CN113321867A - Preparation method of composite glass fiber - Google Patents
Preparation method of composite glass fiber Download PDFInfo
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- CN113321867A CN113321867A CN202010829253.5A CN202010829253A CN113321867A CN 113321867 A CN113321867 A CN 113321867A CN 202010829253 A CN202010829253 A CN 202010829253A CN 113321867 A CN113321867 A CN 113321867A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/02—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor
- C03B37/022—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor from molten glass in which the resultant product consists of different sorts of glass or is characterised by shape, e.g. hollow fibres, undulated fibres, fibres presenting a rough surface
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/48—Coating with two or more coatings having different compositions
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
- C08J5/08—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials glass fibres
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2469/00—Characterised by the use of polycarbonates; Derivatives of polycarbonates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
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- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Polymers & Plastics (AREA)
- Geochemistry & Mineralogy (AREA)
- Health & Medical Sciences (AREA)
- Manufacturing & Machinery (AREA)
- General Chemical & Material Sciences (AREA)
- Surface Treatment Of Glass Fibres Or Filaments (AREA)
- Reinforced Plastic Materials (AREA)
Abstract
The invention relates to the technical field of composite glass fiber preparation, in particular to a preparation method of composite glass fiber. The preparation method of the composite glass fiber comprises the steps of heating glass to the temperature of wire drawing viscosity, drawing the glass fiber into the glass fiber, spraying a layer of impregnating compound on the surface of the glass fiber in a spraying mode, and cooling the glass fiber to 180-240 ℃; the resin is doped with the perfluorinated cationic surfactant, then the resin doped with the perfluorinated cationic surfactant is melted at the melting temperature of 150-170 ℃, the melted resin is placed in a resin containing groove, the glass fiber sprayed with the impregnating compound is cooled to the temperature of 180-240 ℃ and then rapidly passes through the resin containing groove, a resin layer is formed on the surface of the glass fiber, and the plastic property is extruded. The preparation method of the composite glass fiber improves the uniformity of the resin attached to the surface of the glass fiber, and further improves various performances of the composite glass fiber material.
Description
Technical Field
The invention relates to the technical field of composite glass fiber preparation, in particular to a preparation method of composite glass fiber.
Background
The commonly used glass fiber composite material refers to a resin-based composite material, and can adopt molding processes such as hand pasting, winding, pressing and the like, and can also adopt injection and pultrusion molding processes.
One of the existing production methods of composite glass fiber is to soak the finished glass fiber yarn in resin (yarn running in resin liquid), and then to cut the yarn, so that the produced product contains 60% of glass fiber and 40% of resin. The problem of this mode of production is that the resin sticks to the surface of the glass fiber, and the resin and the glass fiber are not mixed uniformly.
The second existing production method of composite glass fiber is to heat the glass fiber roll/filament finished product and the resin finished product at high temperature (about 1000 ℃) to make the two products in a molten state, and then mix the two products and perform extrusion molding, so that the produced product contains 70% of glass fiber and 30% of resin. The production method has the problems that when the impregnating agent coating equipment is started and shut down, the impregnating agent coated on the glass fiber yarns is not uniform, so that the resin adhered to the glass fiber yarns is not uniform, and the performance of the composite glass fiber is influenced.
Disclosure of Invention
The invention aims to provide a preparation method of composite glass fiber, which overcomes the defects of the production mode of the composite glass fiber in the prior art and enables the resin and the glass fiber of the finally prepared composite glass fiber to be uniformly mixed.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of composite glass fiber comprises the following steps:
(1) heating the glass to the temperature of drawing viscosity of 1000-1200 ℃, drawing the glass into glass fiber, spraying a layer of impregnating compound on the surface of the glass fiber in a spraying manner, and cooling the glass fiber to the temperature of 180-240 ℃;
(2) doping a perfluorinated cationic surfactant in resin, then melting the resin doped with the perfluorinated cationic surfactant at the melting temperature of 150-170 ℃, placing the melted resin in a resin containing groove, cooling the glass fiber coated with the impregnating compound to the temperature of 180-240 ℃, and quickly passing through the resin containing groove to form a resin layer on the surface of the glass fiber;
(3) and adding the glass fiber of the marked line formed resin layer into a double-screw extruder, extruding and performing injection molding to obtain the composite glass fiber.
Preferably, the spraying thickness of the impregnating compound is 500nm-50 μm.
Preferably, the size is mainly prepared from methyl silicone oil, triethylene diamine, synde 141 polymer dispersion and lithium nitrate according to the weight ratio of (5-7): (1-3): 3: 1; the synde 141 polymer is dispersed into a polymer dispersant with the model number of synde 141, which is produced and manufactured by new material science and technology Limited liability company of Zhuhai Xiandade.
Preferably, the resin is mainly formed by one or more of PP resin, PCE resin, PET resin, PA resin and PC resin.
Preferably, the resin is mainly prepared from PP resin, PCE resin, PET resin, PA resin and PC resin according to the weight ratio of (20-40): (5-18): (0-7): (0-7): (3-10) are compounded.
Preferably, the impregnating compound mainly comprises methyl silicone oil, triethylene diamine, synde 141 polymeric dispersant and lithium nitrate according to the weight ratio of 6: 2: 3: 1.
Preferably, the resin is mainly prepared from PP resin, PCE resin, PET resin, PA resin and PC resin according to a weight ratio of 30: 12: 5: 2: 7 are compounded.
Preferably, the temperature of the glass fiber is reduced to 210 ℃ in the step (1).
Preferably, the perfluorinated cationic surfactant is a perfluorinated cationic surfactant manufactured by Wuhanding high tech, Inc. and having a model number of FC-911.
Preferably, the resin melting temperature is 160 ℃.
The invention has the beneficial effects that: compared with the prior art, the preparation method of the composite glass fiber has the following advantages: (1) directly mixing the molten glass fiber on a glass fiber production line with resin in a molten state, and then extruding and shaping, wherein 70% of glass fiber and 30% of resin in the produced product are not limited by the drawing length, so that the cost is saved; (2) after the glass fiber is drawn, an impregnating compound is sprayed, so that the glass fiber is more easily and uniformly mixed with resin, wherein the methyl silicone oil in the impregnating compound improves the lubricating fluidity when the resin is in contact with the surface of the glass fiber, so that the extension efficiency and the performance of the resin on the glass fiber are improved, the synde 141 high-molecular dispersing agent eliminates fine bubbles generated in the mixing process of the glass fiber and the resin, and simultaneously, the resin is uniformly dispersed on the surface of a glass fiber yarn as a dispersing agent, lithium nitrate is used for improving the combination degree between the surface of the glass fiber yarn and the resin, and triethylene diamine emulsifies and bonds the whole impregnating compound together, so that the performance of the synergistic effect of all components is improved; (3) the perfluorinated cationic surfactant is added into the resin, so that the self-wetting effect of the resin is improved, the surface tension in the bonding process of the resin and the glass fiber is reduced, and the efficiency and the uniformity in the bonding process of the resin and the glass fiber are improved.
Detailed Description
Example 1
A preparation method of composite glass fiber comprises the following steps:
(1) heating glass to the temperature of 1080 ℃ of wire drawing viscosity, drawing the glass into glass fibers, and spraying a layer of impregnating compound on the surfaces of the glass fibers in a spraying manner to cool the glass fibers to 210 ℃;
(2) doping a perfluorinated cationic surfactant in resin, then melting the resin doped with the perfluorinated cationic surfactant at the melting temperature of 160 ℃, placing the melted resin in a resin containing groove, cooling the glass fiber sprayed with the impregnating compound to 160 ℃, and then quickly passing through the resin containing groove to form a resin layer on the surface of the glass fiber;
(3) and adding the glass fiber of the marked line formed resin layer into a double-screw extruder, extruding and performing injection molding to obtain the composite glass fiber.
The spraying thickness of the impregnating compound is 200 nm.
The impregnating compound is mainly prepared from methyl silicone oil, triethylene diamine, synde 141 macromolecule dispersion and lithium nitrate according to the weight ratio of 6: 2: 3: 1; the synde 141 polymer is dispersed into a polymer dispersant with the model number of synde 141, which is produced and manufactured by new material science and technology Limited liability company of Zhuhai Xiandade.
The resin is mainly prepared from PP resin, PCE resin, PET resin, PA resin and PC resin according to the weight ratio of 30: 12: 5: 2: 7 are compounded.
The perfluorinated cationic surfactant is a perfluorinated cationic surfactant which is manufactured by Wuhanding high-tech limited and has the model number of FC-911.
Example 2
A preparation method of composite glass fiber comprises the following steps:
(1) heating glass to 1050 ℃ of drawing viscosity, drawing the glass into glass fiber, and spraying a layer of impregnating compound on the surface of the glass fiber in a spraying manner to cool the glass fiber to 180 ℃;
(2) doping a perfluorinated cationic surfactant in resin, then melting the resin doped with the perfluorinated cationic surfactant at the melting temperature of 150 ℃, placing the melted resin in a resin containing groove, cooling the glass fiber sprayed with the impregnating compound to 180 ℃, and then quickly passing through the resin containing groove to form a resin layer on the surface of the glass fiber;
(3) and adding the glass fiber of the marked line formed resin layer into a double-screw extruder, extruding and performing injection molding to obtain the composite glass fiber.
The spraying thickness of the impregnating compound is 500nm and mu m.
The impregnating compound is mainly prepared from methyl silicone oil, triethylene diamine, synde 141 macromolecule dispersion and lithium nitrate according to the weight ratio of 5: 1: 3: 1; the synde 141 polymer is dispersed into a polymer dispersant with the model number of synde 141, which is produced and manufactured by new material science and technology Limited liability company of Zhuhai Xiandade.
The resin is mainly prepared from PP resin, PCE resin and PC resin according to the weight ratio of 20: 5: (3 is prepared by compounding.
The perfluorinated cationic surfactant is a perfluorinated cationic surfactant which is manufactured by Wuhanding high-tech limited and has the model number of FC-911.
Example 3
A preparation method of composite glass fiber comprises the following steps:
(1) heating glass to the temperature of wire drawing viscosity of 1200 ℃, drawing the glass fiber, spraying a layer of impregnating compound on the surface of the glass fiber in a spraying manner, and cooling the glass fiber to 240 ℃;
(2) doping a perfluorinated cationic surfactant in resin, then melting the resin doped with the perfluorinated cationic surfactant at the melting temperature of 170 ℃, placing the melted resin in a resin containing groove, cooling the glass fiber sprayed with the impregnating compound to 240 ℃, and quickly passing through the resin containing groove to form a resin layer on the surface of the glass fiber;
(3) and adding the glass fiber of the marked line formed resin layer into a double-screw extruder, extruding and performing injection molding to obtain the composite glass fiber.
The spraying thickness of the impregnating compound is 50 mu m.
The impregnating compound is mainly prepared from methyl silicone oil, triethylene diamine, synde 141 macromolecule dispersion and lithium nitrate according to the weight ratio of 7: 3: 3: 1; the synde 141 polymer is dispersed into a polymer dispersant with the model number of synde 141, which is produced and manufactured by new material science and technology Limited liability company of Zhuhai Xiandade.
The resin is mainly prepared from PP resin, PCE resin, PET resin, PA resin and PC resin according to the weight ratio of 40: 18: 7: 7: 10 are compounded.
The perfluorinated cationic surfactant is a perfluorinated cationic surfactant which is manufactured by Wuhanding high-tech limited and has the model number of FC-911.
Comparative example 1
Comparative example 1 was prepared substantially the same as example 1 except that: the impregnating compound is prepared from methyl silicone oil, triethylene diamine, synde 141 polymer dispersion and lithium nitrate according to the weight ratio of 1: 1: 1: 1.
Comparative example 2
Comparative example 2 was prepared substantially identically to example 1, except that: heating the glass to the temperature of 1080 ℃ of wire drawing viscosity, drawing the glass fiber, and spraying a layer of impregnating compound on the surface of the glass fiber in a spraying manner to cool the glass fiber to 300 ℃.
Test example 1
The composite glass fiber materials of examples 1-3 and comparative examples 1-2 were tested for flexibility, impact strength, and hardness according to the methods of GB/T8805, 1988, GB 1697-82, and GB/T6739-2006, respectively, and the test results are shown in Table 1:
TABLE 1
As can be seen from Table 1, the composite glass fiber materials prepared in examples 1-3 of the present invention have much higher performance than comparative examples 1 and 2.
The above embodiments are only specific examples of the present invention, and the protection scope of the present invention includes but is not limited to the product forms and styles of the above embodiments, and any suitable changes or modifications made by those skilled in the art according to the claims of the present invention shall fall within the protection scope of the present invention.
Claims (10)
1. A preparation method of composite glass fiber is characterized by comprising the following steps: the method comprises the following steps:
(1) heating the glass to the temperature of drawing viscosity of 1000-1200 ℃, drawing the glass into glass fiber, spraying a layer of impregnating compound on the surface of the glass fiber in a spraying manner, and cooling the glass fiber to the temperature of 180-240 ℃;
(2) doping a perfluorinated cationic surfactant in resin, then melting the resin doped with the perfluorinated cationic surfactant at the melting temperature of 150-170 ℃, placing the melted resin in a resin containing groove, cooling the glass fiber coated with the impregnating compound to the temperature of 180-240 ℃, and quickly passing through the resin containing groove to form a resin layer on the surface of the glass fiber;
(3) and adding the glass fiber of the marked line formed resin layer into a double-screw extruder, extruding and performing injection molding to obtain the composite glass fiber.
2. The method of claim 1, wherein the composite glass fiber is prepared by: the spraying thickness of the impregnating compound is 500nm-50 μm.
3. The method of claim 1, wherein the composite glass fiber is prepared by: the impregnating compound is prepared from methyl silicone oil, triethylene diamine, synde 141 macromolecule dispersion and lithium nitrate according to the weight ratio of (5-7): (1-3): 3: 1.
4. The method of claim 1, wherein the composite glass fiber is prepared by: the resin is mainly formed by combining one or more of PP resin, PCE resin, PET resin, PA resin and PC resin.
5. The method of claim 1, wherein the composite glass fiber is prepared by: the resin is mainly prepared from PP resin, PCE resin, PET resin, PA resin and PC resin according to the weight ratio of (20-40): (5-18): (0-7): (0-7): (3-10) are compounded.
6. The method of claim 3, wherein the composite glass fiber is prepared by: the impregnating compound is mainly prepared from methyl silicone oil, triethylene diamine, synde 141 polymeric dispersant and lithium nitrate according to the weight ratio of 6: 2: 3: 1.
7. The method of claim 4, wherein the composite glass fiber is prepared by: the resin is mainly prepared from PP resin, PCE resin, PET resin, PA resin and PC resin according to the weight ratio of 30: 12: 5: 2: 7 are compounded.
8. The method of claim 1, wherein the composite glass fiber is prepared by: in the step (1), the temperature of the glass fiber is reduced to 210 ℃.
9. The method of claim 1, wherein the composite glass fiber is prepared by: the perfluorinated cationic surfactant is a perfluorinated cationic surfactant which is manufactured by Wuhanding high-tech limited and has the model number of FC-911.
10. The method of claim 1, wherein the composite glass fiber is prepared by: the resin melt temperature was 160 ℃.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008111602A1 (en) * | 2007-03-15 | 2008-09-18 | Nippon Electric Glass Co., Ltd. | Glass composition for glass fiber, glass fiber, process for producing glass fiber and composite material |
| CN103660071A (en) * | 2013-12-18 | 2014-03-26 | 上海日之升新技术发展有限公司 | Melt impregnation device for continuous long glass fiber reinforced polyester production as well as impregnation method |
| CN103921388A (en) * | 2013-01-10 | 2014-07-16 | 神讯电脑(昆山)有限公司 | Manufacturing method for glass fibre product and portable electronic apparatus |
| CN107604673A (en) * | 2017-10-16 | 2018-01-19 | 高伟 | A kind of glass fibre infiltration swelling agent and preparation method |
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2020
- 2020-08-18 CN CN202010829253.5A patent/CN113321867B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008111602A1 (en) * | 2007-03-15 | 2008-09-18 | Nippon Electric Glass Co., Ltd. | Glass composition for glass fiber, glass fiber, process for producing glass fiber and composite material |
| CN103921388A (en) * | 2013-01-10 | 2014-07-16 | 神讯电脑(昆山)有限公司 | Manufacturing method for glass fibre product and portable electronic apparatus |
| CN103660071A (en) * | 2013-12-18 | 2014-03-26 | 上海日之升新技术发展有限公司 | Melt impregnation device for continuous long glass fiber reinforced polyester production as well as impregnation method |
| CN107604673A (en) * | 2017-10-16 | 2018-01-19 | 高伟 | A kind of glass fibre infiltration swelling agent and preparation method |
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