CN105036571A - Preparation method of basalt fiber sizing - Google Patents

Preparation method of basalt fiber sizing Download PDF

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Publication number
CN105036571A
CN105036571A CN201510370436.4A CN201510370436A CN105036571A CN 105036571 A CN105036571 A CN 105036571A CN 201510370436 A CN201510370436 A CN 201510370436A CN 105036571 A CN105036571 A CN 105036571A
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China
Prior art keywords
coupling agent
treating compound
agent
membrane
preparation
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CN201510370436.4A
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Chinese (zh)
Inventor
黄明
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Sichuan Aerospace Wuyuan Composite Co Ltd
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Sichuan Aerospace Wuyuan Composite Co Ltd
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Priority to CN201510370436.4A priority Critical patent/CN105036571A/en
Publication of CN105036571A publication Critical patent/CN105036571A/en
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Abstract

The invention discloses a preparation method of basalt fiber sizing. The basalt fiber sizing is mixed emulsion which is prepared from a film forming agent, a coupling agent, a lubricating agent and water, wherein the film forming agent is the main component. The preparation method comprises the preparation steps of adding the coupling agent, the lubricating agent and the like after diluting the film forming agent by water, and stirring after complete mixing so as to obtain a sizing finished product. The basalt fiber sizing is mainly used for coating basalt fiber, has the function of improving the beam collection property and the wear resistance of the basalt fiber besides good permeability and good stability, and is capable of increasing the mechanical property of the basalt fiber and increasing the breaking strength, tensile property and shearing strength.

Description

A kind of preparation method of basalt fibre treating compound
Technical field
The invention belongs to the preparation field of matrix material, specifically, is a kind of preparation method of basalt fibre treating compound.
Background technology
In existing field of compound material, fiber as composite material reinforcement body mainly contains glass fibre, carbon fiber, boron fibre, sapphire whisker, silicon carbide fiber, polyethylene fibre etc., but due to the restriction of price factor, major part fiber is all only for military field, glass fibre is only had to be widely used in civil area, but in actual application, also there is certain defect as composite material reinforcement body in glass fibre, as:
(1) the production process energy consumption of glass fibre is comparatively large, is unfavorable for energy-conserving and environment-protective;
(2) preparation technology of glass fibre is to harmful, and especially glass fibre hair can produce hormesis to human body skin, can not be decomposed or absorb, probably cause pulmonary disorder even to produce canceration after sucking human body;
(3) environmental pollution is large, can not recycle or natural degradation, be unfavorable for the protection of environment after glass fiber compound material is discarded, etc.
Certainly, for overcoming the familiar lacunas of above-mentioned composite material reinforcement body, there has been proposed the use adopting basalt fibre as composite material reinforcement body, for basalt fibre, we know, it is for raw material with natural volcano extrusive rock, under the high temperature of 1450 ~ 1500 DEG C after melting, by the continuous fibre of platinum germanium alloy bushing wire drawing manufacture, there is high strength, high-modulus, high temperature resistant, anti-oxidant, acid and alkali-resistance, radioprotective, electrical isolation, adiabatic sound insulation, filterableness is good, ultimate compression strength is high, many premium propertiess such as damping and shearing resistance height, simultaneously, also be a kind of novel tRecycled Fibers.
At present, conventional basalt fibre treating compound has epoxy emulsion, polyaminoester emulsion and polyester emulsion three kinds, research shows, also certain limitation is there is in existing three kinds of basalt fibre treating compounds when practical application, as: polyaminoester emulsion, as treating compound solution hydrolysis in alkali environment, uses when polyester emulsion is then useful in weaving as treating compound.Existing patent documentation CN102432733.A(cation type emulsion for basalt fibre treating compound and preparation method thereof, 2012.05.02) a kind of ionic emulsion that can be used as membrane-forming agent use in basalt fibre treating compound and glass fiber infiltration agent is disclosed, there is synthesis cost low, can dissolve each other with other components in treating compound, treating compound can be made to show good impregnability and stability.
For improving the characteristic of existing composite products, the development for the treatment of compound is also being updated.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of basalt fibre treating compound, adopt the mixing of membrane-forming agent, coupling agent, lubricant and water obtained, the coating being mainly used in basalt fibre uses, except there is good impregnability, stability, also there is the effect improving basalt fibre convergency, wear resistance, the mechanical property of basalt fibre can be improved, ultimate strength, tensile property and shearing resistance are improved.
The present invention is achieved through the following technical solutions: a kind of preparation method of basalt fibre treating compound, and described treating compound is that its preparation process is as follows by the obtained mixed emulsion of membrane-forming agent, coupling agent, lubricant and water:
A: deposit the obtained membrane-forming agent through polymerization in case by epoxy monomer at emulsifying agent, the particle diameter of described membrane-forming agent is 0.05 ~ 1 μm, for subsequent use;
B: use H 2n-silane coupling agent is as coupling agent, for subsequent use;
C: use the mixture of one or more compositions in fatty acid amide, polyester, synthetic ester, carboxylic acid as lubricant, for subsequent use;
D: use water that the membrane-forming agent that steps A is obtained is diluted with water to 40 ~ 55% concentration, after stirring, adds the H that step B selects successively 2the lubricant that N-silane coupling agent and step C obtain, is uniformly mixed 1 ~ 2h again after mixing fully, obtains treating compound finished product.
The treating compound that the present invention relates to is based on membrane-forming agent, be equipped with the coupling agent of suitable proportion again, lubricant, water makes, membrane-forming agent prepares polymerized emulsion by epoxy resin, this polymerized emulsion moderate in grain size, after being combined with other auxiliary agents, show good spreadability, can improve the surface property of basalt fibre, mechanical property and composite property, suitability is strong.
In percentage terms, described treating compound finished product include 44 ~ 62% membrane-forming agent, 8 ~ 15% coupling agent, 1.2 ~ 2.6% lubricant, all the other are for water.
To better implement the present invention, in described steps A, the structural formula of the emulsifying agent of use meets:
Further, in described steps A, the size controlling of membrane-forming agent is at 0.15 ~ 0.75 μm, and concentration controls 45 ~ 52%.
For convenience of mixing mutually with other components, first the coupling agent that the present invention relates to uses deionized water be hydrolyzed, after acetic acid adjustment pH value, then adds and adds in the lump in membrane-forming agent with other components, for the preparation for the treatment of compound, therefore, in described step B, also comprise H 2the dilution of N-silane coupling agent, comprising: at H 2add deionized water and acetic acid successively in N-silane coupling agent, after mix and blend, obtained pH value is the hydrating solution of 4 ~ 6, counts in mass ratio, described deionized water: acetic acid: H 2n-silane coupling agent=(20 ~ 40): (1 ~ 1.5): (2 ~ 2.5).
The lubricant that the present invention relates to has good lubricant effect, has again good organic antistatic property concurrently simultaneously, in described step C, uses water to be after the mixed solution of 50 ~ 60% by the concentration of lubricant formulation, for subsequent use.
The present invention compared with prior art, has the following advantages and beneficial effect:
(1) the present invention adopts based on membrane-forming agent, be equipped with again the coupling agent of suitable proportion, lubricant, water mixing method prepare treating compound, the coating being mainly used in basalt fibre uses, except there is good impregnability, stability, also there is the effect improving basalt fibre convergency, wear resistance, the mechanical property of basalt fibre can be improved, ultimate strength, tensile property and shearing resistance are improved.
(2) membrane-forming agent that the present invention relates to is base-material by epoxy resin, polymerized emulsion is prepared with after emulsifying agent condensation reaction, this polymerized emulsion moderate in grain size, after being combined with other auxiliary agents, show good spreadability, can improve the surface property of basalt fibre, mechanical property and composite property, suitability is strong.
(3) the present invention uses the object of coupling agent to be do tackifier to use, and particle assembly and polymkeric substance in sizing system can be avoided to have multiviscosisty, also can improve organic polymer to strong wettability of mending filler, usually use H 2n-silane coupling agent, in treating compound, shared composition is 8 ~ 15%.
(4) lubricant that the present invention relates to has good lubricant effect, has again good organic antistatic property concurrently simultaneously.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1:
The preparation method of the basalt fibre treating compound that the present embodiment relates to comprises the steps:
A: deposit the obtained membrane-forming agent through polymerization in case by epoxy monomer at emulsifying agent, the particle diameter of membrane-forming agent is 0.05 μm, for subsequent use;
B: use H 2n-silane coupling agent is as coupling agent, for subsequent use;
C: use the mixture of fatty acid amide and polyester composition as lubricant, for subsequent use, the mass ratio of fatty acid amide and polyester is 1:1;
D: use water that the membrane-forming agent that steps A is obtained is diluted with water to 40% concentration, after stirring, adds the H that step B selects successively 2the lubricant that N-silane coupling agent and step C obtain, is uniformly mixed 1h again after mixing fully, obtains treating compound finished product.
In percentage terms, include in the treating compound finished product that above-mentioned preparation method obtains the membrane-forming agent of 44%, 8% coupling agent, 1.2% lubricant, all the other are water.
Embodiment 2:
The preparation method of the basalt fibre treating compound that the present embodiment relates to comprises the steps:
A: deposit the obtained membrane-forming agent through polymerization in case by epoxy monomer at emulsifying agent, the particle diameter of membrane-forming agent is 1 μm, for subsequent use;
B: use H 2n-silane coupling agent is as coupling agent, for subsequent use;
C: use synthetic ester as lubricant, for subsequent use;
D: use water that the membrane-forming agent that steps A is obtained is diluted with water to 55% concentration, after stirring, adds the H that step B selects successively 2the lubricant that N-silane coupling agent and step C obtain, is uniformly mixed 2h again after mixing fully, obtains treating compound finished product.
In percentage terms, include in the treating compound finished product that above-mentioned preparation method obtains the membrane-forming agent of 62%, 15% coupling agent, 2.6% lubricant, all the other are water.
Embodiment 3:
The difference of the present embodiment and embodiment 1 is: in the steps A that the present embodiment relates to, and the structural formula of the emulsifying agent of use meets:
In percentage terms, include in the treating compound finished product that the present embodiment obtains the membrane-forming agent of 45%, 10% coupling agent, 1.5% lubricant, all the other are for water.
Embodiment 4:
The difference of the present embodiment and embodiment 2 is: in the steps A that the present embodiment relates to, and the structural formula of the emulsifying agent of use meets:
In percentage terms, include in the treating compound finished product that the present embodiment obtains the membrane-forming agent of 44%, 10% coupling agent, 1.3% lubricant, all the other are for water.
Embodiment 5:
The difference of the present embodiment and embodiment 1 is: in the steps A that the present embodiment relates to, and the size controlling of membrane-forming agent is at 0.15 μm, and concentration controls 45%.
In percentage terms, include in the treating compound finished product that the present embodiment obtains the membrane-forming agent of 48%, 11% coupling agent, 2.0% lubricant, all the other are for water.
Embodiment 6:
The difference of the present embodiment and embodiment 2 is: in the steps A that the present embodiment relates to, and the size controlling of membrane-forming agent is at 0.75 μm, and concentration controls 52%.
In percentage terms, include in the treating compound finished product that the present embodiment obtains the membrane-forming agent of 45%, 12% coupling agent, 2.2% lubricant, all the other are for water.
Embodiment 7:
The difference of the present embodiment and embodiment 1 is: in the step B that the present embodiment relates to, also comprise H 2the dilution of N-silane coupling agent, comprising: at H 2add deionized water and acetic acid successively in N-silane coupling agent, after mix and blend, obtained pH value is the hydrating solution of 4, counts in mass ratio, deionized water: acetic acid: H 2n-silane coupling agent=20:1:2.
In percentage terms, include in the treating compound finished product that the present embodiment obtains the membrane-forming agent of 55%, 10% coupling agent, 1.2% lubricant, all the other are for water.
Embodiment 8:
The difference of the present embodiment and embodiment 2 is: in the step B that the present embodiment relates to, also comprise H 2the dilution of N-silane coupling agent, comprising: at H 2add deionized water and acetic acid successively in N-silane coupling agent, after mix and blend, obtained pH value is the hydrating solution of 6, counts in mass ratio, deionized water: acetic acid: H 2n-silane coupling agent=40:1.5:2.5.
In percentage terms, include in the treating compound finished product that the present embodiment obtains the membrane-forming agent of 50%, 11.5% coupling agent, 1.5% lubricant, all the other are for water.
Embodiment 9:
The difference of the present embodiment and embodiment 1 is: in the step C that the present embodiment relates to, and uses water to be after the mixed solution of 60% by the concentration of lubricant formulation, for subsequent use.
In percentage terms, include in the treating compound finished product that the present embodiment obtains the membrane-forming agent of 52%, 10% coupling agent, 2.2% lubricant, all the other are for water.
Embodiment 10:
The difference of the present embodiment and embodiment 2 is: in the step C that the present embodiment relates to, and uses water to be after the mixed solution of 50% by the concentration of lubricant formulation, for subsequent use.
In percentage terms, include in the treating compound finished product that the present embodiment obtains the membrane-forming agent of 47%, 9% coupling agent, 2.6% lubricant, all the other are for water.
Embodiment 11:
The preparation method of the basalt fibre treating compound that the present embodiment relates to comprises the steps:
A: be prepared into film, deposit the obtained membrane-forming agent through polymerization in case by epoxy monomer at emulsifying agent, for subsequent use, the size controlling of membrane-forming agent is at 0.35 μm, and concentration controls 50%, and the structural formula of the emulsifying agent of use meets:
B: prepare coupling agent, selects H 2n-silane coupling agent, at H 2add deionized water and acetic acid successively in N-silane coupling agent, after mix and blend, obtained pH value is the hydrating solution of 5, for subsequent use, counts in mass ratio, deionized water: acetic acid: H 2n-silane coupling agent=30:1:2.2;
C: use fatty acid amide as lubricant, then use water to be after the mixed solution of 52% by the concentration of this lubricant formulation, for subsequent use;
D: use water that the membrane-forming agent that steps A is obtained is diluted with water to 45% concentration, after stirring, adds the H that step B selects successively 2the lubricant that N-silane coupling agent and step C obtain, is uniformly mixed 1h again after mixing fully, obtains treating compound finished product.
In percentage terms, include in the treating compound finished product that above-mentioned preparation method obtains the membrane-forming agent of 50%, 10% coupling agent, 2.1% lubricant, all the other are water.
Embodiment 12:
The preparation method of the basalt fibre treating compound that the present embodiment relates to comprises the steps:
A: be prepared into film, deposit the obtained membrane-forming agent through polymerization in case by epoxy monomer at emulsifying agent, for subsequent use, the size controlling of membrane-forming agent is at 0.45 μm, and concentration controls 48%, and the structural formula of the emulsifying agent of use meets:
B: prepare coupling agent, selects H 2n-silane coupling agent, at H 2add deionized water and acetic acid successively in N-silane coupling agent, after mix and blend, obtained pH value is the hydrating solution of 5, for subsequent use, counts in mass ratio, deionized water: acetic acid: H 2n-silane coupling agent=28:1.2:2;
C: use the mixture of fatty acid amide and carboxylic acid composition as lubricant, then use water to be after the mixed solution of 58% by the concentration of this lubricant formulation, for subsequent use, the mass ratio of fatty acid amide and carboxylic acid is 1:2;
D: use water that the membrane-forming agent that steps A is obtained is diluted with water to 42% concentration, after stirring, adds the H that step B selects successively 2the lubricant that N-silane coupling agent and step C obtain, is uniformly mixed 2h again after mixing fully, obtains treating compound finished product.
In percentage terms, include in the treating compound finished product that above-mentioned preparation method obtains the membrane-forming agent of 56%, 12% coupling agent, 2.3% lubricant, all the other are water.
Embodiment 13:
The preparation method of the basalt fibre treating compound that the present embodiment relates to comprises the steps:
A: be prepared into film, deposit the obtained membrane-forming agent through polymerization in case by epoxy monomer at emulsifying agent, for subsequent use, the size controlling of membrane-forming agent is at 0.42 μm, and concentration controls 50%, and the structural formula of the emulsifying agent of use meets:
B: prepare coupling agent, selects H 2n-silane coupling agent, at H 2add deionized water and acetic acid successively in N-silane coupling agent, after mix and blend, obtained pH value is the hydrating solution of 5.5, for subsequent use, counts in mass ratio, deionized water: acetic acid: H 2n-silane coupling agent=35:1.2:2.4;
C: use the mixture of polyester, synthetic ester and carboxylic acid composition as lubricant, then use water to be after the mixed solution of 54% by the concentration of this lubricant formulation, for subsequent use, the mass ratio of polyester, synthetic ester and carboxylic acid is 2:3:1;
D: use water that the membrane-forming agent that steps A is obtained is diluted with water to 52% concentration, after stirring, adds the H that step B selects successively 2the lubricant that N-silane coupling agent and step C obtain, is uniformly mixed 1.5h again after mixing fully, obtains treating compound finished product.
In percentage terms, include in the treating compound finished product that above-mentioned preparation method obtains the membrane-forming agent of 60%, 14% coupling agent, 2.5% lubricant, all the other are water.
The above is only preferred embodiment of the present invention, and not do any pro forma restriction to the present invention, every any simple modification, equivalent variations done above embodiment according to technical spirit of the present invention, all falls within protection scope of the present invention.

Claims (6)

1. a preparation method for basalt fibre treating compound, is characterized in that: described treating compound is that its preparation process is as follows by the obtained mixed emulsion of membrane-forming agent, coupling agent, lubricant and water:
A: deposit the obtained membrane-forming agent through polymerization in case by epoxy monomer at emulsifying agent, the particle diameter of described membrane-forming agent is 0.05 ~ 1 μm, for subsequent use;
B: use H 2n-silane coupling agent is as coupling agent, for subsequent use;
C: use the mixture of one or more compositions in fatty acid amide, polyester, synthetic ester, carboxylic acid as lubricant, for subsequent use;
D: use water that the membrane-forming agent that steps A is obtained is diluted with water to 40 ~ 55% concentration, after stirring, adds the H that step B selects successively 2the lubricant that N-silane coupling agent and step C obtain, is uniformly mixed 1 ~ 2h again after mixing fully, obtains treating compound finished product.
2. the preparation method of a kind of basalt fibre treating compound according to claim 1, is characterized in that: in percentage terms, described treating compound finished product include 44 ~ 62% membrane-forming agent, 8 ~ 15% coupling agent, 1.2 ~ 2.6% lubricant, all the other are for water.
3. the preparation method of a kind of basalt fibre treating compound according to claim 1, is characterized in that: in described steps A, and the structural formula of the emulsifying agent of use meets:
4. the preparation method of a kind of basalt fibre treating compound according to claim 1, is characterized in that: in described steps A, and the size controlling of membrane-forming agent is at 0.15 ~ 0.75 μm, and concentration controls 45 ~ 52%.
5. the preparation method of a kind of basalt fibre treating compound according to claim 1, is characterized in that: in described step B, also comprises H 2the dilution of N-silane coupling agent, comprising: at H 2add deionized water and acetic acid successively in N-silane coupling agent, after mix and blend, obtained pH value is the hydrating solution of 4 ~ 6, counts in mass ratio, described deionized water: acetic acid: H 2n-silane coupling agent=(20 ~ 40): (1 ~ 1.5): (2 ~ 2.5).
6. the preparation method of a kind of basalt fibre treating compound according to claim 1, is characterized in that: in described step C, uses water to be after the mixed solution of 50 ~ 60% by the concentration of lubricant formulation, for subsequent use.
CN201510370436.4A 2015-06-30 2015-06-30 Preparation method of basalt fiber sizing Pending CN105036571A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108098964A (en) * 2017-10-30 2018-06-01 江苏中牛高科技材料有限公司 A kind of heat insulating inner wall bamboo fiberboard and preparation method thereof

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CN101734869A (en) * 2009-12-29 2010-06-16 巨石集团有限公司 Treating compound of alkali-free glass fiber direct roving used for wind energy fabric
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

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050084675A1 (en) * 2003-10-17 2005-04-21 Boy-Chy Wang Sizing composition for glass fibers
CN101734869A (en) * 2009-12-29 2010-06-16 巨石集团有限公司 Treating compound of alkali-free glass fiber direct roving used for wind energy fabric
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

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108098964A (en) * 2017-10-30 2018-06-01 江苏中牛高科技材料有限公司 A kind of heat insulating inner wall bamboo fiberboard and preparation method thereof

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