CN110184821A - A kind of alumina fibre flexible modifying agent and preparation method thereof - Google Patents
A kind of alumina fibre flexible modifying agent and preparation method thereof Download PDFInfo
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- CN110184821A CN110184821A CN201910365886.2A CN201910365886A CN110184821A CN 110184821 A CN110184821 A CN 110184821A CN 201910365886 A CN201910365886 A CN 201910365886A CN 110184821 A CN110184821 A CN 110184821A
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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
-
- 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
-
- 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
-
- 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 a kind of alumina fibre flexible modifying agent and preparation method thereof, which includes: 10-20 parts of main slurry, 1-3 parts of surfactant, 0.5-1 parts of additive, 1-2 parts of finishing agent, 80-110 parts of deionized water by weight.The present invention is coated in alumina fibre surface by allotment flexible modifying agent, dipping, so that fragile fibre obtains higher bending property and ultimate strength, reduces fiber fracture of wire and lousiness, improves braiding process production efficiency.
Description
Technical field
The present invention relates to a kind of flexible modifying agents, belong to textile sizing technical field, fine more particularly, to a kind of aluminium oxide
Tie up flexible modifying agent and preparation method thereof.
Background technique
Alumina fibre is a kind of important polycrystalline ceramic fiber, is a kind of fragile fibre material, main component is
Al2O3And SiO2, also B can be added according to practical application request2O3、ZrO3Etc. micro constitutents, since it has high-strength and high-modulus, resistance to height
The good characteristics such as warm chemical attack, stable structure, specific gravity be small can be applied to high temperature thermal insulation material, the catalyst in pyroreaction
The preparation of the materials such as carrier, refractory material and resin, metal and ceramic matric composite reinforcement, in metallurgy, building materials, change
The multiple fields such as work, ship, aerospace have broad based growth prospect.
Foreign countries' alumina fibre production technology tends to be mature at present, and domestic alumina fibre research is started late, most of
The problems such as that there are matter is crisp for alumina fibre, flexible performance is low, production technology is more single, and equipment also falls behind relatively.Research in recent years
It was found that the tensile strength of alumina fibre is controlled by crackle and defects count in fiber, due to intrastitial crackle and defect
Certain dispersibility is presented in random distribution, fibre strength, will also result in influence to application in practice.And it is directed to existing aluminium oxide
The rare report of research in terms of fiber flexibility agent modification and its weavability, correlative study are concentrated mainly on carbon fiber, carbonization
The high performance fibers such as silica fibre, such as patent 201510512327.1 " a kind of silicon carbide fibre sizing agent and preparation method thereof ",
Patent 201510512327.1 " a kind of carbon fiber sizing agent and preparation method thereof " and a kind of " stone of patent 201510720194.7
Cream fiber flexibility modifying agent and preparation method thereof ", by adjusting formula of size, flexibility is carried out to fiber and is modified, is obtained compound
The good heat resistance of material, toughness and interface performance.Therefore suitable preparation method is found, overcomes existing production technology defect,
The suitable alumina fibre flexible modifying agent of preparation, obtaining the excellent modified fibre of high-strength and high-modulus, flexibility is urgent need.
Summary of the invention
For technical problem of the existing technology, the present invention provides a kind of alumina fibre flexible modifying agent and its systems
Preparation Method.Being modified processing to alumina fibre using alumina fibre flexible modifying agent of the invention can get high-strength height
The excellent modified oxidized aluminum fiber of mould, flexibility.
Technical scheme is as follows:
A kind of alumina fibre flexible modifying agent includes: 10-20 parts of main slurry by weight, surfactant 1-3
Part, 0.5-1 parts of additive, 1-2 parts of finishing agent, 80-110 parts of deionized water.
The main slurry is aqueous epoxy resins, and the aqueous epoxy resins are bisphenol A-type aqueous epoxy resins E-
10, one of E-15, E-20.
The surfactant is the mixture of two kinds of nonionic agents of Tween and polyethylene glycol laurate,
The weight ratio of the Tween and polyethylene glycol laurate is 4:1-1:1.
The Tween is one of Tween-20, Tween-40, Tween-80.
The additive is oligomeric silsesquioxane organic-inorganic nano hybrid particle, with three Siloxysilane monomers
RSiY3 is raw material, methanol is solvent, hydrochloric acid is catalyst, is synthesized using silane direct hydrolysis method of condensing.Using the prior art
In the method preparation that has disclosed, bibliography is as follows:
[1] Anhui study on the synthesis [D] the science and engineering of Liu Xueying cage-type silsesquioxane (POSS) and POSS/ polymer is big
It learns, 2011.
[2] Qi Gang, Jiang Huiping, Xiong Ting cage modle polysilsesquioxane (POSS) and the application study in organosilicon material
[J] Chinese architecture metal structure, 2018, No.436 (04): 61-62.
[3] Lin Qian, Chen Chao, Sun Zhengguang, et al. polyhedral oligomeric silsesquioxane modified polymer material progress
[J] organosilicon material, 2009 (3): 194-198.
[4] development of Li Wei Hydrophilic Silicone Micro Emulsion and application [D] Institutes Of Technology Of Zhejiang, 2011.
The finishing agent is hydrophilically modified organic silicone oil.
A kind of preparation method of alumina fibre flexible modifying agent, includes the following steps:
(1) by 0.5-1 parts by weight additive and 1-2 parts by weight finishing agent, stirring makes its inner material be uniformly dispersed, and is formed
Mixture A；
(2) 10-20 parts by weight main slurry is added in the mixture A, first sonic oscillation makes it after 60 DEG C of stirrings
Inner material is uniformly dispersed, and forms mixture B；
(3) 1-3 parts surfactant is added in the mixture B, makes its inner material point in 60 DEG C of stirrings
It dissipates uniformly, forms mixture C；The surfactant is two kinds of non-ionic activities of Tween and polyethylene glycol laurate
The weight ratio of the mixture of agent, the Tween and polyethylene glycol laurate is 4:1-1:1；
(4) 80-110 parts by weight of deionized water is poured slowly into the mixture C, during pouring into controlled at
It 40 DEG C, is first stirred with 800r/min, stirring is continued until being formed uniform and stable with 500r/min after deionized water is poured into completely
Slurries；
(5) cooling to slurries, obtain alumina fibre flexible modifying agent.
As a kind of optimal technical scheme, the condition of stirring described in step (1) is to be stirred under room temperature with 800r/min
10min；The condition of stirring described in step (2) and sonic oscillation is first to stir 10min at 60 DEG C with 800r/min, then 60
DEG C sonic oscillation 20min；The condition of stirring described in step (3) is to stir 20min at 60 DEG C with 800r/min；In step (4)
Controlled at 40 DEG C during the pouring into of deionized water, first stirred with 800r/min, after deionized water is poured into completely with
500r/min continues to stir 30min until forming uniform and stable slurries.
Raw material according to the present invention unless otherwise indicated, can be bought by market and be obtained.
Room temperature of the present invention is 25 ± 5 DEG C.
The invention has the benefit that
1, the main slurry in the present invention selects aqueous epoxy resins to be conducive to improve surface adhesiveness, improves continuous tow
Intensity and flexibility；
2, the surfactant in the present invention selects Tween and polyethylene glycol lauric acid, two kinds of non-ionic surfactants
Agent advantageously forms stable emulsion, improves slurry wellability and permeability；
3, the additive in the present invention selects oligomeric silsesquioxane organic-inorganic nano hybrid particle, nano effect
Assign the good toughness of alumina fibre and interface performance.
4, the finishing agent in the present invention selects hydrophilically modified organic silicone oil, with non-ionic additive compatibility, assigns fiber
It is preferably flexible.
5, the alumina fibre flexible modifying agent in the present invention, modest viscosity, wellability be good and energy conservation and environmental protection.
Specific embodiment
Below with reference to embodiment, the present invention is specifically described.
Embodiment 1
A kind of alumina fibre flexible modifying agent, is prepared using following steps:
(1) 0.5 parts by weight additive (oligomeric silsesquioxane organic-inorganic nano hybrid particle) and 2 parts by weight is whole
It manages agent (hydrophilically modified organic silicone oil, Shanghai Jing Ming Chemical Co., Ltd., SH-205), is stirred under room temperature with 800r/min
10min makes its inner material be uniformly dispersed, and forms mixture A；
(2) 20 parts by weight main slurries are added in said mixture A, selects bisphenol A-type aqueous epoxy resins E-10, first exists
60 DEG C are stirred 10min with 800r/min, and then 60 DEG C of sonic oscillation 20min, make its inner material be uniformly dispersed, and form mixture
B；
(3) 1 parts surfactant is added in said mixture B, wherein control Tween-80 and the polyethylene glycol moon
Two kinds of nonionic agent weight ratios of cinnamic acid ester are 4:1, stir 20min at 60 DEG C with 800r/min, make its inner material point
It dissipates uniformly, forms mixture C；
(4) it is added in said mixture C and is poured slowly into 80 parts by weight of deionized water, controlled at 40 during pouring into
DEG C, it is first stirred with 800r/min, continues to stir 30min until being formed uniformly steady with 500r/min after deionized water is poured into completely
Fixed slurries；
(5) cooling to slurries, obtain alumina fibre flexible modifying agent.
Embodiment 2
A kind of alumina fibre flexible modifying agent, is prepared using following steps:
(1) by 0.75 parts by weight additive (oligomeric silsesquioxane organic-inorganic nano hybrid particle) and 1.5 parts by weight
Finishing agent (hydrophilically modified organic silicone oil, Shanghai Jing Ming Chemical Co., Ltd., SH-205) is stirred with 800r/min under room temperature
10min makes its inner material be uniformly dispersed, and forms mixture A；
(2) 15 parts by weight main slurries, bisphenol A-type aqueous epoxy resins E-15, first at 60 DEG C are added in said mixture A
10min is stirred with 800r/min, then 60 DEG C of sonic oscillation 20min, make its inner material be uniformly dispersed, and form mixture B；
(3) 2 parts surfactants are added in said mixture B, wherein control Tween-40 and the polyethylene glycol moon
Two kinds of nonionic agent weight ratios of cinnamic acid ester are 2.5:1, stir 20min at 60 DEG C with 800r/min, make its inner material
It is uniformly dispersed, forms mixture C；
(4) it is added in said mixture C and is poured slowly into 95 parts by weight of deionized water, controlled at 40 during pouring into
DEG C, it is first stirred with 800r/min, continues to stir 30min until being formed uniformly steady with 500r/min after deionized water is poured into completely
Fixed slurries；
(5) cooling to slurries, obtain alumina fibre flexible modifying agent.
Embodiment 3
A kind of alumina fibre flexible modifying agent, is prepared using following steps:
(1) 1 parts by weight additive (oligomeric silsesquioxane organic-inorganic nano hybrid particle) and 1 parts by weight are arranged
Agent (hydrophilically modified organic silicone oil, Shanghai Jing Ming Chemical Co., Ltd., SH-205) stirs 10min with 800r/min under room temperature,
So that its inner material is uniformly dispersed, forms mixture A；
(2) 10 parts by weight main slurries, bisphenol A-type aqueous epoxy resins E-20, first at 60 DEG C are added in said mixture A
10min is stirred with 800r/min, then 60 DEG C of sonic oscillation 20min, make its inner material be uniformly dispersed, and form mixture B；
(3) 3 parts surfactants are added in said mixture B, wherein control Tween-20 and the polyethylene glycol moon
Two kinds of nonionic agent weight ratios of cinnamic acid ester are 1:1, stir 20min at 60 DEG C with 800r/min, make its inner material point
It dissipates uniformly, forms mixture C；
(4) in said mixture C be added be poured slowly into 110 parts by weight of deionized water, during pouring into controlled at
It 40 DEG C, is first stirred with 800r/min, continues to stir 30min until being formed uniform with 500r/min after deionized water is poured into completely
Stable slurries；
(5) cooling to slurries, obtain alumina fibre flexible modifying agent.
Processing is modified to alumina fibre using alumina fibre flexible modifying agent prepared by Examples 1 to 3, is being knitted
During making, yarn breakage≤1.5%, strength retention ratio >=95%.
Claims (8)
1. a kind of alumina fibre flexible modifying agent, which is characterized in that by weight include: 10-20 parts of main slurry, surface is living
1-3 parts of agent, 0.5-1 parts of additive, 1-2 parts of finishing agent, 80-110 parts of deionized water of property.
2. alumina fibre flexible modifying agent according to claim 1, which is characterized in that the main slurry is aqueous ring
Oxygen resin, the aqueous epoxy resins are one of bisphenol A-type aqueous epoxy resins E-10, E-15, E-20.
3. alumina fibre flexible modifying agent according to claim 1, which is characterized in that the surfactant is
The mixture of two kinds of nonionic agents of Tween and polyethylene glycol laurate, the Tween and polyethylene glycol laurate
Weight ratio be 4:1-1:1.
4. alumina fibre flexible modifying agent according to claim 3, which is characterized in that the Tween is Tween-
20, one of Tween-40, Tween-80.
5. alumina fibre flexible modifying agent according to claim 1, which is characterized in that the additive is oligomeric times
Half siloxanes organic-inorganic nano hybrid particle.
6. alumina fibre flexible modifying agent according to claim 1, which is characterized in that the finishing agent is hydrophily
Modification organic silicon oil.
7. a kind of preparation method of alumina fibre flexible modifying agent, which comprises the steps of:
(1) by 0.5-1 parts by weight additive and 1-2 parts by weight finishing agent, stirring makes its inner material be uniformly dispersed, and forms mixing
Object A；
(2) 10-20 parts by weight main slurry is added in the mixture A, first sonic oscillation makes inside it after 60 DEG C of stirrings
Substance is uniformly dispersed, and forms mixture B；
(3) 1-3 parts surfactant is added in the mixture B, keeps the dispersion of its inner material equal in 60 DEG C of stirrings
It is even, form mixture C；
(4) 80-110 parts by weight of deionized water is poured slowly into the mixture C, controlled at 40 during pouring into
DEG C, it is first stirred with 800r/min, stirring is continued until being formed uniform and stable with 500r/min after deionized water is poured into completely
Slurries；
(5) cooling to slurries, obtain alumina fibre flexible modifying agent.
8. preparation method according to claim 7, which is characterized in that the condition of stirring described in step (1) is under room temperature
10min is stirred with 800r/min；The condition of stirring described in step (2) and sonic oscillation is first to be stirred at 60 DEG C with 800r/min
10min is mixed, then 60 DEG C of sonic oscillation 20min；The condition of stirring described in step (3) is to be stirred at 60 DEG C with 800r/min
20min；Controlled at 40 DEG C during the pouring into of deionized water in step (4), first stirred with 800r/min, to deionized water
Continue to stir 30min until forming uniform and stable slurries with 500r/min after pouring into completely.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910365886.2A CN110184821B (en) | 2019-05-05 | 2019-05-05 | Alumina fiber flexible modifier and preparation method thereof |
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| CN201910365886.2A CN110184821B (en) | 2019-05-05 | 2019-05-05 | Alumina fiber flexible modifier and preparation method thereof |
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| CN110184821A true CN110184821A (en) | 2019-08-30 |
| CN110184821B CN110184821B (en) | 2022-02-11 |
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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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