CN107385915A - A kind of polyformaldehyde material enhancing basalt fibre sizing agent special and preparation method thereof - Google Patents
A kind of polyformaldehyde material enhancing basalt fibre sizing agent special and preparation method thereof Download PDFInfo
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- CN107385915A CN107385915A CN201611082866.7A CN201611082866A CN107385915A CN 107385915 A CN107385915 A CN 107385915A CN 201611082866 A CN201611082866 A CN 201611082866A CN 107385915 A CN107385915 A CN 107385915A
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- 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
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- D06M11/51—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 sulfur, selenium, tellurium, polonium or compounds thereof
- D06M11/54—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 sulfur, selenium, tellurium, polonium or compounds thereof with sulfur dioxide; with sulfurous acid or its salts
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Abstract
The invention discloses a kind of polyformaldehyde material enhancing basalt fibre sizing agent special and preparation method thereof, size of the present invention, including following parts by weight of component：40 60 parts of film forming agent, 5 15 parts of coupling agent, 15 parts of lubricants, 10 20 parts of modifying agent, 30 50 parts of solvent；The modifying agent includes the hypophosphites and acid that mass ratio is 58 ︰ 13；Fiber surface is modified while infiltration by modifying agent, increase fiber surface roughness and be grafted a large amount of active groups, so as to improve chemical bonding and the mechanical riveted ability between basalt fibre and polyformaldehyde material, the compatibility of basalt fibre and polyformaldehyde material is improved, promotes popularization and application of the basalt fibre in polyformaldehyde material enhancing field.
Description
Technical field
The present invention relates to basalt fibre size field, and in particular to a kind of polyformaldehyde material enhancing basalt fibre is special
With size and preparation method thereof.
Background technology
Basalt fibre is a kind of emerging novel inorganic environment-friendly and green high performance fibre material, is following China's emphasis
One of four big high-performance fibers of development, it is aoxidized by silica, aluminum oxide, calcium oxide, iron oxide and titanium dioxide etc.
The basalt building stones of thing composition are prepared after high-temperature fusion by spinning technique.Basalt continuous fiber is not only stablized
Property it is good, but also with a variety of excellent properties such as electrical insulating property, anticorrosive, flame resistant, high temperature resistant, moreover, basalt fibre
Discarded object is few caused by production technology, and environmental pollution is small, directly can be transferred to after product abandonment in ecological environment, without any danger
Evil, thus be a kind of qualified green, environment-friendly materials.Basalt continuous fiber is in fibre reinforced composites, friction
The many aspects such as material, shipbuilding materials, heat-barrier material, automobile industry, high temperature filtration fabric and protection field have obtained extensively
Application.
Polyformaldehyde also known as acetal resin, polyoxymethylene.Full name acetal resin, abbreviation polyformaldehyde, english abbreviation are
POM, thermoplastic crystalline polymer, it is one of five big general engineering plastics, high comprehensive performance, there is high mechanical property, such as
Intensity, modulus, wearability, toughness, fatigue durability and creep resistance, also with excellent electrical insulating property, solvent resistance and Ke Jia
Work；But because crystallinity is high in polyformaldehyde（Crystallinity ＞ 70%）, cause polyformaldehyde material poor toughness to be present（Elongation at break
＜ 15%）, molding shrinkage（2.0-3.5%）It is the defects of big, therefore, more without using pure polyformaldehyde material, poly- first when in use
Aldehyde material needs to be applied after carrying out the composite modified processing of the enhancing such as mechanical property, fire-retardant, corrosion-resistant.Now to poly- first
The fiber-reinforced modified of aldehyde material is mainly modified processing using glass fiber material, and modified effect is notable, but glass fibre
Production cost is high, environmental pollution is big, seriously limits the application of compound polyformaldehyde material, develops that a kind of cost is cheap, green ring
Protect, the new fiber materials of excellent performance substitute the problem of glass fibre is modified processing to polyformaldehyde material and are badly in need of being solved
Certainly.Therefore, it is possible to, it is envisioned that nontoxic, pollution-free, wide material sources, excellent performance, the basalt fibre stablized are used for polyformaldehyde
The enhancing of material will improve the new trend of polyformaldehyde material performance from now on.But due to existing basalt fibre self structure and
Stable performance, fiber surface is smooth, surface-active site is few, causes basalt fibre to be difficult in modifying process and polyformaldehyde material
Material chemical bonding and mechanical riveted form unified, stable entirety, i.e. basalt fibre is independently to deposit in polyformaldehyde material
The modification humidification to polyformaldehyde material is relatively weak, and enhancing effect is not satisfactory, and basalt fibre addition is few.
Size can not only carry out physics bag as the most important auxiliary reagent used in fiber production process to fiber
Cover, increase tenacity of fibre and lubricity, moreover it is possible to fiber surface is chemically treated, increases fiber feature, therefore, using leaching
Profit agent is modified processing to fibrous material, i.e., is combined into one the production of fiber and modification, and section simplifies production stage, saves
Production cost, shortens the production cycle, moreover it is possible to assign the new performance of fiber to meet fiber in different field, varying environment
Application, therefore, basalt fibre surface is modified to carry in basalt fibre production process using sizing agent special
The compatibility of high basalt fibre and polyformaldehyde material is feasible, and may advantageously facilitate basalt fibre strengthens in polyformaldehyde material
Popularization and application in field.
The content of the invention
It is an object of the invention to overcome existing basalt fibre size to improve basalt fibre and polyformaldehyde material
A kind of the defects of expecting compatibility, there is provided polyformaldehyde enhancing basalt fibre sizing agent special and preparation method thereof；Present invention infiltration
Contain modifying agent in agent, fiber surface is modified while infiltration by modifying agent, makes the increase of fiber surface roughness
And a large amount of active groups are grafted, so as to improve chemical bonding and the mechanical riveted energy between basalt fibre and polyformaldehyde material
Power, the compatibility of basalt fibre and polyformaldehyde material is improved, promote basalt fibre strengthens field in polyformaldehyde material
In popularization and application.
In order to realize foregoing invention purpose, the invention provides a kind of polyformaldehyde material to strengthen the special infiltration of basalt fibre
Agent, including following parts by weight of component：The film forming agent of 40-60 parts, the coupling agent of 5-15 parts, 1-5 parts lubricants, 10-20 parts change
Property agent, the solvent of 30-50 parts.
Above-mentioned a kind of polyformaldehyde material enhancing basalt fibre sizing agent special, wherein described modifying agent includes hypophosphorous acid
The Yan ︰ acid mixture that 5-8 ︰ 1-3 are mixed in mass ratio；The modifying agent composition can be quickly rotten to basalt fibre surface
Erosion, activation, form rough surface, and are grafted a large amount of active groups, fiber surface is formed a large amount of avtive spots and active group,
So that basalt fibre can carry out chemical bonding and mechanical riveted with polyformaldehyde；Described mechanical riveted refers to that matrix material leads to
Cross shrinkage stress pack tightly rough surface fiber and caused frictional engagement；Preferably, described modifying agent includes Ci Lin Suan Yan ︰
The acid mixture that 6 ︰ 2 are mixed in mass ratio.
Above-mentioned a kind of polyformaldehyde material enhancing basalt fibre sizing agent special, wherein described hypophosphites is dimethyl
Hypophosphites, ethylmethylphosphiniacid acid salt, methyl n-propyl hypophosphites, dimethylamino methane base hypophosphites, benzene-Isosorbide-5-Nitrae-dimethyl
The one or more of hypophosphites, aminomethyl phenyl hypophosphites or diphenyl hypophosphites.
A kind of above-mentioned polyformaldehyde material enhancing basalt fibre sizing agent special, wherein described acid be sulfurous acid, oxalic acid,
One or more in formic acid, acetic acid, ethanedioic acid.
A kind of polyformaldehyde material strengthens basalt fibre sizing agent special, in modifying agent under the collective effect of each component,
With can quickly to basalt fibre surface corrosion formed rough surface and fiber surface grafting largely can with polyformaldehyde chemistry
The effect of bonded active group, so that basalt fibre after the processing by the size, not only has preferably tough
Property and lubricity, be advantageous to the post-production of basalt fibre, moreover it is possible to improve basalt fibre and be chemically bonded with polyformaldehyde
With the ability of mechanical riveted, that is, improve the compatibility of basalt fibre and polyformaldehyde；Size of the present invention promotes basalt
Extensive use of the fiber in polyformaldehyde material enhancing field.
Above-mentioned a kind of polyformaldehyde material enhancing basalt fibre sizing agent special, wherein described film forming agent is butadiene tree
Fat film forming agent；Film forming agent can form membrane structure on basalt fibre surface well, increase basalt fibre toughness, and can improve
The compatibility of basalt fibre and polyformaldehyde material.
Above-mentioned a kind of polyformaldehyde material enhancing basalt fibre sizing agent special, wherein described coupling agent is to contain aldehyde
The modified silane coupler of one or two kinds of groups in base, ether；The silane coupler can be with silicon atom in basalt fibre
Coupling, and can are coupled with polyformaldehyde material, and coupling effect is best.
Above-mentioned a kind of polyformaldehyde material enhancing basalt fibre sizing agent special, wherein described lubricant is stearic acid first
One kind in ester and zinc stearate.
Above-mentioned a kind of polyformaldehyde material enhancing basalt fibre sizing agent special, wherein described solvent is the water-soluble of ethanol
Liquid；The volume ratio of ethanol and water is 1-3 ︰ 1 in the aqueous solution of the ethanol；Preferably, ethanol and water in the aqueous solution of ethanol
Volume ratio is 2 ︰ 1.
Preferably, a kind of polyformaldehyde material enhancing basalt fibre sizing agent special, including following parts by weight of component：50 parts
Film forming agent, 10 parts of coupling agent, 3 parts of lubricants, 15 parts of modifying agent, 40 parts of solvent.
In order to realize foregoing invention purpose, further, the invention provides a kind of polyformaldehyde material enhancing basalt is fine
The preparation method of sizing agent special is tieed up, is comprised the following steps：
（1）Modifying agent is dissolved to form mixed solution A with solvent；Coupling agent and lubricant are added after film forming agent is dissolved with solvent
Form mixed solution B；
（2）The mixed solution A that step 1 is obtained, which is added to be well mixed in mixed solution B, forms mixed solution C；
（3）The mixed solution C defoaming treatment that step 2 obtains is obtained into polyformaldehyde material enhancing basalt fibre sizing agent special.
The preparation method of above-mentioned a kind of polyformaldehyde material enhancing basalt fibre sizing agent special, wherein described in step 3
Defoaming treatment is physical defoaming；Avoid the generation of introducing or the side reaction of impurity.
A kind of preparation method of polyformaldehyde material enhancing basalt fibre sizing agent special, by the dilution dissolving of modifying agent with
Film forming agent, coupling agent, the mixed dissolution of lubricant are separately handled, and a large amount of thermal conductivities for avoiding modifying agent from being released when diluting and dissolving cause
The generation of side reaction, and it is clear, succinct to produce orderliness；The inventive method is simple, reliable, is adapted to polyformaldehyde material enhancing basalt
Extensive, the industrialized production of fiber sizing agent special.
Compared with prior art, beneficial effects of the present invention：
1st, polyformaldehyde material enhancing basalt fibre sizing agent special of the present invention can be formed quickly to basalt fibre surface corrosion
Rough surface, improve the mechanical riveted ability between basalt fibre and polyformaldehyde material.
2nd, polyformaldehyde material enhancing basalt fibre sizing agent special infiltration of the present invention can be quickly big in fiber surface grafting
Amount can improve the chemical bonding energy between basalt fibre and polyformaldehyde material with the active group of polyformaldehyde chemical bonding
Power.
3rd, polyformaldehyde material enhancing basalt fibre sizing agent special of the present invention can improve basalt fibre and polyformaldehyde material
Compatibility between material, promote extensive use of the basalt fibre in polyformaldehyde material enhancing field.
4th, the preparation method of polyformaldehyde material enhancing basalt fibre sizing agent special of the present invention is simple, reliable, is adapted to poly-
Formaldehyde materials strengthen extensive, the industrialized production of basalt fibre sizing agent special.
Embodiment
With reference to test example and embodiment, the present invention is described in further detail.But this should not be understood
Following embodiment is only limitted to for the scope of the above-mentioned theme of the present invention, it is all that this is belonged to based on the technology that present invention is realized
The scope of invention.
Embodiment 1
（1）15 parts by weight are contained into dimethyl Ci Lin Suan Na ︰ oxalic acid 10 parts by weight of the modifying agent that 6 ︰ 2 are mixed in mass ratio
Ethanol and the water of 10 parts by weight dissolve to form mixed solution A；By the butadiene resin film forming agent of 50 parts by weight with 10 parts by weight
Ethanol and 10 parts by weight water dissolving after add the silane coupler of 10 parts by weight and the methyl stearate of 3 parts by weight formed it is mixed
Close solution B；
（2）The mixed solution A that step 1 is obtained, which is added to be well mixed in mixed solution B, forms mixed solution C；
（3）The mixed solution C defoaming treatment that step 2 obtains is obtained into polyformaldehyde material enhancing basalt fibre sizing agent special.
Embodiment 2
（1）10 parts by weight are contained into benzene-Isosorbide-5-Nitrae-dimethyl hypophosphorous acid Jia ︰ sulfurous acid modifying agent that 5 ︰ 1 are mixed in mass ratio
Dissolve to form mixed solution A with the ethanol of 5 parts by weight and the water of 5 parts by weight；The butadiene resin film forming agent of 60 parts by weight is used
The silane coupler of 15 parts by weight and the zinc stearate of 1 parts by weight are added after the ethanol of 20 parts by weight and the dissolving of the water of 10 parts by weight
Form mixed solution B；
（2）The mixed solution A that step 1 is obtained, which is added to be well mixed in mixed solution B, forms mixed solution C；
（3）The mixed solution C defoaming treatment that step 2 obtains is obtained into polyformaldehyde material enhancing basalt fibre sizing agent special.
Embodiment 3
（1）20 parts by weight are contained into ethylmethylphosphiniacid acid Na ︰ acetic acid 10 weight of the modifying agent that 8 ︰ 3 are mixed in mass ratio
The ethanol of part and the water of 10 parts by weight dissolve to form mixed solution A；By the butadiene resin film forming agent of 40 parts by weight with 10 weight
The silane coupler of 5 parts by weight is added after the ethanol of part and the water dissolving of 20 parts by weight and the methyl stearate of 5 parts by weight is formed
Mixed solution B；
（2）The mixed solution A that step 1 is obtained, which is added to be well mixed in mixed solution B, forms mixed solution C；
（3）The mixed solution C defoaming treatment that step 2 obtains is obtained into polyformaldehyde material enhancing basalt fibre sizing agent special.
Comparative example 1
（1）10 are added after the butadiene resin film forming agent of 50 parts by weight is dissolved with the ethanol of 20 parts by weight and the water of 20 parts by weight
The silane coupler of parts by weight and the methyl stearate of 3 parts by weight form mixed solution；
（2）The mixed solution defoaming treatment that step 1 obtains is obtained into size.
Comparative example 2
（1）15 parts by weight are contained into dimethyl Ci Lin Suan Na ︰ oxalic acid 10 parts by weight of the modifying agent that 6 ︰ 4 are mixed in mass ratio
Ethanol and the water of 10 parts by weight dissolve to form mixed solution A；By the butadiene resin film forming agent of 50 parts by weight with 10 parts by weight
Ethanol and 10 parts by weight water dissolving after add the silane coupler of 10 parts by weight and the methyl stearate of 3 parts by weight formed it is mixed
Close solution B；
（2）The mixed solution A that step 1 is obtained, which is added to be well mixed in mixed solution B, forms mixed solution C；
（3）The mixed solution C defoaming treatment that step 2 obtains is obtained into polyformaldehyde material enhancing basalt fibre sizing agent special.
Comparative example 3
（1）15 parts by weight are contained into dimethyl Ci Lin Suan Na ︰ oxalic acid 10 parts by weight of the modifying agent that 4 ︰ 2 are mixed in mass ratio
Ethanol and the water of 10 parts by weight dissolve to form mixed solution A；By the butadiene resin film forming agent of 50 parts by weight with 10 parts by weight
Ethanol and 10 parts by weight water dissolving after add the silane coupler of 10 parts by weight and the methyl stearate of 3 parts by weight formed it is mixed
Close solution B；
（2）The mixed solution A that step 1 is obtained, which is added to be well mixed in mixed solution B, forms mixed solution C；
（3）The mixed solution C defoaming treatment that step 2 obtains is obtained into polyformaldehyde material enhancing basalt fibre sizing agent special.
Preparation-obtained size in above-described embodiment 1-3 and comparative example 1-3 is respectively used to infiltrate basalt of the same race
Fiber, obtained basalt fibre is subjected to performance test and acetal plastic（Elongation at break 15%, notch impact strength 7.6
KJ/m2, molding shrinkage 2.0-3.5%）Enhancing（Basalt fibre dosage is the 30% of polyformaldehyde quality）Experiment, record experiment knot
Fruit, record data are as follows：
| Numbering | Tensile strength（MPa） | Elongation at break（%） | Modified acetal plastic notch impact strength（KJ/m2） | Modified acetal plastic elongation at break（%） | Modified acetal plastic molding shrinkage（%） |
| Embodiment 1 | 3850 | 2.6 | 15.3 | 35 | 0.5-0.9 |
| Embodiment 2 | 3810 | 2.4 | 15.0 | 38 | 0.5-0.9 |
| Embodiment 3 | 3820 | 2.5 | 14.9 | 37 | 0.5-0.9 |
| Comparative example 1 | 3940 | 2.6 | 9.4 | 23 | 1.1-1.6 |
| Comparative example 2 | 3510 | 1.8 | 8.6 | 16 | 0.7-1.3 |
| Comparative example 3 | 3620 | 2.3 | 8.5 | 19 | 0.8-1.5 |
Above-mentioned analysis of experimental data is understood, size is obtained to basalt fibre using technical solution of the present invention in embodiment 1-3
Dimension carries out infiltration processing, and obtained basalt fibre draws Shen intensity and elongation at break good, good with polyformaldehyde compatibility, to poly- first
Aldehyde plastics enhancing effect is notable；And size does not add modifying agent in comparative example 1, as conventional size, with the size
Basalt fibre after processing is conventional basalt fibre, and the poor compatibility between the basalt fibre and polyformaldehyde material is right
Polyformaldehyde material humidification is obviously reduced；Do not have to use using the modifier components proportioning protected in the present invention in comparative example 2
Amount, consumption of oxalic acid is excessive, and size is damaged to basalt fiber construction, caused to basalt fibre surface erosion transition
The tensile strength and elongation at break of basalt fibre significantly reduce, so as to the humidification of polyformaldehyde fibre also significantly under
Drop；Do not have in comparative example 3 using the modifier components proportioning dosage protected in the present invention, dimethyl sodium hypophosphite dosage mistake
Greatly, size weakens to basalt fibre surface activation, and the active group of basalt fibre surface grafting is few, with polyformaldehyde
The chemical bonding ability of material, is obviously reduced to polyformaldehyde material humidification.
Claims (10)
1. a kind of polyformaldehyde material strengthens basalt fibre sizing agent special, it is characterised in that including following parts by weight of component：
The film forming agent of 40-60 parts, the coupling agent of 5-15 parts, 1-5 parts lubricant, the modifying agent of 10-20 parts, the solvent of 30-50 parts；It is described
Modifying agent includes the hypophosphites and acid that mass ratio is 5-8 ︰ 1-3.
2. size according to claim 1, it is characterised in that the modifying agent includes the hypophosphorous acid that mass ratio is 6 ︰ 2
Salt and acid.
3. size according to claim 1, it is characterised in that including following parts by weight of component：50 parts of film forming agent, 10
The coupling agent, 3 parts of lubricants, 15 parts of modifying agent, 40 parts of solvent of part.
4. size according to claim 1, it is characterised in that the hypophosphites is dimethyl hypophosphites, ethyl
Methyl hypophosphites, methyl n-propyl hypophosphites, dimethylamino methane base hypophosphites, benzene-Isosorbide-5-Nitrae-dimethyl hypophosphites, methyl
The one or more of phenyl hypophosphites or diphenyl hypophosphites.
5. size according to claim 1, it is characterised in that the acid is sulfurous acid, oxalic acid, formic acid, acetic acid, second two
One or more in acid.
6. size according to claim 1, it is characterised in that the film forming agent is butadiene resin film forming agent.
7. size according to claim 1, it is characterised in that the coupling agent be containing a kind of in aldehyde radical, ether or
The modified silane coupler of two kinds of groups.
8. size according to claim 1, it is characterised in that the lubricant is in methyl stearate and zinc stearate
One kind.
9. size according to claim 1, it is characterised in that the solvent is the aqueous solution of ethanol.
10. the preparation method of polyformaldehyde material enhancing basalt fibre sizing agent special, its feature exist described in a kind of claim 1
In comprising the following steps：
（1）Modifying agent is dissolved to form mixed solution A with solvent；Coupling agent and lubricant are added after film forming agent is dissolved with solvent
Form mixed solution B；
（2）The mixed solution A that step 1 is obtained, which is added to be well mixed in mixed solution B, forms mixed solution C；
（3）The mixed solution C defoaming treatment that step 2 obtains is obtained into polyformaldehyde material enhancing basalt fibre sizing agent special.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611082866.7A CN107385915A (en) | 2016-11-30 | 2016-11-30 | A kind of polyformaldehyde material enhancing basalt fibre sizing agent special and preparation method thereof |
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| CN201611082866.7A CN107385915A (en) | 2016-11-30 | 2016-11-30 | A kind of polyformaldehyde material enhancing basalt fibre sizing agent special and preparation method thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102515570A (en) * | 2011-11-30 | 2012-06-27 | 淄博新力特种纤维科技有限公司 | Pre-processing reinforced type impregnating agent for basalt fiber chopped spun yarn and preparation method of pre-processing reinforced type impregnating agent |
| CN103936302A (en) * | 2014-04-21 | 2014-07-23 | 四川航天拓鑫玄武岩实业有限公司 | Continuous basalt fiber assembled twist-less roving impregnating compound and preparation method thereof |
| CN104692674A (en) * | 2015-02-10 | 2015-06-10 | 四川省西玄科技有限公司 | Special epoxy impregnating compound for basalt fiber and preparation method of special epoxy impregnating compound |
| CN105036568A (en) * | 2015-06-30 | 2015-11-11 | 四川航天五源复合材料有限公司 | Stable basalt continuous fiber impregnating compound |
| CN105601129A (en) * | 2015-12-23 | 2016-05-25 | 晏玲莉 | Reinforced soakage agent for basalt fibers |
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2016
- 2016-11-30 CN CN201611082866.7A patent/CN107385915A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102515570A (en) * | 2011-11-30 | 2012-06-27 | 淄博新力特种纤维科技有限公司 | Pre-processing reinforced type impregnating agent for basalt fiber chopped spun yarn and preparation method of pre-processing reinforced type impregnating agent |
| CN103936302A (en) * | 2014-04-21 | 2014-07-23 | 四川航天拓鑫玄武岩实业有限公司 | Continuous basalt fiber assembled twist-less roving impregnating compound and preparation method thereof |
| CN104692674A (en) * | 2015-02-10 | 2015-06-10 | 四川省西玄科技有限公司 | Special epoxy impregnating compound for basalt fiber and preparation method of special epoxy impregnating compound |
| CN105036568A (en) * | 2015-06-30 | 2015-11-11 | 四川航天五源复合材料有限公司 | Stable basalt continuous fiber impregnating compound |
| CN105601129A (en) * | 2015-12-23 | 2016-05-25 | 晏玲莉 | Reinforced soakage agent for basalt fibers |
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