CN109133671A - A kind of high temperature resistant basalt fibre size and preparation method thereof - Google Patents
A kind of high temperature resistant basalt fibre size and preparation method thereof Download PDFInfo
- Publication number
- CN109133671A CN109133671A CN201811116390.3A CN201811116390A CN109133671A CN 109133671 A CN109133671 A CN 109133671A CN 201811116390 A CN201811116390 A CN 201811116390A CN 109133671 A CN109133671 A CN 109133671A
- Authority
- CN
- China
- Prior art keywords
- parts
- high temperature
- basalt fibre
- temperature resistant
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
- C03C25/24—Coatings containing organic materials
- C03C25/40—Organo-silicon compounds
Abstract
The invention discloses a kind of high temperature resistant basalt fibre sizes and preparation method thereof, the following steps are included: in a high pressure reaction kettle, after emulsifier is dissolved in deionized water, diethylene glycol (DEG), diethylene glycol ether, dicyclopentadiene phenol epoxy resin, caprolactam, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride and vinyltriethoxysilane are sequentially added in autoclave；After being stirred to react under the high temperature conditions, then reaction temperature turned down, be eventually adding water-soluble epoxy resin, continue to stir, obtains film forming agent emulsion；Obtained film forming agent is cooled to room temperature, coupling agent, plasticizer and lubricant is added and is mixed by weight, high temperature resistant basalt fibre size is made.Not only preparation method is simple, easily operated for size of the invention, but also high with the compatibility of basalt fibre；The basalt fibre being prepared by the size is for a long time in use, the high retention rate of basalt fiber performance can be realized under high temperature and acid condition.
Description
Technical field
The present invention relates to basalt fibre size fields, and in particular to a kind of high temperature resistant basalt fibre size and
Preparation method.
Background technique
Basalt fibre (CBF) was developed in 1953~1954 years by Soviet Union's Moscow glass and plastics research institute, was one
Kind novel inorganic environment-friendly and green high performance fibre material, has good stability, electrical insulating property, anticorrosive, flame resistant, high temperature resistant etc.
A variety of excellent properties.The research that China carries out CBF is later, developmental retardation, until in November, 2002 China is by " CBF and its composite wood
Material " approval be classified as National 863 plan (2002AA334110) since, CBF welcome oneself development golden age, become and possess
Most leading one of several countries of CBF production technology in the world.Currently, China CBF has been classified as that China gives priority to four
One of big fiber, has substantially carried out industrialized production in China.
In basalt fibre production, size is a vital core technology, greatly influences the production of fiber
The physical and chemical performance of quality, fiber compatible with resin matrix wellability and composite material.As China's basalt fibre produces
Rapid growth is measured, China's size technology is also rapidly developing, however compared with international advanced enterprises, China's size researches and develops water
Low-level difficult situation in being still within is put down, and then constrains the development and application of China's basalt fibre.
Summary of the invention
That the purpose of the present invention is to provide this one kind is cheap, prepare simple, acid corrosion-resistant, can be in high temperature environment
High temperature resistant basalt fibre size used and preparation method thereof.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of high temperature resistant basalt fibre size and preparation method thereof, which is characterized in that its component and its component contain
Amount are as follows: 100 parts of agent emulsion, 0.5~2.5 part of coupling agent, 0.3~1.6 part of plasticizer, 0.1~0.7 part of lubricant of film forming.
Wherein, its component and its constituent content of the film forming agent emulsion are as follows: the water-soluble epoxy resin that the trade mark is 681
5~10 parts；20~30 parts of dicyclopentadiene phenol epoxy resin；11~18 parts of vinyltriethoxysilane；Caprolactam 2~
11 parts；2.3~3.0 parts of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride；10~24 parts of diethylene glycol (DEG)；2~8 parts of diethylene glycol ether；
0.8-2.5 parts of emulsifier；45~65 parts of deionized water.
The coupling agent is three (beta-methoxy of vinyltriethoxysilane, vinyltrimethoxysilane or vinyl
Ethyoxyl) silane.
The plasticizer is (2- ethyl hexyl) ester of phthalic acid two or diisononyl phthalate.
The lubricant is the polyene hydrocarbon lubricants that the trade mark is YZS-03D, originates from Guangzhou paulownia up to the limited public affairs of chemical engineering
Department.
The emulsifier is ethoxylated dodecyl alcohol, Dodecyl Polyoxyethylene Ether sodium sulphate, octadecanol polyoxy second
One of alkene ether, -7 ester of stearic acid polyoxyethylene or more than one.
A kind of high temperature resistant basalt fibre size and preparation method thereof, which is characterized in that include following steps:
(1) under the conditions of 75~90 DEG C and in nitrogen or argon atmosphere, by 45~65 parts of deionized water and emulsifier 0.8-
In 2.5 parts of addition autoclaves, it is sufficiently stirred after dissolving emulsifier, by 10~24 parts of diethylene glycol (DEG), diethylene glycol ether 2~8
Part, 20~30 parts of dicyclopentadiene phenol epoxy resin, 2~11 parts of caprolactam, methylacryoyloxyethyl trimethyl ammonia chloride
2.3~3.0 parts and 11~18 parts of vinyltriethoxysilane of ammonium sequentially add in autoclave；
(2) reaction condition of step 1) is warming up to 105~115 DEG C, after being stirred to react 1~4 hour, then by reaction temperature
75~87 DEG C are adjusted to, the water-soluble epoxy resin that the trade mark is 681 is eventually adding, continues stirring 1~2 hour, obtains film forming agent cream
Liquid；
(3) film forming agent that step (2) obtains is cooled to room temperature, it then will film forming agent emulsion, coupling agent, plasticizer and profit
Lubrication prescription is mixed in proportion, and high temperature resistant basalt fibre size, constituent content is made are as follows: 100 parts of agent emulsion of film forming,
0.5~2.5 part of coupling agent, 0.3~1.6 part of plasticizer, 0.1~0.7 part of lubricant.
Beneficial effects of the present invention: size preparation method of the invention is simple, easily operated；The size and basalt
The compatibility of fiber is high；The basalt fibre being prepared by the size for a long time under high temperature and acid condition in use,
The high retention rate of basalt fiber performance can be achieved.
Specific embodiment
Below in conjunction with specific embodiment, the present invention will be further described, and following embodiments are only preferable realities of the invention
Example is applied, is not intended to limit the present invention in any form.
Embodiment 1
1, under the conditions of 90 DEG C and in argon atmosphere, by 65 kilograms of deionized water and Dodecyl Polyoxyethylene Ether sodium sulphate
In 0.8 kilogram of addition autoclave, it is sufficiently stirred after dissolving Dodecyl Polyoxyethylene Ether sodium sulphate, by diethylene glycol (DEG) 10,000
Gram, 2 kilograms of diethylene glycol ether, 30 kilograms of dicyclopentadiene phenol epoxy resin, 2 kilograms of caprolactam, methacryloxypropyl second
2.3 kilograms and 11 kilograms of vinyltriethoxysilane of base trimethyl ammonium chloride sequentially add in autoclave；
2, the reaction condition of step 1) is warming up to 105 DEG C, after being stirred to react 4 hours, then reaction temperature is adjusted to 75 DEG C,
10 kilograms of water-soluble epoxy resin that the trade mark is 681 are eventually adding, stirring 2 hours is continued, obtain film forming agent emulsion；
3, the film forming agent that step (2) obtains is cooled to room temperature, then will form a film agent emulsion double centner, three second of vinyl
The polyene hydrocarbon lubricants that 0.5 kilogram of oxysilane, 1.6 kilograms of phthalic acid two (2- ethyl hexyl) ester and the trade mark are YZS-03D
0.4 kilogram is mixed, and high temperature resistant basalt fibre size is made.
Embodiment 2
1, under the conditions of 75 DEG C and in nitrogen atmosphere, 55 parts and 1.2 kilograms of ethoxylated dodecyl alcohol of deionized water are added
Enter in autoclave, is sufficiently stirred after dissolving ethoxylated dodecyl alcohol, by 20 kilograms of diethylene glycol (DEG), diethylene glycol ether 5,000
Gram, 25 kilograms of dicyclopentadiene phenol epoxy resin, 9 kilograms of caprolactam, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride 2.6
Kilogram and 16 kilograms of vinyltriethoxysilane sequentially add in autoclave；
(2) reaction condition of step 1) is warming up to 115 DEG C, after being stirred to react 1 hour, then reaction temperature is adjusted to 85
DEG C, 7 kilograms of water-soluble epoxy resin that the trade mark is 681 are eventually adding, stirring 1 hour is continued, obtain film forming agent emulsion；
(3) film forming agent that step (2) obtains is cooled to room temperature, then will form a film agent emulsion double centner, vinyl front three
1.5 kilograms of oxysilane, 0.8 kilogram of diisononyl phthalate and the trade mark are the polyene hydrocarbon lubricants 0.4 thousand of YZS-03D
Gram.
Embodiment 3
1, under the conditions of 80 DEG C and in nitrogen atmosphere, by 60 parts of deionized water and emulsifier (- 7 ester of stearic acid polyoxyethylene
Mixed with Dodecyl Polyoxyethylene Ether sodium sulphate by the weight ratio of 7:3) 1.5 parts be added in autoclave, being sufficiently stirred makes cream
After agent dissolution, by 19 kilograms of diethylene glycol (DEG), 6 kilograms of diethylene glycol ether, 25 kilograms of dicyclopentadiene phenol epoxy resin, acyl in oneself
7 kilograms of amine, 2.3 kilograms of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride and 14 kilograms of vinyltriethoxysilane sequentially add
In autoclave；
(2) reaction condition of step 1) is warming up to 110 DEG C, after being stirred to react 1 hour, then reaction temperature is adjusted to 80
DEG C, 6 kilograms of water-soluble epoxy resin that the trade mark is 681 are eventually adding, stirring 1 hour is continued, obtain film forming agent emulsion；
(3) film forming agent that step (2) obtains is cooled to room temperature, then will form a film agent emulsion, (the beta-methoxy second of vinyl three
Oxygroup) 2.0 kilograms of silane, 1.0 kilograms of diisononyl phthalate and the trade mark be YZS-03D polyene hydrocarbon lubricants 0.6 thousand
It gram is mixed, high temperature resistant basalt fibre size is made.
It is respectively used to above-described embodiment 1-3 and preparation-obtained size to infiltrate basalt fibre of the same race, will obtain
Basalt fibre be tested for the property experiment, record experimental result, record data are as follows:
To above-mentioned analysis of experimental data it is found that obtaining size to the Black Warrior using technical solution of the present invention in embodiment 1-3
Rock fiber carries out infiltration processing, and obtained basalt fibre tensile strength is good, and after 80 DEG C of 3% sulfuric acid solution 30 days impregnate
Tensile strength performance retention rate it is high, up to 91% or more.
Claims (10)
1. a kind of high temperature resistant basalt fibre size and preparation method thereof, which is characterized in that by weight, including it is following
Component: 100 parts of agent emulsion, 0.5~2.5 part of coupling agent, 0.3~1.6 part of plasticizer, 0.1~0.7 part of lubricant of film forming.
Wherein, the film forming agent emulsion, by weight, including following components: the water-soluble epoxy resin 5 that the trade mark is 681
~10 parts；20~30 parts of dicyclopentadiene phenol epoxy resin；11~18 parts of vinyltriethoxysilane；Caprolactam 2~
11 parts；2.3~3.0 parts of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride；10~24 parts of diethylene glycol (DEG)；2~8 parts of diethylene glycol ether；
0.8-2.5 parts of emulsifier；45~65 parts of deionized water.The film forming agent emulsion synthesis method are as follows: 1) in 75~90 DEG C of conditions
In lower and nitrogen or argon atmosphere, deionized water and emulsifier are added in autoclave, being sufficiently stirred dissolves emulsifier
Afterwards, by diethylene glycol (DEG), diethylene glycol ether, dicyclopentadiene phenol epoxy resin, caprolactam, methylacryoyloxyethyl trimethyl
Ammonium chloride and vinyltriethoxysilane sequentially add in autoclave；2) reaction condition of step 1) is warming up to 105
~115 DEG C, after being stirred to react 1~4 hour, then reaction temperature is adjusted to 75~85 DEG C, is eventually adding the water solubility that the trade mark is 681
Epoxy resin continues stirring 1~2 hour, obtains film forming agent emulsion.
2. a kind of high temperature resistant basalt fibre size according to claim 1 and preparation method thereof, which is characterized in that
The coupling agent is vinyltriethoxysilane, vinyltrimethoxysilane or vinyl three (beta-methoxy ethyoxyl) silicon
Alkane.
3. a kind of high temperature resistant basalt fibre size according to claim 1 and preparation method thereof, which is characterized in that
The plasticizer is (2- ethyl hexyl) ester of phthalic acid two or diisononyl phthalate.
4. a kind of high temperature resistant basalt fibre size according to claim 1 and preparation method thereof, which is characterized in that
The lubricant is the polyene hydrocarbon lubricants that the trade mark is YZS-03D, originates from Guangzhou paulownia up to chemical engineering Co., Ltd.
5. a kind of high temperature resistant basalt fibre size according to claim 1 and preparation method thereof, which is characterized in that
The emulsifier is ethoxylated dodecyl alcohol, Dodecyl Polyoxyethylene Ether sodium sulphate, octadecanol polyoxyethylene ether, tristearin
One of sour -7 ester of polyoxyethylene or more than one.
6. described in any item a kind of high temperature resistant basalt fibre sizes of claim 1-5 and preparation method thereof, including with
Lower step:
(1) under the conditions of 75~90 DEG C and in nitrogen or argon atmosphere, by 45~65 parts and emulsifier 0.8-2.5 parts of deionized water
It is added in autoclave, is sufficiently stirred after dissolving emulsifier, by 10~24 parts of diethylene glycol (DEG), 2~8 parts of diethylene glycol ether, double
20~30 parts of cyclopentadiene phenol epoxy resin, 2~11 parts of caprolactam, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride 2.3
~3.0 parts and 11~18 parts of vinyltriethoxysilane sequentially add in autoclave；
(2) reaction condition of step 1) is warming up to 105~115 DEG C, after being stirred to react 1~4 hour, then reaction temperature is adjusted to
75~87 DEG C, it is eventually adding the water-soluble epoxy resin that the trade mark is 681, continues stirring 1~2 hour, obtains film forming agent emulsion；
(3) film forming agent that step (2) obtains is cooled to room temperature, it then will film forming agent emulsion, coupling agent, plasticizer and lubricant
It is mixed in proportion, high temperature resistant basalt fibre size, constituent content is made are as follows: 100 parts of agent emulsion of film forming, coupling
0.5~2.5 part of agent, 0.3~1.6 part of plasticizer, 0.1~0.7 part of lubricant.
7. a kind of high temperature resistant basalt fibre size according to claim 6 and preparation method thereof, which is characterized in that
The coupling agent is vinyltriethoxysilane, vinyltrimethoxysilane or vinyl three (beta-methoxy ethyoxyl) silicon
Alkane.
8. a kind of high temperature resistant basalt fibre size according to claim 1 and preparation method thereof, which is characterized in that
The plasticizer is (2- ethyl hexyl) ester of phthalic acid two or diisononyl phthalate.
9. a kind of high temperature resistant basalt fibre size according to claim 6 and preparation method thereof, which is characterized in that
The lubricant is the polyene hydrocarbon lubricants that the trade mark is YZS-03D, originates from Guangzhou paulownia up to chemical engineering Co., Ltd.
10. a kind of high temperature resistant basalt fibre size according to claim 6 and preparation method thereof, feature exists
In, the emulsifier be ethoxylated dodecyl alcohol, Dodecyl Polyoxyethylene Ether sodium sulphate, octadecanol polyoxyethylene ether,
One of -7 ester of stearic acid polyoxyethylene or more than one.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811116390.3A CN109133671B (en) | 2018-09-25 | 2018-09-25 | Medium-high temperature resistant basalt fiber impregnating compound and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811116390.3A CN109133671B (en) | 2018-09-25 | 2018-09-25 | Medium-high temperature resistant basalt fiber impregnating compound and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109133671A true CN109133671A (en) | 2019-01-04 |
| CN109133671B CN109133671B (en) | 2021-03-30 |
Family
ID=64823706
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811116390.3A Active CN109133671B (en) | 2018-09-25 | 2018-09-25 | Medium-high temperature resistant basalt fiber impregnating compound and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109133671B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110790518A (en) * | 2019-09-06 | 2020-02-14 | 贵州玄武岩新材料工程技术开发有限公司 | Basalt fiber surface treating agent |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3803069A (en) * | 1968-05-03 | 1974-04-09 | Ppg Industries Inc | Glass fiber size of curable,blocked polyurethane emulsion with amino silane |
| CN102745908A (en) * | 2012-08-06 | 2012-10-24 | 四川省玻纤集团有限公司 | Reinforcing yarn size for glass fibers and preparation method thereof |
| CN103466964A (en) * | 2013-09-10 | 2013-12-25 | 西安友基复合材料有限公司 | Preparation method of wetting agent for E glass fishing rod gauze |
| CN104944804A (en) * | 2015-06-30 | 2015-09-30 | 四川航天五源复合材料有限公司 | Wetting agent for basalt fibers |
-
2018
- 2018-09-25 CN CN201811116390.3A patent/CN109133671B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3803069A (en) * | 1968-05-03 | 1974-04-09 | Ppg Industries Inc | Glass fiber size of curable,blocked polyurethane emulsion with amino silane |
| CN102745908A (en) * | 2012-08-06 | 2012-10-24 | 四川省玻纤集团有限公司 | Reinforcing yarn size for glass fibers and preparation method thereof |
| CN103466964A (en) * | 2013-09-10 | 2013-12-25 | 西安友基复合材料有限公司 | Preparation method of wetting agent for E glass fishing rod gauze |
| CN104944804A (en) * | 2015-06-30 | 2015-09-30 | 四川航天五源复合材料有限公司 | Wetting agent for basalt fibers |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110790518A (en) * | 2019-09-06 | 2020-02-14 | 贵州玄武岩新材料工程技术开发有限公司 | Basalt fiber surface treating agent |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109133671B (en) | 2021-03-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102702874B (en) | A kind of anticorrosive paint | |
| CN105645823A (en) | Low-addition-amount environment-friendly alkali-free chlorine liquid accelerator and preparation method thereof | |
| CN111439985B (en) | Inorganic interior wall coating and preparation method thereof | |
| WO2016110038A1 (en) | Guanidine gum fracturing fluid system | |
| CN103450767A (en) | Super-weather-resistant anti-fouling real stone paint | |
| CN103740177A (en) | Development of super weather-proof marble coating rock slice paint | |
| CN109133671A (en) | A kind of high temperature resistant basalt fibre size and preparation method thereof | |
| CN113698124B (en) | Alkali-free liquid accelerator and preparation method thereof | |
| CN112358864B (en) | Nano emulsion acid system and preparation method and application thereof | |
| CN107880225A (en) | A kind of sustained-release polycarboxylic water reducer and preparation method thereof | |
| CN109943316A (en) | A kind of alkaline-resisting overlay film proppant suitable for ternary composite driving | |
| WO2021109731A1 (en) | Self-emulsifying epoxy resin emulsion, preparation method therefor and application thereof | |
| CN106398469A (en) | Microcapsule, self-healing electrophoretic coating containing microcapsule and preparation method of microcapsule | |
| CN117343703A (en) | Branched epoxy resin pressure-bearing plugging material and oil-based drilling fluid | |
| WO2019006940A1 (en) | Artificial compound staining agent for textiles and preparation method therefor | |
| CN106010813A (en) | Oil sludge cleaning agent for fracturing flow-back fluid and preparation method of oil sludge cleaning agent | |
| CN106893569A (en) | A kind of pit shaft de-plugging agent for repairing gas well reservoir permeability | |
| CN110577776A (en) | Desert sand stone-like paint and preparation method thereof | |
| CN108276624A (en) | A kind of preparation that graphene adulterates anti-impact modifier and the application in PVC matrix | |
| CN104530758A (en) | Heterocyclic disperse dye and preparation method thereof | |
| CN108949079A (en) | A kind of water-resistant type Artificial Plate Adhesive | |
| CN104141231B (en) | A kind of fabric coating slurry and preparation method thereof | |
| CN111732946B (en) | Anti-swelling cleanup additive for fracturing and preparation method thereof | |
| CN113731297A (en) | Amido sulfonate gemini surfactant as well as preparation method and application thereof | |
| CN113307572A (en) | Anti-weathering plastering mortar and preparation process thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |