for producing high-strength high-modulus polyethylene fiber by using tetrachloroethylene as second solvent through gel method Download PDF

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Publication number
CN112342645A
CN112342645A CN201910719744.1A CN201910719744A CN112342645A CN 112342645 A CN112342645 A CN 112342645A CN 201910719744 A CN201910719744 A CN 201910719744A CN 112342645 A CN112342645 A CN 112342645A
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China
Prior art keywords
tetrachloroethylene
solvent
water
tank
modulus polyethylene
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CN201910719744.1A
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Chinese (zh)
Inventor
朱建军
周新基
李文建
李珣珣
朱德钧
陈俊明
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Kyushu Star Technology Co ltd
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Jiangsu Jiujiujiu Technology Co ltd
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Priority to CN201910719744.1A priority Critical patent/CN112342645A/en
Publication of CN112342645A publication Critical patent/CN112342645A/en
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F11/00Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/04Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers
    • D01F11/06Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds

Abstract

The invention discloses a method for producing high-strength high-modulus polyethylene fibers by a gel method with tetrachloroethylene as a second solvent, which comprises the steps of enabling fluid strands to enter a water bath, cooling the fluid strands by water to form gel strands, and extracting the gel strands in an extraction tank, wherein white oil is used as a first solvent, and a tetrachloroethylene raw material storage tank for storing tetrachloroethylene is arranged; tetrachloroethylene is used as a second solvent; a system stabilizer is added into the water bath tank, the extraction tank and the tetrachloroethylene raw material storage tank; the system stabilizer is one or a combination of more of ammonia, phenols, amines, alcohols and nitriles; a water bath tank assembly is provided with a water treatment facility. The invention can effectively remove the floccules and has good product quality.

Description

Method for producing high-strength high-modulus polyethylene fiber by using tetrachloroethylene as second solvent through gel method
Technical Field
The invention relates to a method for producing high-strength high-modulus polyethylene fibers by a gel method.
Background
The high-strength high-modulus polyethylene fiber is a new material developed in the last 50 th century and has excellent mechanical properties. Has obvious advantages in the aspects of sports clothing, navigation, maritime work, labor protection, military industry and the like. The gel spinning adopts white oil as a first solvent to swell and unwind polyethylene particles with high molecular weight (the molecular weight is more than 50 ten thousand), so that the polyethylene particles can be entangled with each other after extrusion, and the polyethylene particles are in a linear chain state through high-power stretching to form a high-performance product. Before stretching, the molecular chains need to be relatively fixed, namely white oil in the gel silk is removed as much as possible, and extrusion, extraction and other methods can be used for removing the white oil. The extraction method is adopted when the high-strength and high-modulus polyethylene fiber is produced by the traditional gel spinning method, and the extraction solvent, namely the second solvent, can adopt hydrocarbon solvent, toluene, gasoline and the like. The hydrocarbon solvent (a mixture of normal alkane and naphthenic alkane of C6-C8) has a flash point of less than 40 ℃, is very dangerous in the use process, is easy to generate fire risks, and similarly has the fire risks of toluene, gasoline and the like. More than one enterprise has a fire problem in the production process, and the loss is very large. In order to solve the problem, the inventor replaces the extracting agent with tetrachloroethylene, and after years of practice, the fire risk is solved. However, after the solvent is replaced, the tetrachloroethylene solvent is not stable enough under high temperature conditions, and is easily decomposed into acidic substances at high temperatures, and the acidic substances cause corrosion of equipment, and the corrosion occurs not only in a portion of the equipment in contact with a liquid but also in a portion of the equipment not in direct contact with the liquid. The iron rust on the corroded equipment can pollute the PE wires, and meanwhile, the corroded equipment surface becomes rough, so that the problems of broken wires and the like are caused in production. In order to solve this problem, the present inventors stabilized an aqueous solution system by adding a substance containing a specific group. Such as amines or ammonia, may be effective. Generally, ammonia water is selected, and the first is cheap and easy to obtain; secondly, the buffer has certain buffer capacity; thirdly, the irritation is weaker than that of the organic amines. After the system is stabilized, a small amount of system stabilizer is remained in the white oil, and the small amount of system stabilizer is subjected to high-temperature treatment in the process of producing the gel silk and reacts with the white oil to generate a new substance, the new substance is flocculent in water after being aggregated, and the flocculent is further aggregated in a cooling water system and then adhered to the gel silk. This process results in foreign matter on the gel wire that is also difficult to separate thoroughly from the gel wire. Floccules are adhered to the gel yarns, and in the stretching process, a section of the floccules is mixed with the finished product yarns, so that the problems of color difference, foreign matters and the like are caused.
Disclosure of Invention
The invention aims to provide a method for producing high-strength high-modulus polyethylene fibers by a jelly glue method with tetrachloroethylene as a second solvent, wherein the produced product has good quality.
The technical solution of the invention is as follows:
a method for producing high-strength high-modulus polyethylene fibers by a gel method with tetrachloroethylene as a second solvent comprises the steps of enabling fluid strands to enter a water bath, cooling the fluid strands into gel strands through water, extracting the gel strands in an extraction tank, and adopting white oil as a first solvent, and is characterized in that: a tetrachloroethylene raw material storage tank for storing tetrachloroethylene is arranged; tetrachloroethylene is used as a second solvent; a system stabilizer is added into the water bath tank, the extraction tank and the tetrachloroethylene raw material storage tank; the system stabilizer is one or a combination of more of ammonia, phenols, amines, alcohols and nitriles; a water bath tank assembly is provided with a water treatment facility.
The water treatment equipment is one or a combination of a plurality of air floatation devices, flocculation devices and electrolysis devices.
The water treatment equipment is an air floatation device; the water in the cooling tank flows through the air floatation device, the treated water flows to the heat exchange unit, and the treated water returns to the cooling water tank after being stabilized at a constant temperature.
And returning the water with constant temperature and stability to the cooling water tank.
The system stabilizer is ammonia water.
The liquid level of the extracting agent tetrachloroethylene in the extraction tank is covered with a layer of water.
And drying after extraction, wherein the drying operation is carried out in a drying box, and the fiber inlet and outlet of the drying box are maintained at negative pressure.
The amine is one or more of monomethylamine, dimethylamine, trimethylamine, monoethylamine, diethylamine, triethylamine, monopropylamine, dipropylamine and tripropylamine.
The invention can effectively remove the floccules and has good product quality.
The present invention will be further described with reference to the following examples.
Detailed Description
A method for producing high-strength high-modulus polyethylene fiber by using a gel method with tetrachloroethylene as a second solvent comprises the steps of enabling fluid strands to enter a water bath, cooling the fluid strands by water to form gel strands, and extracting the gel strands in an extraction tank, wherein white oil is used as a first solvent, and a tetrachloroethylene raw material storage tank for storing tetrachloroethylene is arranged; tetrachloroethylene is used as a second solvent; a system stabilizer is added into the water bath tank, the extraction tank and the tetrachloroethylene raw material storage tank; the system stabilizer is one or a combination of more of ammonia, phenols, amines, alcohols and nitriles; a water bath tank assembly is provided with a water treatment facility.
The water treatment equipment is one or a combination of a plurality of air floatation devices, flocculation devices and electrolysis devices.
The water treatment equipment is an air floatation device; the water in the cooling tank flows through the air floatation device, the treated water flows to the heat exchange unit, and the treated water returns to the cooling water tank after being stabilized at a constant temperature.
And returning the water with constant temperature and stability to the cooling water tank.
The system stabilizer is ammonia water.
The liquid level of the extracting agent tetrachloroethylene in the extraction tank is covered with a layer of water.
And drying after extraction, wherein the drying operation is carried out in a drying box, and the fiber inlet and outlet of the drying box are maintained at negative pressure.
The amine is one or more of monomethylamine, dimethylamine, trimethylamine, monoethylamine, diethylamine, triethylamine, monopropylamine, dipropylamine and tripropylamine.
The following may be the case in the specific process:
(1) ammonia water is not added in the production process, the equipment is rusted after 3 months, and the surface of the godet roller is rough.
(2) And 5% ammonia water is added in the production process, the pH = 5.5-10.5 of the system is maintained, the equipment is not rusted all the time, and the surface of the godet roller is smooth and clean as new. A small amount of yellow floccule appears in the water tank within one week, and the condition is gradually aggravated.
(3) 2% ammonia water is added in the production process, the pH = 5.5-10.5 of the system is maintained, the equipment is not rusted all the time, and the surface of the godet roller is smooth and clean as new. A small amount of yellow floccule appears in the water tank within one week, and the condition is gradually aggravated.
(4) 2% ammonia water is added in the production process, the pH = 5.5-10.5 of the system is maintained, the equipment is not rusted all the time, and the surface of the godet roller is smooth and clean as new. A small amount of yellow floccule appears in the water tank within one week, and the condition is gradually aggravated. An air floatation decontamination device is added in the water circulation system, so that yellow floccules are removed completely within 3 days and do not occur again.
(5) During the production process, 40% of dimethylamine is added, the pH = 5.5-10.5 of the system is maintained, the equipment is not rusted all the time, and the surface of the godet roller is smooth and clean as new. The surrounding environment is gradually harsher and has a fishy amine smell.
(6) And disodium hydrogen phosphate and sodium hydrogen phosphate mixed buffer solution is added in the production process, the pH = 5.5-10.5 of the system is maintained, the equipment is not rusted all the time, and the surface of the godet roller is smooth and clean as new. The surrounding environment has no problem, and the phosphorus content in a small amount of discharged production sewage is more than 150 mg/kg.
(7) Taking (3) water containing the floccules, carrying out electrolysis treatment, selecting the current density of 350mA/cm2, and electrolyzing for 30 minutes to disperse and reduce the floccules.
(8) And (3) flocculating the water containing the floccules with PAC and PAM, wherein the floccules are completely agglomerated and precipitate to the bottom, and the water is clear and transparent.
(9) The gel silk passes through an extraction tank, tetrachloroethylene is used for extracting white oil, and water seal is not added in the extraction tank. The extraction rate of the white oil is 99 percent, and the consumption of tetrachloroethylene is as high as 30-50 kg per hour. The surrounding environment has a strong odor of tetrachloroethylene. The equipment is corroded to different degrees at the contact positions of tetrachloroethylene liquid and gas.
(10) The gel silk passes through an extraction tank, white oil is extracted by tetrachloroethylene, 10cm of water seal is added into the extraction tank, and a stabilizing agent is added into water. The extraction rate of the white oil is 99%, and the consumption of tetrachloroethylene is 5-10 kg per hour. The surrounding environment had little tetrachloroethylene odor. The equipment in contact with the liquid is not corroded. The apparatus was slightly corroded in the portion in contact with the gas phase.
(11) And (4) drawing the white oil-extracted silk obtained in the step (10) into a hot box to dry tetrachloroethylene and moisture on the surface of the silk. The hot box does not adopt negative pressure treatment, and the odor of tetrachloroethylene in the surrounding environment is obvious. Slight corrosion occurred inside the equipment and at the air outlet.
(12) And (4) drawing the white oil-extracted silk obtained in the step (10) into a hot box to dry tetrachloroethylene and moisture on the surface of the silk. The hot box adopts negative pressure treatment, and the odor of tetrachloroethylene in the surrounding environment disappears. The inside of the apparatus was slightly corroded.

Claims (8)

1. A method for producing high-strength high-modulus polyethylene fibers by a gel method with tetrachloroethylene as a second solvent comprises the steps of enabling fluid strands to enter a water bath, cooling the fluid strands into gel strands through water, extracting the gel strands in an extraction tank, and adopting white oil as a first solvent, and is characterized in that: a tetrachloroethylene raw material storage tank for storing tetrachloroethylene is arranged; tetrachloroethylene is used as a second solvent; a system stabilizer is added into the water bath tank, the extraction tank and the tetrachloroethylene raw material storage tank; the system stabilizer is one or a combination of more of ammonia, phenols, amines, alcohols and nitriles; a water bath tank assembly is provided with a water treatment facility.
2. The process of claim 1 for producing high strength and high modulus polyethylene fibers by the jelly glue method using tetrachloroethylene as a second solvent, which comprises: the water treatment equipment is one or a combination of a plurality of air floatation devices, flocculation devices and electrolysis devices.
3. The process of claim 2 for producing high strength and high modulus polyethylene fibers by the jelly glue method using tetrachloroethylene as a second solvent, which comprises: the water treatment equipment is an air floatation device; the water in the cooling tank flows through the air floatation device, the treated water flows to the heat exchange unit, and the treated water returns to the cooling water tank after being stabilized at a constant temperature.
4. The process of claim 3 for producing high strength and high modulus polyethylene fiber by the gel process using tetrachloroethylene as the second solvent, which comprises: and returning the water with constant temperature and stability to the cooling water tank.
5. The process of claim 1, 2 or 3 for producing high strength and high modulus polyethylene fibers by the jelly glue method using tetrachloroethylene as a second solvent, which comprises: the system stabilizer is ammonia water.
6. The process of claim 1, 2 or 3 for producing high strength and high modulus polyethylene fibers by the jelly glue method using tetrachloroethylene as a second solvent, which comprises: the liquid level of the extracting agent tetrachloroethylene in the extraction tank is covered with a layer of water.
7. A process according to claim 1, 2 or 3 for the production of high strength and high modulus polyethylene fibres by the jelly glue process using tetrachloroethylene as a second solvent, characterised in that: and drying after extraction, wherein the drying operation is carried out in a drying box, and the fiber inlet and outlet of the drying box are maintained at negative pressure.
8. A process according to claim 1, 2 or 3 for the production of high strength and high modulus polyethylene fibres by the jelly glue process using tetrachloroethylene as a second solvent, characterised in that: the amine is one or more of monomethylamine, dimethylamine, trimethylamine, monoethylamine, diethylamine, triethylamine, monopropylamine, dipropylamine and tripropylamine.
CN201910719744.1A 2019-08-06 2019-08-06 Method for producing high-strength high-modulus polyethylene fiber by using tetrachloroethylene as second solvent through gel method Pending CN112342645A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101962819A (en) * 2010-09-13 2011-02-02 杭州翔盛高强纤维材料股份有限公司 Ultrawhite ultrahigh-molecular weight ultrahigh-modulus polyethylene fibers and preparation process thereof
CN103866425A (en) * 2014-03-06 2014-06-18 江苏九九久科技股份有限公司 Solvent used by jelly spinning method in preparation of ultra-high-molecular-weight polyethylene fiber
CN103882561A (en) * 2014-03-06 2014-06-25 江苏九九久科技股份有限公司 Microwave-assisted extraction and drying process for high-strength high-modulus polyethylene gel fiber
CN203834073U (en) * 2014-02-18 2014-09-17 江苏神泰科技发展有限公司 Water seal type tetrachloroethylene extraction plant
CN106757405A (en) * 2017-01-11 2017-05-31 江苏必康制药股份有限公司 The preparation method of high-strength high-modulus polyethylene fiber
CN106978654A (en) * 2017-04-01 2017-07-25 浙江千禧龙纤特种纤维股份有限公司 The solidification method for shaping of gel fiber in superhigh molecular weight polyethylene fibers production process

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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CN203834073U (en) * 2014-02-18 2014-09-17 江苏神泰科技发展有限公司 Water seal type tetrachloroethylene extraction plant
CN103866425A (en) * 2014-03-06 2014-06-18 江苏九九久科技股份有限公司 Solvent used by jelly spinning method in preparation of ultra-high-molecular-weight polyethylene fiber
CN103882561A (en) * 2014-03-06 2014-06-25 江苏九九久科技股份有限公司 Microwave-assisted extraction and drying process for high-strength high-modulus polyethylene gel fiber
CN106757405A (en) * 2017-01-11 2017-05-31 江苏必康制药股份有限公司 The preparation method of high-strength high-modulus polyethylene fiber
CN106978654A (en) * 2017-04-01 2017-07-25 浙江千禧龙纤特种纤维股份有限公司 The solidification method for shaping of gel fiber in superhigh molecular weight polyethylene fibers production process

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