CN110184821B - Alumina fiber flexible modifier and preparation method thereof - Google Patents
Alumina fiber flexible modifier and preparation method thereof Download PDFInfo
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- CN110184821B CN110184821B CN201910365886.2A CN201910365886A CN110184821B CN 110184821 B CN110184821 B CN 110184821B CN 201910365886 A CN201910365886 A CN 201910365886A CN 110184821 B CN110184821 B CN 110184821B
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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
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
- D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
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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
- 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
- D06M15/55—Epoxy resins
-
- 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
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
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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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/50—Modified hand or grip properties; Softening compositions
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses an alumina fiber flexible modifier and a preparation method thereof, wherein the alumina fiber flexible modifier comprises the following components in parts by weight: 10-20 parts of main slurry, 1-3 parts of surfactant, 0.5-1 part of additive, 1-2 parts of finishing agent and 80-110 parts of deionized water. According to the invention, the flexible modifier is prepared and impregnated and coated on the surface of the alumina fiber, so that the brittle fiber obtains higher bending performance and breaking strength, the broken filaments and broken filaments of the fiber are reduced, and the production efficiency of the weaving process is improved.
Description
Technical Field
The invention relates to a flexible modifier, belongs to the technical field of textile sizing, and particularly relates to an alumina fiber flexible modifier and a preparation method thereof.
Background
Alumina fiber is an important polycrystalline ceramic fiber and is a brittle fiber material, and the main component of the alumina fiber is Al2O3And SiO2B can also be added according to the actual application requirements2O3、ZrO3And the like, and the micro-component has excellent characteristics of high strength, high modulus, high temperature chemical corrosion resistance, stable structure, small specific gravity and the like, can be applied to the preparation of high temperature heat-insulating materials, catalyst supports in high temperature reaction, refractory materials, resin, metal and ceramic matrix composite material reinforcements and other materials, and has wide development prospects in the fields of metallurgy, building materials, chemical industry, ships, aerospace and the like.
At present, the production technology of foreign alumina fibers tends to be mature, the research of the domestic alumina fibers is late, most alumina fibers have the problems of brittle quality, low flexibility and the like, the production process is single, and the equipment is relatively lagged behind. In recent years, researches show that the tensile strength of the alumina fiber is controlled by the number of cracks and defects in the fiber, and the fiber strength shows certain dispersity due to the random distribution of the cracks and the defects in the fiber, thereby having influence on practical application. However, few reports exist on the research on the modification treatment and weavability of the existing alumina fiber flexibilizer, and related research mainly focuses on high-performance fibers such as carbon fibers, silicon carbide fibers and the like, for example, patent 201510512327.1 "a silicon carbide fiber sizing agent and a preparation method thereof", patent 201510512327.1 "a carbon fiber sizing agent and a preparation method thereof", and patent 201510720194.7 "a gypsum fiber flexibilizer and a preparation method thereof" all adjust the formula of the sizing agent to flexibly modify the fibers, so that the composite material with good heat resistance, toughness and interface performance is obtained. Therefore, a proper preparation method is found, the defects of the existing production process are overcome, a proper alumina fiber flexible modifier is prepared, and the urgent need is to obtain the modified fiber with high strength, high modulus and excellent flexibility.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides an alumina fiber flexibility modifier and a preparation method thereof. The modified alumina fiber with high strength, high modulus and excellent flexibility can be obtained by modifying the alumina fiber by adopting the alumina fiber flexible modifier.
The technical scheme of the invention is as follows:
an alumina fiber flexibility modifier comprises the following components in parts by weight: 10-20 parts of main slurry, 1-3 parts of surfactant, 0.5-1 part of additive, 1-2 parts of finishing agent and 80-110 parts of deionized water.
The main slurry is water-based epoxy resin, and the water-based epoxy resin is one of bisphenol A type water-based epoxy resins E-10, E-15 and E-20.
The surfactant is a mixture of two nonionic surfactants, namely Tween and polyethylene glycol laurate, and the weight ratio of the Tween to the polyethylene glycol laurate is 4:1-1: 1.
The Tween is one of Tween-20, Tween-40 and Tween-80.
The additive is oligomeric silsesquioxane organic-inorganic nano hybrid particles, is synthesized by taking trisiloxysilane monomer RSiY3 as a raw material, methanol as a solvent and hydrochloric acid as a catalyst and adopting a direct hydrolytic condensation method of silane. Prepared by the method disclosed in the prior art, and the reference documents are as follows:
【1】 Liuxue Ying, Synthesis of polyhedral oligomeric silsesquioxanes (POSS) and POSS/polymers [ D ]. university of Anhui Physician, 2011.
【2】 Lacquer steel, Jiangyiping, bear Ting, cage Polysilsesquioxane (POSS) and application research in organosilicon materials [ J ] China building metal structure, 2018, No.436(04):61-62.
【3】 Forest, Chen super, Sun dispute, et al, research progress on polyhedral oligomeric silsesquioxane modified polymeric materials [ J ] organosilicon materials, 2009(3):194-198.
【4】 Li Wei, development and application of hydrophilic organosilicon softener [ D ]. Zhejiang university of science and technology, 2011.
The finishing agent is hydrophilic modified organic silicone oil.
A preparation method of an alumina fiber flexibility modifier comprises the following steps:
(1) stirring 0.5-1 part of additive and 1-2 parts of finishing agent by weight to uniformly disperse the substances in the mixture to form a mixture A;
(2) adding 10-20 parts by weight of main slurry into the mixture A, stirring at 60 ℃, and then carrying out ultrasonic oscillation to uniformly disperse substances in the mixture A to form a mixture B;
(3) adding 1-3 parts by weight of surfactant into the mixture B, and stirring at 60 ℃ to uniformly disperse the substances in the mixture B to form a mixture C; the surfactant is a mixture of two nonionic surfactants, namely Tween and polyethylene glycol laurate, and the weight ratio of the Tween to the polyethylene glycol laurate is 4:1-1: 1;
(4) slowly pouring 80-110 parts by weight of deionized water into the mixture C, controlling the temperature to be 40 ℃ in the pouring process, firstly stirring at 800r/min, and continuously stirring at 500r/min after the deionized water is completely poured until uniform and stable slurry is formed;
(5) and cooling the slurry to obtain the alumina fiber flexibility modifier.
As a preferred technical scheme, the stirring condition in the step (1) is that the stirring is carried out for 10min at the normal temperature and at the speed of 800 r/min; the conditions of stirring and ultrasonic oscillation in the step (2) are that stirring is firstly carried out at 60 ℃ and at 800r/min for 10min, and then ultrasonic oscillation is carried out at 60 ℃ for 20 min; the stirring condition in the step (3) is that the mixture is stirred for 20min at the temperature of 60 ℃ at the speed of 800 r/min; and (4) controlling the temperature to be 40 ℃ in the pouring process of the deionized water in the step (4), firstly stirring at 800r/min, and after the deionized water is completely poured, continuously stirring at 500r/min for 30min until uniform and stable slurry is formed.
The raw materials of the present invention can be obtained by market purchase, unless otherwise specified.
The normal temperature of the invention is 25 +/-5 ℃.
The invention has the beneficial effects that:
1. the main sizing agent in the invention adopts the water-based epoxy resin, which is beneficial to improving the surface caking property and the strength and the flexibility of the continuous fiber bundle;
2. the surfactant in the invention selects Tween and polyethylene glycol lauric acid, and the two nonionic surfactants are beneficial to forming stable emulsion and improving the wettability and permeability of the slurry;
3. the additive in the invention selects oligomeric silsesquioxane organic-inorganic nano hybrid particles, and the nano effect of the oligomeric silsesquioxane organic-inorganic nano hybrid particles endows the alumina fiber with good toughness and interface performance.
4. The finishing agent in the invention is hydrophilic modified organic silicone oil which is compatible with nonionic auxiliary agent, so that the fiber is endowed with better flexibility.
5. The alumina fiber flexible modifier disclosed by the invention is moderate in viscosity, good in wettability, energy-saving and environment-friendly.
Detailed Description
The present invention will be described in detail with reference to examples.
Example 1
An alumina fiber flexibility modifier is prepared by the following steps:
(1) stirring 0.5 part by weight of additive (oligomeric silsesquioxane organic-inorganic nano hybrid particles) and 2 parts by weight of finishing agent (hydrophilic modified silicone oil, Shanghai Jingming chemical Co., Ltd., SH-205) at normal temperature at 800r/min for 10min to uniformly disperse the internal substances to form a mixture A;
(2) adding 20 parts by weight of main slurry into the mixture A, selecting bisphenol A type waterborne epoxy resin E-10, firstly stirring at 60 ℃ at 800r/min for 10min, and then ultrasonically oscillating at 60 ℃ for 20min to uniformly disperse substances in the mixture A to form a mixture B;
(3) adding 1 part by weight of surfactant into the mixture B, wherein the weight ratio of two nonionic surfactants, namely Tween-80 and polyethylene glycol laurate is controlled to be 4:1, and stirring at 60 ℃ at 800r/min for 20min to uniformly disperse the internal substances to form a mixture C;
(4) slowly pouring 80 parts by weight of deionized water into the mixture C, controlling the temperature to be 40 ℃ in the pouring process, firstly stirring at 800r/min, and continuously stirring for 30min at 500r/min after the deionized water is completely poured into the mixture C until uniform and stable slurry is formed;
(5) and cooling the slurry to obtain the alumina fiber flexibility modifier.
Example 2
An alumina fiber flexibility modifier is prepared by the following steps:
(1) stirring 0.75 parts by weight of additive (oligomeric silsesquioxane organic-inorganic nano hybrid particles) and 1.5 parts by weight of finishing agent (hydrophilic modified silicone oil, Shanghai Jingming chemical Co., Ltd., SH-205) at normal temperature at 800r/min for 10min to uniformly disperse the internal substances to form a mixture A;
(2) adding 15 parts by weight of main slurry and bisphenol A type waterborne epoxy resin E-15 into the mixture A, firstly stirring at 60 ℃ for 10min at 800r/min, and then ultrasonically oscillating at 60 ℃ for 20min to uniformly disperse substances in the mixture A to form a mixture B;
(3) adding 2 parts by weight of surfactant into the mixture B, wherein the weight ratio of Tween-40 to polyethylene glycol laurate to nonionic surfactant is controlled to be 2.5:1, and stirring at 60 ℃ at 800r/min for 20min to uniformly disperse the internal substances to form a mixture C;
(4) slowly pouring 95 parts by weight of deionized water into the mixture C, controlling the temperature to be 40 ℃ in the pouring process, firstly stirring at 800r/min, and continuously stirring for 30min at 500r/min after the deionized water is completely poured into the mixture C until uniform and stable slurry is formed;
(5) and cooling the slurry to obtain the alumina fiber flexibility modifier.
Example 3
An alumina fiber flexibility modifier is prepared by the following steps:
(1) 1 part by weight of additive (oligomeric silsesquioxane organic-inorganic nano hybrid particles) and 1 part by weight of finishing agent (hydrophilic modified organic silicone oil, Shanghai Jingming chemical Co., Ltd., SH-205) are stirred at the normal temperature of 800r/min for 10min, so that the substances in the additive are uniformly dispersed to form a mixture A;
(2) adding 10 parts by weight of main slurry and bisphenol A type waterborne epoxy resin E-20 into the mixture A, firstly stirring at 60 ℃ for 10min at 800r/min, and then ultrasonically oscillating at 60 ℃ for 20min to uniformly disperse substances in the mixture A to form a mixture B;
(3) adding 3 parts by weight of surfactant into the mixture B, wherein the weight ratio of two nonionic surfactants, namely Tween-20 and polyethylene glycol laurate is controlled to be 1:1, and stirring at 60 ℃ at 800r/min for 20min to uniformly disperse the internal substances to form a mixture C;
(4) slowly pouring 110 parts by weight of deionized water into the mixture C, controlling the temperature to be 40 ℃ in the pouring process, firstly stirring at 800r/min, and continuously stirring for 30min at 500r/min after the deionized water is completely poured into the mixture C until uniform and stable slurry is formed;
(5) and cooling the slurry to obtain the alumina fiber flexibility modifier.
The alumina fiber flexible modifier prepared in the embodiment 1-3 is adopted to modify alumina fibers, and in the weaving process, the yarn breakage rate is less than or equal to 1.5%, and the strength retention rate is more than or equal to 95%.
Claims (5)
1. The alumina fiber flexibility modifier is characterized by comprising the following components in parts by weight: 10-20 parts of main slurry, 1-3 parts of surfactant, 0.5-1 part of additive, 1-2 parts of finishing agent and 80-110 parts of deionized water;
the main slurry is water-based epoxy resin;
the surfactant is a mixture of two nonionic surfactants, namely Tween and polyethylene glycol laurate, and the weight ratio of the Tween to the polyethylene glycol laurate is 4:1-1: 1;
the additive is oligomeric silsesquioxane organic-inorganic nano hybrid particles;
the finishing agent is hydrophilic modified organic silicone oil.
2. The alumina fiber flexibility modifier according to claim 1, wherein the waterborne epoxy resin is one of bisphenol a waterborne epoxy resins E-10, E-15 and E-20.
3. The alumina fiber flexibility modifier as claimed in claim 1, wherein the Tween is one of Tween-20, Tween-40 and Tween-80.
4. The preparation method of the alumina fiber flexibility modifier is characterized by comprising the following steps:
(1) stirring 0.5-1 part of additive and 1-2 parts of finishing agent by weight to uniformly disperse the substances in the mixture to form a mixture A;
(2) adding 10-20 parts by weight of main slurry into the mixture A, stirring at 60 ℃, and then carrying out ultrasonic oscillation to uniformly disperse substances in the mixture A to form a mixture B;
(3) adding 1-3 parts by weight of surfactant into the mixture B, and stirring at 60 ℃ to uniformly disperse the substances in the mixture B to form a mixture C;
(4) slowly pouring 80-110 parts by weight of deionized water into the mixture C, controlling the temperature to be 40 ℃ in the pouring process, firstly stirring at 800r/min, and continuously stirring at 500r/min after the deionized water is completely poured until uniform and stable slurry is formed;
(5) cooling the slurry to obtain the alumina fiber flexible modifier;
the main slurry is water-based epoxy resin;
the surfactant is a mixture of two nonionic surfactants, namely Tween and polyethylene glycol laurate, and the weight ratio of the Tween to the polyethylene glycol laurate is 4:1-1: 1;
the additive is oligomeric silsesquioxane organic-inorganic nano hybrid particles;
the finishing agent is hydrophilic modified organic silicone oil.
5. The method according to claim 4, wherein the stirring in step (1) is performed at a normal temperature at 800r/min for 10 min; the conditions of stirring and ultrasonic oscillation in the step (2) are that stirring is firstly carried out at 60 ℃ and at 800r/min for 10min, and then ultrasonic oscillation is carried out at 60 ℃ for 20 min; the stirring condition in the step (3) is that the mixture is stirred for 20min at the temperature of 60 ℃ at the speed of 800 r/min; and (4) controlling the temperature to be 40 ℃ in the pouring process of the deionized water in the step (4), firstly stirring at 800r/min, and after the deionized water is completely poured, continuously stirring at 500r/min for 30min until uniform and stable slurry is formed.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0427873A1 (en) * | 1989-06-08 | 1991-05-22 | Kanebo, Ltd. | Textile of long high-purity alumina fiber, long high-purity alumina fiber used for producing said textile, and method of producing them |
| CN106065528A (en) * | 2016-08-18 | 2016-11-02 | 江苏恒神股份有限公司 | A kind of aqueous epoxy emulsion type carbon fiber sizing agent and preparation method thereof |
| CN106884328A (en) * | 2017-03-24 | 2017-06-23 | 武汉龙图新材料科技有限公司 | A kind of alumina fibre sizing agent and preparation method thereof |
| CN106948176A (en) * | 2017-03-24 | 2017-07-14 | 武汉龙图新材料科技有限公司 | A kind of silicon nitride fiber sizing agent and preparation method thereof |
| CN107447522A (en) * | 2017-09-11 | 2017-12-08 | 哈尔滨工业大学 | A kind of preparation method of high-temperature-resistant epoxy resin emulsion type carbon fiber sizing agent |
-
2019
- 2019-05-05 CN CN201910365886.2A patent/CN110184821B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0427873A1 (en) * | 1989-06-08 | 1991-05-22 | Kanebo, Ltd. | Textile of long high-purity alumina fiber, long high-purity alumina fiber used for producing said textile, and method of producing them |
| CN106065528A (en) * | 2016-08-18 | 2016-11-02 | 江苏恒神股份有限公司 | A kind of aqueous epoxy emulsion type carbon fiber sizing agent and preparation method thereof |
| CN106884328A (en) * | 2017-03-24 | 2017-06-23 | 武汉龙图新材料科技有限公司 | A kind of alumina fibre sizing agent and preparation method thereof |
| CN106948176A (en) * | 2017-03-24 | 2017-07-14 | 武汉龙图新材料科技有限公司 | A kind of silicon nitride fiber sizing agent and preparation method thereof |
| CN107447522A (en) * | 2017-09-11 | 2017-12-08 | 哈尔滨工业大学 | A kind of preparation method of high-temperature-resistant epoxy resin emulsion type carbon fiber sizing agent |
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Address after: 214200 Fangqiao Street industrial concentration area, Yixing City, Wuxi City, Jiangsu Province Patentee after: YIXING XINLI WEAVING Co.,Ltd. Address before: 214212 Dajian village, Wanshi Town, Yixing City, Wuxi City, Jiangsu Province Patentee before: YIXING XINLI WEAVING Co.,Ltd. |