CN111270337A - Mosquito-repellent polyester fiber and preparation method thereof - Google Patents

Mosquito-repellent polyester fiber and preparation method thereof Download PDF

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Publication number
CN111270337A
CN111270337A CN202010285246.3A CN202010285246A CN111270337A CN 111270337 A CN111270337 A CN 111270337A CN 202010285246 A CN202010285246 A CN 202010285246A CN 111270337 A CN111270337 A CN 111270337A
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CN
China
Prior art keywords
mosquito
repellent
fiber
polyester fiber
forming polymer
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Pending
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CN202010285246.3A
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Chinese (zh)
Inventor
王小华
汪春波
王炳奎
陆清峰
袁慧丽
邓成浩
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Zhejiang Zhink Chemical Fiber Co ltd
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Zhejiang Zhink Chemical Fiber Co ltd
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Priority to CN202010285246.3A priority Critical patent/CN111270337A/en
Publication of CN111270337A publication Critical patent/CN111270337A/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
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/92Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
    • 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
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Polyesters Or Polycarbonates (AREA)

Abstract

The mosquito-repellent polyester fiber is characterized by comprising the following components in parts by weight: 0.05-0.2% of graphene oxide, 98.8-99.45% of fiber forming polymer and 0.5-1.0% of mosquito repellent. The invention also discloses a preparation method of the mosquito-repellent polyester fiber. Graphene oxide reduces the melting point of polyester to reduce the processing temperature, reduce the diffusion of mosquito repellent active ingredient, promote mosquito repellent polyester fiber's mosquito repellent effect from a plurality of aspects on the one hand to the good adsorption of grease.

Description

Mosquito-repellent polyester fiber and preparation method thereof
Technical Field
The invention relates to a polyester fiber and a preparation method thereof, belonging to the technical field of chemical fibers.
Background
Female mosquitoes sucking blood by the mosquito repellent are intermediate hosts of other pathogens such as dengue fever, malaria, yellow fever, filariasis, Japanese encephalitis and the like, in recent years, the damage to people caused by viruses such as dengue fever, Seka and the like transmitted by mosquitoes is more and more serious, and the mosquito repellent fabric is produced at the same time.
The terylene has excellent performance, high quality and low price, is applied to various fields, and can be widely applied to military clothes, fashion clothes, sportswear, outdoor clothes and some clothes brands if the terylene has a long-acting and safe mosquito repellent function, thereby bringing excellent healthy and comfortable experience to consumers.
The mosquito-proof fabric is divided into two technologies of yarn mosquito-proof and after-finishing mosquito-proof. The post-finishing method is common, but the fabric is not resistant to water washing, cannot realize long-acting mosquito repelling, and also can influence the hand feeling of the fabric. The preparation technology of the mosquito-repellent yarn is not mature, particularly, the mosquito-repellent terylene mostly adopts a single blending mode, and the effective mosquito-repellent ingredients are easy to escape at high temperature, so that the final mosquito-repellent effect is influenced. The patent document of the blending mode can refer to the disclosure of Chinese invention patent application with application number 201510268620.8, a PET composite material with mosquito repellent effect (application publication number CN 104817833A); reference may also be made to the disclosure of Chinese patent application with application number 201810860923.2, the disclosure of which is "preparation of functional polyester fiber and its use method" (application publication number CN 109056100A). The patent document of the after-finishing mode can refer to the Chinese invention patent application with the application number of 201310098263.6, which discloses a manufacturing method of a fabric for antifouling mosquito-repellent terylene and chinlon interwoven mesh shoes (the application publication number is CN 103147299A).
Therefore, a new technology for producing the mosquito-repellent polyester fiber needs to be developed to fill the blank in the field of mosquito-repellent polyester and fully embody the people-oriented development strategy of textiles.
Disclosure of Invention
The first technical problem to be solved by the invention is to provide the mosquito-repellent polyester fiber which is combined with the graphene oxide to improve the mosquito-repellent effect aiming at the technical current situation.
The second technical problem to be solved by the invention is to provide a preparation method of the mosquito-repellent polyester fiber for improving the mosquito-repellent effect by combining graphene oxide, aiming at the technical current situation.
The technical scheme adopted by the invention for solving the first technical problem is as follows: the mosquito-repellent polyester fiber is characterized by comprising the following components in parts by weight:
0.05 to 0.2 percent of graphene oxide,
98.8 to 99.45 percent of fiber-forming polymer,
0.5-1.0% of mosquito repellent.
Preferably, the mosquito repellent is at least one of permethrin, tetramethrin, transfluthrin and benzyl benzoate.
Preferably, the mosquito repellent is added in the form of master batch.
Preferably, the fiber-forming polymer is obtained by copolymerizing at least two of terephthalic acid, isophthalic acid and adipic acid, 2- (2-hydroxyethyl) piperidine-1-carboxylic acid sec-butyl ester and ethylene glycol in the presence of a catalyst after mixing.
The technical scheme adopted by the invention for solving the second technical problem is as follows: the preparation method of the mosquito-repellent polyester fiber is characterized by comprising the following steps:
① preparation of fiber-forming polymers
Mixing the components of graphene oxide and a fiber-forming polymer at 50-70 ℃ for 120-180 min to prepare slurry, wherein the molar ratio of carboxyl to hydroxyl is 1.05: 1-1.10: 1, and the dosage of a catalyst is 200-300 ppm; reacting the slurry at 260-265 ℃ for 280-320 min, and removing water generated by polycondensation reaction by using high-purity nitrogen in a bubbling manner to obtain a polycondensate; reacting the prepolymer at 270-275 ℃ for 90-110 min, wherein the pressure is 1-2 kpa absolute; reacting for 180-200 min at 280-285 ℃ under the absolute pressure of 80-120 pa to obtain a fiber-forming polymer containing graphene oxide, wherein the content of sec-butyl 2- (2-hydroxyethyl) piperidine-1-carboxylate is 0.01-0.05%, and granulating, crystallizing and drying to obtain fiber-forming polymer particles;
② preparation method of mosquito-repellent polyester fiber
Preparing the mosquito repellent into mosquito repellent master batches, then respectively metering the fiber-forming polymer particles and the mosquito repellent master batches, inputting the mixture into a mixer for mixing, and uniformly mixing the mixture and then entering a screw; the temperature of the screw is set to be 150-200 ℃, the pressure of the assembly is controlled to be 12-20 Mpa, the temperature of the box body is set to be 150-200 ℃, and the mosquito-repellent polyester fiber is obtained after circular blowing or side blowing, oiling and winding.
Compared with the prior art, the invention has the advantages that: the invention solves the problem of uniform dispersion of graphene oxide by an in-situ polymerization technology, and enables the mosquito repellent to become a part of a polyester macromolecular chain by a copolymerization technology, thereby realizing long-acting mosquito repelling. Graphene oxide reduces the melting point of polyester to reduce the processing temperature, reduce the diffusion of mosquito repellent active ingredient, promote mosquito repellent polyester fiber's mosquito repellent effect from a plurality of aspects on the one hand to the good adsorption of grease. The invention has mature manufacturing process, no special requirement on equipment, easy industrial implementation and convenient popularization. The mosquito-repellent polyester fiber prepared by the invention has the advantages of outstanding and lasting functions, smooth hand feeling, safety and reliability.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1:
preparation of (I) fiber-forming polymers
1) Raw materials of 0.1% of graphene oxide, 0.05% of 2- (2-hydroxyethyl) piperidine-1-carboxylic acid sec-butyl ester, terephthalic acid: isophthalic acid ═ 8: 2, the using amount of the ethylene glycol is 1.08: 1, controlling, mixing for 180min at 70 ℃ to prepare slurry, wherein the using amount of the catalyst is 300 ppm;
2) reacting the slurry 1) at 265 ℃ for 320min, and removing water generated by polycondensation reaction by using high-purity nitrogen in a bubbling manner;
3) reacting the prepolymer 2) at 275 ℃ for 110min under the absolute pressure of 1 kpa; then reacting for 180min at 280 ℃ under the absolute pressure of 80pa to obtain a fiber-forming polymer, wherein the content of graphene oxide is 0.1%, and the content of 2- (2-hydroxyethyl) piperidine-1-carboxylic acid sec-butyl ester is 0.05%. Granulating, crystallizing and drying to obtain fiber-forming polymer particles.
(II) preparation of mosquito-repellent polyester fiber
4) Preparing mosquito repellent into mosquito repellent master batches, metering fiber-forming polymer particles and the mosquito repellent master batches respectively through a weight loss type metering device, inputting the fiber-forming polymer particles and the mosquito repellent master batches into a special dynamic mixer for mixing, and uniformly mixing the fiber-forming polymer particles and the mosquito repellent master batches, wherein the addition amount of the master batches is 3%;
5) the temperature of the screw is set at 150/155/160/165/168 ℃, the pressure of the assembly is controlled at 12Mpa, the temperature of the box body is set at 170 ℃, and after circular blowing or side blowing, oiling and winding are carried out to obtain the mosquito-repellent polyester fiber.
The mosquito repelling rate of the mosquito repelling polyester fiber reaches 70.4 percent (the detection standard GB/T30126-2013).
Example 2:
preparation of (I) fiber-forming polymers
1) Raw materials of 0.15% of graphene oxide, 0.06% of 2- (2-hydroxyethyl) piperidine-1-carboxylic acid sec-butyl ester, terephthalic acid: isophthalic acid ═ 8: 2, the using amount of the ethylene glycol is 1.08: 1, controlling, mixing for 180min at 70 ℃ to prepare slurry, wherein the using amount of the catalyst is 300 ppm;
2) reacting the slurry 1) at 265 ℃ for 320min, and removing water generated by polycondensation reaction by using high-purity nitrogen in a bubbling manner;
3) reacting the prepolymer 2) at 275 ℃ for 110min under the absolute pressure of 1 kpa; and then reacting for 180min at 280 ℃ under the absolute pressure of 80pa to obtain a fiber-forming polymer, wherein the content of graphene oxide is 0.15%, and the content of 2- (2-hydroxyethyl) piperidine-1-carboxylic acid sec-butyl ester is 0.06%. Granulating, crystallizing and drying for later use.
(II) preparation of mosquito-repellent polyester fiber
4) Preparing mosquito repellent into mosquito repellent master batches, metering fiber-forming polymer particles and the mosquito repellent master batches respectively through a weight loss type metering device, inputting the fiber-forming polymer particles and the mosquito repellent master batches into a special dynamic mixer for mixing, and uniformly mixing the fiber-forming polymer particles and the mosquito repellent master batches, wherein the addition amount of the master batches is 3.5%;
5) the temperature of the screw is set at 150/155/160/165/168 ℃, the pressure of the assembly is controlled at 12Mpa, the temperature of the box body is set at 170 ℃, and after circular blowing or side blowing, oiling and winding are carried out to obtain the mosquito-repellent polyester fiber.
The mosquito repelling rate of the mosquito repelling polyester fiber reaches 74.6 percent (the detection standard GB/T30126-2013).
Example 3:
preparation of (I) fiber-forming polymers
1) Raw materials of 0.15% of graphene oxide, 0.06% of 2- (2-hydroxyethyl) piperidine-1-carboxylic acid sec-butyl ester, terephthalic acid: isophthalic acid ═ 8: 2, the using amount of the ethylene glycol is 1.08: 1, controlling, mixing for 180min at 70 ℃ to prepare slurry, wherein the using amount of the catalyst is 300 ppm;
2) reacting the slurry 1) at 265 ℃ for 320min, and removing water generated by polycondensation reaction by using high-purity nitrogen in a bubbling manner;
3) reacting the prepolymer 2) at 275 ℃ for 110min under the absolute pressure of 1 kpa; and then reacting for 180min at 280 ℃ under the absolute pressure of 80pa to obtain a fiber-forming polymer, wherein the content of graphene oxide is 0.15%, and the content of 2- (2-hydroxyethyl) piperidine-1-carboxylic acid sec-butyl ester is 0.06%. Granulating, crystallizing and drying for later use.
(II) preparation of mosquito-repellent polyester fiber
4) Preparing mosquito repellent into mosquito repellent master batches, metering fiber-forming polymer particles and the mosquito repellent master batches respectively through a weight-loss metering device, inputting the fiber-forming polymer particles and the mosquito repellent master batches into a special dynamic mixer for mixing, and uniformly mixing the fiber-forming polymer particles and the mosquito repellent master batches, wherein the addition amount of the master batches is 4%;
5) the temperature of the screw is set at 150/155/160/165/168 ℃, the pressure of the assembly is controlled at 12Mpa, the temperature of the box body is set at 170 ℃, and after circular blowing or side blowing, oiling and winding are carried out to obtain the mosquito-repellent polyester fiber.
The mosquito repelling rate of the mosquito repelling polyester fiber reaches 79.6 percent (the detection standard GB/T30126-2013).

Claims (5)

1. The mosquito-repellent polyester fiber is characterized by comprising the following components in parts by weight:
0.05 to 0.2 percent of graphene oxide,
98.8 to 99.45 percent of fiber-forming polymer,
0.5-1.0% of mosquito repellent.
2. The mosquito-repellent polyester fiber according to claim 1, wherein the mosquito repellent is at least one of permethrin, tetramethrin, transfluthrin and benzyl benzoate.
3. The mosquito-repellent polyester fiber according to claim 1, wherein the mosquito repellent is added in the form of master batch.
4. The mosquito-repellent polyester fiber according to claim 1, wherein the fiber-forming polymer is obtained by copolymerizing at least two of terephthalic acid, isophthalic acid and adipic acid, 2- (2-hydroxyethyl) piperidine-1-carboxylic acid sec-butyl ester and ethylene glycol in the presence of a catalyst after mixing.
5. A preparation method of the mosquito-repellent polyester fiber according to any one of claims 1 to 4, which is characterized by comprising the following steps:
① preparation of fiber-forming polymers
Mixing the components of graphene oxide and a fiber-forming polymer at 50-70 ℃ for 120-180 min to prepare slurry, wherein the molar ratio of carboxyl to hydroxyl is 1.05: 1-1.10: 1, and the dosage of a catalyst is 200-300 ppm; reacting the slurry at 260-265 ℃ for 280-320 min, and removing water generated by polycondensation reaction by using high-purity nitrogen in a bubbling manner to obtain a polycondensate; reacting the prepolymer at 270-275 ℃ for 90-110 min, wherein the pressure is 1-2 kpa absolute; reacting for 180-200 min at 280-285 ℃ under the absolute pressure of 80-120 pa to obtain a fiber-forming polymer containing graphene oxide, wherein the content of sec-butyl 2- (2-hydroxyethyl) piperidine-1-carboxylate is 0.01-0.05%, and granulating, crystallizing and drying to obtain fiber-forming polymer particles;
② preparation method of mosquito-repellent polyester fiber
Preparing the mosquito repellent into mosquito repellent master batches, then respectively metering the fiber-forming polymer particles and the mosquito repellent master batches, inputting the mixture into a mixer for mixing, and uniformly mixing the mixture and then entering a screw; the temperature of the screw is set to be 150-200 ℃, the pressure of the assembly is controlled to be 12-20 Mpa, the temperature of the box body is set to be 150-200 ℃, and the mosquito-repellent polyester fiber is obtained after circular blowing or side blowing, oiling and winding.
CN202010285246.3A 2020-04-13 2020-04-13 Mosquito-repellent polyester fiber and preparation method thereof Pending CN111270337A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101698658A (en) * 2009-10-16 2010-04-28 厦门森美达生物技术有限公司 Method for preparing wormer sec-Butyl 2-(2-hydroxyethyl)piperidine-1-carboxylate
CN102828273A (en) * 2012-07-25 2012-12-19 敬首雄 Polyester insecticidal fabric production process
CN105017511A (en) * 2015-08-20 2015-11-04 浙江万凯新材料有限公司 Preparation method of oxidized graphene modified PET (polyethylene terephthalate) material
CN106245148A (en) * 2016-08-20 2016-12-21 福建经纬新纤科技实业有限公司 A kind of original liquid coloring anophelifuge polyester fiber
CN110344134A (en) * 2019-07-16 2019-10-18 福建百宏聚纤科技实业有限公司 A kind of modified polyester fibre and its production method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101698658A (en) * 2009-10-16 2010-04-28 厦门森美达生物技术有限公司 Method for preparing wormer sec-Butyl 2-(2-hydroxyethyl)piperidine-1-carboxylate
CN102828273A (en) * 2012-07-25 2012-12-19 敬首雄 Polyester insecticidal fabric production process
CN105017511A (en) * 2015-08-20 2015-11-04 浙江万凯新材料有限公司 Preparation method of oxidized graphene modified PET (polyethylene terephthalate) material
CN106245148A (en) * 2016-08-20 2016-12-21 福建经纬新纤科技实业有限公司 A kind of original liquid coloring anophelifuge polyester fiber
CN110344134A (en) * 2019-07-16 2019-10-18 福建百宏聚纤科技实业有限公司 A kind of modified polyester fibre and its production method

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Application publication date: 20200612