CN107988650B - Preparation method of graphene-enhanced polyester fiber - Google Patents
Preparation method of graphene-enhanced polyester fiber Download PDFInfo
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- CN107988650B CN107988650B CN201711274206.3A CN201711274206A CN107988650B CN 107988650 B CN107988650 B CN 107988650B CN 201711274206 A CN201711274206 A CN 201711274206A CN 107988650 B CN107988650 B CN 107988650B
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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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
-
- 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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Artificial Filaments (AREA)
Abstract
The invention relates to the field of textile fibers, and discloses a preparation method of graphene-reinforced polyester fibers, which comprises the following steps: 1) adding graphene powder into deionized water, uniformly dispersing, adjusting the pH value to 11-12, heating to 65-75 ℃, dropwise adding an aluminum sulfate solution while adjusting the pH value to 6-7, stirring and curing after dropwise adding, washing to be neutral, and drying to obtain primary coated graphene; 2) mixing the primary coated graphene with water and polyethylene glycol, grinding, washing and drying to obtain secondary coated graphene; 3) preparing a PET slice; 4) spinning to obtain the finished product. The polyester fiber prepared by the method can effectively improve the strength of the polyester fiber on the premise of keeping the hand feeling of the polyester fiber. In addition, the graphene is added into the polyester fiber, so that the dispersity of the graphene can be improved, and the graphene is not easy to agglomerate.
Description
Technical Field
The invention relates to the field of textile fibers, in particular to a preparation method of graphene-enhanced polyester fibers.
Background
Polyester fiber is an important variety of synthetic fiber, and is fiber prepared by using Purified Terephthalic Acid (PTA) or dimethyl terephthalate (DMT) and Ethylene Glycol (EG) as raw materials, performing esterification or ester exchange and polycondensation to prepare fiber-forming high polymer, namely polyethylene terephthalate (PET), and spinning and post-processing the fiber. Polyester fibers are one of the main textile fibers.
There are many high-strength polyester fiber products on the market, and additives with reinforcing function are usually added into the polyester fibers. For example, patent application No. CN201710443947.3 discloses a modified polyester fiber product, in which graphene sheets are present inside and outside the polyester fiber; the polyester fiber product comprises polyester fibers, polyester fiber yarns and polyester fiber fabrics. According to the invention, graphene is attached or added to the inside and the outside of the polyester fiber, so that the uniformity and the firmness of the graphene are improved; according to the invention, the strength of the polyester fiber is improved by adding the graphene and/or the biomass graphene.
However, similar to the above-mentioned technical solution of directly adding the reinforcing agent to the polyester fiber, the reinforcing agent has poor dispersibility due to poor compatibility with the polyester material, and is easily agglomerated, thereby affecting the performance of the function.
Disclosure of Invention
In order to solve the technical problem, the invention provides a preparation method of graphene reinforced polyester fibers. The polyester fiber prepared by the method can effectively improve the strength of the polyester fiber on the premise of keeping the hand feeling of the polyester fiber. In addition, the graphene is added into the polyester fiber, so that the dispersity of the graphene can be improved, and the graphene is not easy to agglomerate.
The specific technical scheme of the invention is as follows: a preparation method of graphene reinforced polyester fibers comprises the following steps:
1) adding graphene powder into deionized water, uniformly dispersing, adjusting the pH value to 11-12, heating to 65-75 ℃, dropwise adding an aluminum sulfate solution while adjusting the pH value to 6-7, stirring and curing after dropwise adding, washing to be neutral, and drying to obtain primary coated graphene;
2) mixing the primary coated graphene with water and polyethylene glycol, grinding, washing and drying to obtain secondary coated graphene;
3) mixing and stirring terephthalic acid and ethylene glycol uniformly, heating for esterification reaction, then adding secondary coated graphene and antimony acetate, heating for polycondensation reaction, cooling and slicing to obtain PET slices;
4) and spinning the PET chips according to a conventional spinning process to obtain the finished product.
The invention adopts graphene as a functional additive for improving the physical properties of polyester fibers. The graphene has strong physical properties and can improve the breaking strength of the polyester fiber. However, graphene is not easily dispersed in polyester and is easily agglomerated due to poor compatibility with polyester.
Therefore, aluminum is used as a precursor of amorphous alumina, colloid is formed after reaction, the amorphous alumina is coated on the surface of graphene, the surface of the amorphous alumina contains a large number of hydroxyl groups, the reaction activity is higher, and the compatibility and the dispersibility of the graphene and polyester are improved. Then, the surface of the graphene is further coated with polyethylene glycol, the polyethylene glycol can participate in the condensation polymerization reaction of polyester, so that the binding property of the graphene and the polyester is better, and meanwhile, due to the good compatibility of the polyethylene glycol and the polyester monomer, the steric hindrance of the graphene in the condensation polymerization reaction can be reduced, the dispersibility of the graphene is further improved, and the graphene is not easy to agglomerate.
In addition, although graphene is effective in improving the breaking strength of polyester fibers, as a raw material for textile fibers, need to be frequently in contact with human skin. Graphene is in reinforcing polyester fiber physical properties, because its granule is comparatively crude, can make polyester fiber surface become to have the hair, has burr sense when contacting with the skin, influences the use and experiences. The graphene is coated for the second time, so that the roughness of graphene particles is greatly reduced, and the hand feeling of the fiber is improved.
Further, in the step 1), the mass ratio of the graphene powder to the aluminum sulfate is 100: 6-8.
Further, in the step 2), the mass usage ratio of the primary coated graphene to the polyethylene glycol is 100: 8-18.
Further, in the step 3), the mass ratio of the terephthalic acid, the ethylene glycol, the secondary coated graphene and the antimony acetate is 90-110:40-60:1-5: 0.5-1.5.
Further, in the step 3), the esterification reaction temperature is 240-250 ℃, and the esterification pressure is 0.3-0.4 MPa.
Further, in the step 3), the polycondensation reaction temperature is 265-275 ℃, and the polycondensation pressure is 400-600 Pa.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention can effectively improve the physical properties of the polyester fiber on the premise of keeping the hand feeling of the polyester fiber.
2. According to the invention, the graphene is added into the polyester fiber, and the dispersibility of the graphene can be improved, so that the graphene is not easy to agglomerate.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
A preparation method of graphene reinforced polyester fibers comprises the following steps:
1) adding graphene powder into deionized water, uniformly dispersing, adjusting the pH value to 11.5, heating to 70 ℃, dropwise adding an aluminum sulfate solution while adjusting the pH value to 6.5 with an acid solution, stirring and curing after dropwise adding, washing to be neutral, and drying to obtain the primary coated graphene. Wherein the mass usage ratio of the graphene to the aluminum sulfate is 100: 7.
2) And mixing the primary coated graphene with water and polyethylene glycol, grinding, washing and drying to obtain the secondary coated graphene. Wherein the mass usage ratio of the primary coated graphene to the polyethylene glycol is 100: 13.
3) Mixing terephthalic acid and ethylene glycol, stirring uniformly, heating for esterification reaction (245 ℃, 0.35MPa of ester), then adding secondary coated graphene and antimony acetate, heating for polycondensation reaction (270 ℃, 500Pa), cooling and slicing to obtain PET slices; wherein the mass usage ratio of the terephthalic acid, the ethylene glycol, the secondary coated graphene and the antimony acetate is 100:50:3: 1.
4) And spinning the PET chips according to a conventional spinning process to obtain the finished product.
Example 2
A preparation method of graphene reinforced polyester fibers comprises the following steps:
1) adding graphene powder into deionized water, uniformly dispersing, adjusting the pH value to 11, heating to 65 ℃, dropwise adding an aluminum sulfate solution while adjusting the pH value to 6 with an acid solution, stirring and curing after dropwise adding, washing to be neutral, and drying to obtain the primary coated graphene. Wherein the mass usage ratio of the graphene to the aluminum sulfate is 100: 6.
2) And mixing the primary coated graphene with water and polyethylene glycol, grinding, washing and drying to obtain the secondary coated graphene. Wherein the mass usage ratio of the primary coated graphene to the polyethylene glycol is 100: 8.
3) Mixing terephthalic acid and ethylene glycol, stirring uniformly, heating for esterification reaction (240 ℃, 0.3MPa of ester), then adding secondary coated graphene and antimony acetate, heating for polycondensation reaction (265 ℃, 400Pa), cooling and slicing to obtain PET slices; wherein the mass usage ratio of the terephthalic acid, the ethylene glycol, the secondary coated graphene and the antimony acetate is 90:40:1: 0.5.
4) And spinning the PET chips according to a conventional spinning process to obtain the finished product.
Example 3
A preparation method of graphene reinforced polyester fibers comprises the following steps:
1) adding graphene powder into deionized water, uniformly dispersing, adjusting the pH value to 12, heating to 75 ℃, dropwise adding an aluminum sulfate solution while adjusting the pH value to 7 with an acid solution, stirring and curing after dropwise adding, washing to be neutral, and drying to obtain the primary coated graphene. Wherein the mass usage ratio of the graphene to the aluminum sulfate is 100: 8.
2) And mixing the primary coated graphene with water and polyethylene glycol, grinding, washing and drying to obtain the secondary coated graphene. Wherein the mass usage ratio of the primary coated graphene to the polyethylene glycol is 100: 18.
3) Mixing terephthalic acid and ethylene glycol, stirring uniformly, heating for esterification reaction (250 ℃, 0.4MPa of ester), then adding secondary coated graphene and antimony acetate, heating for polycondensation reaction (275 ℃, 600Pa), cooling, and slicing to obtain PET slices; wherein the mass and dosage ratio of the terephthalic acid, the ethylene glycol, the secondary coated graphene and the antimony acetate is 110:60:5: 1.5.
4) And spinning the PET chips according to a conventional spinning process to obtain the finished product.
Comparative example 1
The difference from example 4 is that: the graphene is directly added without coating treatment.
According to the method of GBTGBT 16604-2008 polyester fiber industrial filament, the performance of the polyester fiber industrial filament prepared by the invention is compared with that of other polyester fiber industrial filaments, and the results are as follows:
| group of | Breaking strength | Surface hand feeling |
| Example 1 | 8.9cN/dtex | Smooth hand feeling |
| Comparative example 1 | 8.8cN/dtex | Rough and ragged hand feeling |
Comparative example 1 the reason why the breaking strength is not as high as that of example 1 is that the dispersibility of graphene in comparative example 1 is not good, thereby affecting the performance of graphene.
The raw materials and equipment used in the invention are common raw materials and equipment in the field if not specified; the methods used in the present invention are conventional in the art unless otherwise specified.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, alterations and equivalents of the above embodiments according to the technical spirit of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (3)
1. A preparation method of graphene reinforced polyester fibers is characterized by comprising the following steps:
1) adding graphene powder into deionized water, uniformly dispersing, adjusting the pH value to 11-12, heating to 65-75 ℃, dropwise adding an aluminum sulfate solution while adjusting the pH value to 6-7, stirring and curing after dropwise adding, washing to be neutral, and drying to obtain primary coated graphene; the mass ratio of the graphene powder to the aluminum sulfate is 100: 6-8;
2) mixing the primary coated graphene with water and polyethylene glycol, grinding, washing and drying to obtain secondary coated graphene; the mass ratio of the primary coated graphene to the polyethylene glycol is 100: 8-18;
3) mixing and stirring terephthalic acid and ethylene glycol uniformly, heating for esterification reaction, then adding secondary coated graphene and antimony acetate, heating for polycondensation reaction, cooling and slicing to obtain PET slices; the mass ratio of the terephthalic acid to the ethylene glycol to the secondary coated graphene to the antimony acetate is 90-110:40-60:1-5: 0.5-1.5;
4) and spinning the PET chips according to a conventional spinning process to obtain the finished product.
2. The method for preparing the graphene-reinforced polyester fiber according to claim 1, wherein in the step 3), the esterification reaction temperature is 240-250 ℃ and the esterification pressure is 0.3-0.4 MPa.
3. The method as claimed in claim 2, wherein in step 3), the temperature of the polycondensation reaction is 265-275 ℃, and the pressure of the polycondensation reaction is 400-600 Pa.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711274206.3A CN107988650B (en) | 2017-12-06 | 2017-12-06 | Preparation method of graphene-enhanced polyester fiber |
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| CN201711274206.3A CN107988650B (en) | 2017-12-06 | 2017-12-06 | Preparation method of graphene-enhanced polyester fiber |
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| CN107988650A CN107988650A (en) | 2018-05-04 |
| CN107988650B true CN107988650B (en) | 2020-06-30 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105525381A (en) * | 2015-10-27 | 2016-04-27 | 济南圣泉集团股份有限公司 | Graphene-containing composite polyester fiber and its preparation method and use |
| CN105820519A (en) * | 2016-02-29 | 2016-08-03 | 洛阳尖端技术研究院 | PET-based graphene composite material, preparation method thereof, and aerostat |
| CN107083578A (en) * | 2017-04-27 | 2017-08-22 | 南通强生石墨烯科技有限公司 | The preparation method of graphene elastic polyester in-situ polymerization composite functional fiber |
| CN107190382A (en) * | 2017-06-26 | 2017-09-22 | 杭州高烯科技有限公司 | Polyester blended fabric that a kind of graphene is modified and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10774450B2 (en) * | 2016-02-24 | 2020-09-15 | Tingying Zeng | Method to massively manufacture carbon fibers through graphene composites and the use thereof |
-
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- 2017-12-06 CN CN201711274206.3A patent/CN107988650B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105525381A (en) * | 2015-10-27 | 2016-04-27 | 济南圣泉集团股份有限公司 | Graphene-containing composite polyester fiber and its preparation method and use |
| CN105820519A (en) * | 2016-02-29 | 2016-08-03 | 洛阳尖端技术研究院 | PET-based graphene composite material, preparation method thereof, and aerostat |
| CN107083578A (en) * | 2017-04-27 | 2017-08-22 | 南通强生石墨烯科技有限公司 | The preparation method of graphene elastic polyester in-situ polymerization composite functional fiber |
| CN107190382A (en) * | 2017-06-26 | 2017-09-22 | 杭州高烯科技有限公司 | Polyester blended fabric that a kind of graphene is modified and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| "石墨烯/氧化铝复合粉体的制备及其在浇注料中的应用";熊鑫;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20140415(第4期);第B020-132页 * |
| "超细氧化铝的制备及改性研究";朱梅琴;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20131215(第S2期);第B014-47页 * |
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Effective date of registration: 20200604 Address after: 515000 Huaguang Industrial Zone, Gu Rao Town, Chaoyang District, Guangdong, Shantou Applicant after: Guangdong Jinlong fabric technology Co., Ltd Address before: 362804 No. 169, Qiu Cun, Qiu Cun, Quanzhou Town, Quangang District, Fujian, China Applicant before: Qiu Longhai |
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