CN112647146B - Preparation method and application of waterproof polyester fiber - Google Patents
Preparation method and application of waterproof polyester fiber Download PDFInfo
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- CN112647146B CN112647146B CN202011500918.4A CN202011500918A CN112647146B CN 112647146 B CN112647146 B CN 112647146B CN 202011500918 A CN202011500918 A CN 202011500918A CN 112647146 B CN112647146 B CN 112647146B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent 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
- D01F6/92—Monocomponent 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
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/04—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers
- D01F11/08—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/02—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with hydrocarbons
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
- D06M13/282—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing phosphorus
- D06M13/292—Mono-, di- or triesters of phosphoric or phosphorous acids; Salts thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/53—Polyethers
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a preparation method and application of waterproof polyester fiber, which comprises the following steps: mixing the dried waterproof polyester master batch with PET granules, and then carrying out melt spinning and post false twisting to prepare the waterproof polyester master batch, wherein the preparation method of the waterproof polyester master batch comprises the following steps: a. fully and uniformly mixing partially fluorinated piperazine amide, titanium dioxide and polyamide wax to obtain first mixed powder; b. b, adding polyester mixed powder, pentaerythritol and a composite stabilizer into the first mixed powder obtained in the step a, and uniformly mixing to obtain second mixed powder; c. and c, melting and blending the second mixed powder obtained in the step b by using a vacuum double-screw extruder, and then granulating to obtain the waterproof polyester master batch. The woven fabric sample prepared from the waterproof polyester fiber has excellent waterproof performance and good durability after being fully deoiled and heat-set.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a preparation method and application of waterproof polyester fibers.
Background
With the development of synthetic fibers and textile products toward high performance and multifunction, waterproof fibers and fabrics have been widely developed in the fields of sutures, outdoor sportswear, decoration, automobile protection, etc. in recent years. Scientific research shows that the fiber or fabric has to have two elements to achieve good waterproof effect: firstly the fibre or fabric surface itself must be water repellent and secondly the fibre surface must have a rough microstructure.
In the prior art, the method for endowing the fibers or the fabrics with the waterproof performance is to carry out after-treatment on the fabrics so that the waterproof agent is adsorbed on the surfaces of the fibers and is combined with the fibers through polar groups, so that the surface tension of the fibers is reduced, and the fabrics are endowed with good water repellency, oil repellency and antifouling performance. With the development of science and technology in recent years, people begin to research the preparation of waterproof fibers by adopting a copolymerization modification or blending modification mode. Common waterproof agents include polyvinyl chloride, fluorinated polyurethane, fluorinated polyimide, fluorinated ethylene, siloxane, polyfluoro quaternary ammonium silane coupling agents and the like. CN102115543A discloses a technical scheme that polyester is respectively placed in two solvents for dissolution-precipitation treatment to prepare the polyester with strong hydrophobicity. CN1034693563B discloses a preparation method of a sheath-core composite fiber which takes fluorine-containing polyethylene terephthalate as a sheath layer and PET as a core layer material. CN104451938A discloses a technical scheme that hexafluoropropylene oxide and bisphenol A are reacted to prepare a fluorine-containing functional monomer, and then the antifouling flame-retardant waterproof polyester master batch and fiber are prepared. The technical scheme disclosed by CN111041585A selects polysiloxane as a functional component of the water-repellent master batch, and the highest water-wetting grade of the non-woven fabric produced by the functional master batch can reach 4.
However, the above methods have one or more of the following technical problems: firstly, the prepared product has poor waterproof durability, the waterproof performance can be gradually weakened or even disappear along with the use and washing of the fabric, the air permeability and the wearing comfort of the fabric are seriously influenced by adopting a coating mode, more importantly, the commonly used C8 fluorine waterproofing agent can generate nondegradable perfluorooctanoic acid (PFOA) and perfluorooctane sulfonate (PFOS) in synthesis and use, and the post-treatment process has great damage to the environment; secondly, the prepared master batch is only suitable for producing short fibers, but has great difficulty in producing long fibers with higher spinnability requirements; and thirdly, the addition amount of the waterproof agent is high, so that the production cost is greatly increased, and the product quantification and popularization are not facilitated.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of waterproof polyester fibers.
Another object of the present invention is to provide a waterproof fabric.
The technical scheme of the invention is as follows:
a preparation method of waterproof polyester fiber is prepared by mixing dried waterproof polyester master batch and PET granules, and then carrying out melt spinning and post false twisting, and the preparation method of the waterproof polyester master batch comprises the following steps:
a. fully and uniformly mixing partially fluorinated piperazine amide, titanium dioxide and polyamide wax to obtain first mixed powder;
b. b, adding polyester mixed powder, pentaerythritol and a composite stabilizer into the first mixed powder obtained in the step a, and uniformly mixing to obtain second mixed powder, wherein the polyester mixed powder consists of PET powder and PBT powder, and the composite stabilizer consists of IRGAFOS 168 and IRGANOX 1010;
c. and c, melting and blending the second mixed powder obtained in the step b by using a vacuum double-screw extruder, and then granulating to obtain the waterproof polyester master batch.
In a preferred embodiment of the present invention, the number of fluorinated carbon atoms in the structural formula in the partially fluorinated piperazine amide is ≦ 5.
In a preferred embodiment of the invention, the polyester mixed powder consists of PET powder with the intrinsic viscosity of 0.8dL/g and PBT powder with the intrinsic viscosity of 1.0dL/g in a mass ratio of 60-70: 30-40 (the preferred mass ratio is 65: 35).
In a preferred embodiment of the present invention, the composite stabilizer consists of IRGAFOS 168 and IRGANOX 1010 in a mass ratio of 0.8-1.2: 0.8-1.2.
In a preferred embodiment of the invention, the ratio of length to diameter of the screws of the vacuum twin-screw extruder is 40:1, the processing temperature of the screws is 265-275 ℃ and the rotation speed of the screws is 350-450rpm.
In a preferred embodiment of the present invention, the mass ratio of the partially fluorinated piperazine amide, the titanium dioxide, the polyamide wax, the polyester mixed powder and the composite stabilizer is 9-11:4-6:4-5:75-85:0.4-0.6, and the content of pentaerythritol in the second mixed powder is 190-210ppm.
In a preferred embodiment of the present invention, the method comprises the steps of:
(1) Mixing the dried waterproof polyester master batch with the water content of below 30ppm and PET granules according to the mass ratio of 8-10:90-92, and carrying out melt spinning and oiling at 270-280 ℃ to obtain pre-oriented yarns, wherein the melt spinning speed is 2700-3000m/min, and the oiling rate is 1.0-3.0%;
(2) The water-proof polyester fiber is prepared by false twisting and oiling the pre-oriented yarn, wherein the temperature of a first hot box for false twisting is 140-180 ℃, the temperature of a second hot box is 120-180 ℃, the drafting multiplying factor is 1.65-1.78, the processing speed is 500-800m/min, and the oiling rate is 2.0-4.0%.
Further preferably, the mother liquor of the oil agent used for oiling in said step (1) is made from 64-66wt% of C8-18 fatty acid polyethylene glycol ester, 13-15wt% of polyoxyethylene dioleate, 14-169wt% of POE/POP alkyl ether, 1-3wt% of potassium alkyl phosphate, 2-4wt% of POE phosphate potassium salt and 0.5-1.5wt% of water, and the mother liquor and pure water are prepared into a use liquid in a volume ratio of 10-12:88-90 upon oiling.
Further preferably, the oil agent used for oiling in the step (2) consists of 84-86wt% of mineral oil, 4-6wt% of polyethylene glycol fatty acid ester, 2-4wt% of fatty acid ethanol amide, 3-5wt% of fatty alcohol polyoxyethylene ether and 2-4wt% of lauryl alcohol polyoxyethylene ether phosphate potassium salt.
The other technical scheme of the invention is as follows:
the waterproof fabric is prepared from the waterproof polyester fiber prepared by the preparation method.
The invention has the beneficial effects that:
1. the preparation method of the special waterproof polyester master batch is simple, safe, environment-friendly and good in spinnability, and can be used for producing filaments with the filament number of 0.38 dpf.
2. The waterproof polyester fiber prepared by the invention uses special spinning and false twisting oiling agents, and is beneficial to the subsequent processing treatment of the fiber.
3. The woven fabric sample prepared from the waterproof polyester fiber has excellent waterproof performance and good durability after being fully deoiled and heat-set.
Detailed Description
The technical solution of the present invention is further illustrated and described by the following detailed description.
In the following examples, the number of fluorinated carbon atoms in the structural formula of the partially fluorinated piperazine amide is 4, the composite stabilizer consists of IRGAFOS 168 and IRGANOX 1010 in a mass ratio of 1: 1, the particle size of the titanium dioxide is 0.2-0.4 μm, and the particle size of the polyamide wax is not more than 5 μm.
The preparation method of the waterproof polyester master batch comprises the following steps:
a. fully and uniformly mixing 10 parts by weight of partially fluorinated piperazine amide, 5 parts by weight of titanium dioxide and 4.5 parts by weight of polyamide wax to obtain first mixed powder;
b. b, adding 80 parts by weight of polyester mixed powder, 200ppm of pentaerythritol and 0.5 part by weight of composite stabilizer into the first mixed powder obtained in the step a, and uniformly mixing to obtain second mixed powder;
c. and c, melting and blending the second mixed powder obtained in the step b by using a vacuum double-screw extruder (the length-diameter ratio of a screw of the vacuum double-screw extruder is 40:1, the processing temperature of the screw is 270 ℃, and the rotating speed of the screw is 400 rpm), and then granulating to obtain the waterproof polyester master batch.
The polyester mixed powder consists of PET powder with the intrinsic viscosity of 0.8dL/g and PBT powder with the intrinsic viscosity of 1.0dL/g in a mass ratio of 65: 35.
The specific process of melt spinning and oiling comprises the following steps: the preparation method comprises the steps of uniformly mixing the waterproof polyester master batch and PET granules, heating and melting the mixture in a spinning screw pump through an intermediate bin, conveying the mixture to a spinning assembly through a filter and a melt pipeline, accurately metering and pressurizing the mixture through a metering pump, extruding the mixture through a spinneret orifice of a spinneret plate, blowing and cooling the mixture, oiling and winding the mixture to obtain the pre-oriented yarn.
The mother liquor of the oil agent for oiling in the following step (1) was prepared from 65wt% of C8-18 fatty acid polyethylene glycol ester, 14wt% of polyoxyethylene dioleate, 15wt% of POE/POP alkyl ether, 2wt% of potassium alkyl phosphate, 3wt% of POE potassium phosphate, and 1wt% of water, and when oiling, the mother liquor was blended with pure water in a volume ratio of 12:88 to prepare a use liquid.
The oiling agent used in the step (2) is composed of 85wt% of mineral oil, 5wt% of polyethylene glycol fatty acid ester, 3wt% of fatty acid ethanol amide, 4wt% of fatty alcohol-polyoxyethylene ether and 3wt% of lauryl alcohol-polyoxyethylene ether phosphate potassium salt.
Example 1
(1) Mixing the dried waterproof polyester master batch with the water content of below 30ppm and PET granules according to the mass ratio of 10:90, and carrying out melt spinning and oiling at 278 ℃ to obtain pre-oriented yarns, wherein the melt spinning speed is 2800m/min, and the oiling rate is 1.0%;
(2) The pre-oriented yarns are subjected to false twisting processing and oiling to prepare the waterproof polyester fiber (the specification is 83dtex/36 f.), the temperature of a first hot box of the false twisting processing is 140 ℃, the temperature of a second hot box is 120 ℃, the drafting multiplying factor is 1.68, the processing speed is 600m/min, and the oiling rate is 2.0%.
Example 2
(1) Mixing the dried waterproof polyester master batch with the water content of below 30ppm and PET granules according to the mass ratio of 10:90, and carrying out melt spinning and oiling at 278 ℃ to obtain pre-oriented yarns, wherein the melt spinning speed is 2800m/min, and the oiling rate is 1.5%;
(2) The pre-oriented yarn is subjected to false twisting processing and oiling to prepare the waterproof polyester fiber (the specification is 110dtex/48 f.), the temperature of a first hot box of the false twisting processing is 160 ℃, the temperature of a second hot box is 160 ℃, the drafting multiplying power is 1.68, the processing speed is 700m/min, and the oiling rate is 2.5%.
Example 3
(1) Mixing the dried waterproof polyester master batch with the water content of below 30ppm and PET granules according to the mass ratio of 10:90, and carrying out melt spinning and oiling at 278 ℃ to obtain pre-oriented yarns, wherein the melt spinning speed is 2800m/min, and the oiling rate is 2.0%;
(2) The pre-oriented yarn is subjected to false twisting processing and oiling to prepare the waterproof polyester fiber (the specification is 83dtex/48 f.), the temperature of a first hot box of the false twisting processing is 160 ℃, the temperature of a second hot box is 140 ℃, the drafting multiplying power is 1.68, the processing speed is 800m/min, and the oiling rate is 3.0%.
Example 4
(1) Mixing the dried waterproof polyester master batch with the water content of below 30ppm and PET granules according to the mass ratio of 8: 92, and carrying out melt spinning and oiling at 278 ℃ to obtain pre-oriented yarns, wherein the melt spinning speed is 2800m/min, and the oiling rate is 3.0%;
(2) The pre-oriented yarns are subjected to false twisting processing and oiling to prepare the waterproof polyester fiber (the specification is 55dtex/144 f), the temperature of a first hot box of the false twisting processing is 170 ℃, the temperature of a second hot box is 150 ℃, the drafting multiplying power is 1.68, the processing speed is 700m/min, and the oiling rate is 3.0%.
The waterproof polyester fiber prepared in the above example was prepared by the following method for testing the waterproof property: the prepared waterproof polyester fiber is processed into a woven sample cloth, the woven sample cloth is shaped for 2min at 190 ℃ after being fully degreased and dried, the waterproof performance is detected according to the national standard GB/T4745-2012 (detection and evaluation of the waterproof performance of the textile, a water dipping method), the waterproof performance is respectively tested at the temperature of 25 ℃ and 50 ℃, and the test results are shown in the table 1:
TABLE 1 Water repellency of Water-repellent polyester fiber fabrics prepared in examples 1-4
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims.
Claims (3)
1. A preparation method of waterproof polyester fiber is characterized by comprising the following steps: mixing the dried waterproof polyester master batch with PET granules, and then carrying out melt spinning and subsequent false twisting to prepare the waterproof polyester master batch, wherein the preparation method of the waterproof polyester master batch comprises the following steps:
a. fully and uniformly mixing partially fluorinated piperazine amide, titanium dioxide and polyamide wax to obtain first mixed powder, wherein the number of fluorinated carbon atoms in a structural formula of the partially fluorinated piperazine amide is less than or equal to 5;
b. b, adding polyester mixed powder, pentaerythritol and a composite stabilizer into the first mixed powder obtained in the step a, uniformly mixing to obtain second mixed powder, wherein the polyester mixed powder consists of PET powder with the intrinsic viscosity of 0.8dL/g and PBT powder with the intrinsic viscosity of 1.0dL/g in a mass ratio of 60-70: 30-40, and the composite stabilizer consists of IRGAFOS 168 and IRGANOX 1010 in a mass ratio of 0.8-1.2: 0.8-1.2; the mass ratio of the partially fluorinated piperazine amide to the titanium dioxide to the polyamide wax to the polyester mixed powder to the composite stabilizer is 9-11, and the mass ratio of the partially fluorinated piperazine amide to the titanium dioxide to the polyamide wax to the polyester mixed powder to the composite stabilizer is 75-6:4-5, and the content of pentaerythritol in the second mixed powder is 190-210ppm;
c. b, melting and blending the second mixed powder obtained in the step b by using a vacuum double-screw extruder, and then granulating to obtain the waterproof polyester master batch;
the preparation method of the waterproof polyester fiber comprises the following steps:
(1) Mixing the dried waterproof polyester master batch with the water content of below 30ppm and PET granules according to the mass ratio of 8-10 to 90-92, carrying out melt spinning at 270-280 ℃, and oiling to obtain pre-oriented yarns, wherein the melt spinning speed is 2700-3000m/min, and the oiling rate is 1.0-3.0%; the mother liquor of the oiling agent used in the step is prepared from 64-66wt% of C8-18 fatty acid polyethylene glycol ester, 13-15wt% of polyoxyethylene dioleate, 14-16wt% of POE/POP alkyl ether, 1-3wt% of potassium alkyl phosphate, 2-4wt% of potassium POE phosphate and 0.5-1.5wt% of water, and when oiling, the mother liquor and pure water are prepared into a use liquid according to the volume ratio of 10-12;
(2) The pre-oriented yarn is subjected to false twisting and oiling to prepare the waterproof polyester fiber, wherein the temperature of a first hot box for false twisting is 140-180 ℃, the temperature of a second hot box is 120-180 ℃, the drafting multiplying factor is 1.65-1.78, the processing speed is 500-800m/min, and the oiling rate is 2.0-4.0%; the oiling agent used in the oiling step consists of 84-86wt% of mineral oil, 4-6wt% of polyethylene glycol fatty acid ester, 2-4wt% of fatty acid ethanolamide, 3-5wt% of fatty alcohol polyoxyethylene ether and 2-4wt% of lauryl alcohol polyoxyethylene ether phosphate potassium salt.
2. The method of claim 1, wherein: the length-diameter ratio of a screw of the vacuum double-screw extruder is 40, the processing temperature of the screw is 265-270 ℃, and the rotating speed of the screw is 350-450rpm.
3. A waterproof fabric characterized by: the raw material comprises the waterproof polyester fiber prepared by the preparation method of claim 1 or 2.
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| MX2022000197A (en) * | 2008-09-30 | 2022-03-02 | Shaw Ind Group Inc | Recycled polyethylene terephthalate compositions, fibers and articles produced therefrom, and methods for producing same. |
| CN102964782B (en) * | 2012-12-12 | 2015-02-25 | 厦门翔鹭化纤股份有限公司 | Low-melting-point polyester master batch and preparation method thereof |
| CN103469568B (en) * | 2013-09-26 | 2017-01-04 | 江苏立新化纤科技有限公司 | A kind of fluorine-containing polyester FDY fiber oil preparation and preparation method thereof |
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