CN106521709B - Special basalt fibre of a kind of polyphenyl thioether material enhancing and preparation method thereof - Google Patents
Special basalt fibre of a kind of polyphenyl thioether material enhancing and preparation method thereof Download PDFInfo
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- CN106521709B CN106521709B CN201611072797.1A CN201611072797A CN106521709B CN 106521709 B CN106521709 B CN 106521709B CN 201611072797 A CN201611072797 A CN 201611072797A CN 106521709 B CN106521709 B CN 106521709B
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Abstract
Enhance special basalt fibre and preparation method thereof the invention discloses a kind of polyphenyl thioether material, basalt fibre of the present invention is by obtained from the processing in process of production of special size, the size includes following parts by weight of component：40-60 parts of film forming agent, 5-15 parts of coupling agent, 1-5 part lubricant, 10-20 parts of modifying agent, 30-50 parts of solvent；Modifying agent includes sulfonate, sulfuric acid, the phenolic compound that mass ratio is 3-6 ︰ 2-4 ︰ 1-3；The basalt fibre is since surface roughness is big and is grafted with a large amount of active groups, chemical bonding and mechanical riveted ability between basalt fibre and polyphenyl thioether material is strong, the compatibility of the basalt fibre and polyphenyl thioether material is good, largely can add and apply in polyphenyl thioether material.
Description
Technical field
The present invention relates to basalt fibre fields, and in particular to a kind of polyphenyl thioether material enhance special basalt fibre and
Preparation method.
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 the four big high-performance fibers of development, it is by oxidations such as silica, aluminium oxide, calcium oxide, iron oxide and titanium dioxide
The basalt building stones of object 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
The waste that production technology generates is few, and environmental pollution is small, can be directly transferred in ecological environment after product abandonment, 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.
Polyphenylene sulfide English is abbreviated as PPS, is a kind of novel high-performance thermoplastic resin, has high mechanical strength, resistance to height
Temperature, chemical resistance, the advantages that fire retardant, thermal stability is good, excellent electrical properties；But since polyphenylene sulfide crystallinity is high, cause
There are the low defects of poor toughness, impact strength for polyphenyl thioether material, therefore, all do not use pure polyphenylene sulfide material when in use
Material, polyphenyl thioether material need to be applied after the composite modified processing of enhancing such as carrying out toughening, increasing impact strength.It is existing
The fiber-reinforced modified main use glass fiber material and carbon fibre material of modern poly-p-phenylene sulfide ether material are modified processing, change
Property significant effect, but glass fibre and carbon fiber production cost is high, environmental pollution is big seriously limits composite polyphenylene sulfide material
Application, a kind of of low cost, environmentally protective, new fiber materials for haveing excellent performance of exploitation substitute glass fibre and carbon fiber pair
Polyphenyl thioether material is modified the problem of processing urgent need and is resolved.Therefore, it is possible to, it is envisioned that by nontoxic, pollution-free, source is wide
The enhancing that basalt fibre that is general, haveing excellent performance, stablized is used for polyphenyl thioether material will improve polyphenylene sulfide material from now on
Expect the new trend of performance.But since basalt fibre self structure and performance are stablized, fiber surface is smooth, surface-active site
It is few, with polyphenylene sulfide poor compatibility, basalt fibre is caused to be difficult in enhancing modifying process and polyphenyl thioether material chemical bond
It closes and mechanical riveted forms entirety that is unified, stablizing, is i.e. basalt fibre is to be individually present in polyphenyl thioether material, to poly-
The modification humidification of diphenyl sulfide material is relatively weak, and enhancing effect is not satisfactory, and basalt fibre additive amount is few.
Invention content
It is an object of the invention to overcome the defect of existing basalt fibre and polyphenyl thioether material poor compatibility, one is provided
Kind polyphenyl thioether material enhances special basalt fibre and preparation method thereof；Basalt fibre of the present invention is by special size
Obtained from processing in process of production, the basalt fibre since surface roughness is big and is grafted with a large amount of active groups,
Chemical bonding and mechanical riveted ability between basalt fibre and polyphenyl thioether material is strong, the basalt fibre and polyphenylene sulfide
The compatibility of material is good, largely can add and apply in polyphenyl thioether material.
In order to achieve the above-mentioned object of the invention, the present invention provides a kind of polyphenyl thioether materials to enhance special basalt fibre
Preparation method includes the following steps：
（1）Basalt ore is crushed into processing, obtains basalt ore powder；
（2）Step 1 is obtained into powder heating, melting forms spinning melt；
（3）The spinning melt that step 2 is obtained carries out wire drawing, obtains basalt fibre precursor；
（4）The basalt fibre precursor that step 3 obtains is subjected to infiltration modification with size；
（5）The precursor by infiltration modification that step 4 obtains move back and solves and twists, obtains polyphenyl thioether material
Enhance special basalt fibre.
A kind of above-mentioned polyphenyl thioether material enhances the preparation method of special basalt fibre, size packet described in step 4
Include following parts by weight of component：40-60 parts of film forming agent, 5-15 parts of coupling agent, 1-5 part lubricant, 10-20 parts of modifying agent,
30-50 parts of solvent；The size quickly can carry out burn into activation to basalt fibre surface, form rough surface, and connect
The a large amount of active groups of branch, to improve chemical bonding and the mechanical riveted ability between basalt fibre and polyphenyl thioether material,
Improve the compatibility of basalt fibre and polyphenyl thioether material；The mechanical riveted refers to that basis material passes through shrinkage stress packet
The fiber of tight rough surface and the frictional engagement generated.
Above-mentioned size, wherein the modifying agent includes sulphur acid salt ︰ sulphur acid ︰ phenolic compounds 3-6 ︰ 2-4 ︰ in mass ratio
The mixture that 1-3 is mixed；Preferably, the modifying agent includes 3 ︰ of Huang Suan Yan ︰ Liu Suan ︰ phenolic compounds 5 ︰ in mass ratio
2 mixtures mixed.
Above-mentioned size, wherein the sulfonate is one or more in sodium sulfonate, potassium sulfonate, sulfamic acid；Its
Described in phenolic compound be phenol, it is sodium phenate, cresols, amino phenols, one or more in nitrophenols；It is wherein described at
Film is one kind in ptfe emulsion, polyacrylate dispersion；Wherein the coupling agent is to contain sulfonate radical, ether
The modified silane coupler of one or more groups in base, carboxyl；Wherein the lubricant is methyl stearate and stearic acid
One kind in zinc.
Above-mentioned size, wherein the solvent is the aqueous solution of glycerine；The volume ratio of glycerine and water is in the solvent
1-3 ︰ 1；Preferably, the volume ratio of glycerine and water is 2 ︰ 1 in the aqueous solution of glycerine.
A kind of polyphenyl thioether material enhances the preparation method of special basalt fiber material, and the method for the present invention is by production process
In obtained intermediate product basalt fibre precursor handled with the size of special component, so that fiber surface roughness is increased
And a large amount of active groups are grafted, contribute to polyphenyl thioether material to carry out chemical bonding and mechanical riveted on basalt fibre surface,
To directly obtain and the good basalt fibre of polyphenyl thioether material compatibility；The basalt fibre can be in polyphenyl thioether material
In largely add and apply.
A kind of above-mentioned polyphenyl thioether material enhances the preparation method of special basalt fibre, wherein profound described in step 1
Military rock and ore diameter of particle is 0.1-2mm, and grain size is smaller, and speed is faster when heating melts, and energy consumption is lower, but crushes cost and increase
Preferably, the basalt ore diameter of particle is 0.5-1mm.
A kind of above-mentioned polyphenyl thioether material enhances the preparation method of special basalt fibre, wherein molten described in step 2
It is 1100-1500 DEG C to melt temperature, and temperature is too low, and melting speed is slow, and time-consuming, and energy consumption is high, and temperature is excessively high, high to equipment requirement,
Equipment cost increases；Preferably, the melting temperature is 1250-1350 DEG C.
A kind of above-mentioned polyphenyl thioether material enhances the preparation method of special basalt fibre, the wherein drawing described in step 3
The speed of silk is 1500-3000m/min, and drawing speed is too fast, and tensile stress is excessive, can cause fibrous fracture；Drawing speed mistake
Slowly, the basalt fibre obtained is relatively large in diameter, and is unfavorable for the application of basalt fibre.
A kind of above-mentioned polyphenyl thioether material enhances the preparation method of special basalt fibre, wherein profound described in step 3
For military rock fiber precursor diameter control at 3-20 μm, precursor diameter is excessive, cooling slow, causes stress distribution inside and outside fiber not only, fine
It is big to tie up defect, is unfavorable for practical application, precursor diameter is too small, and drawing process operating difficulties is easily broken off；Preferably, described
Basalt fibre precursor diameter control is at 5-10 μm.
A kind of above-mentioned polyphenyl thioether material enhances the preparation method of special basalt fibre, the wherein leaching described in step 4
Moisten the control of agent temperature at 50-80 DEG C, temperature is higher, and reaction speed is faster, and treatment effect is better, but temperature is excessively high, surface treatment
Extent control is difficult, unstable product quality；Preferably, the size temperature is controlled at 60-70 DEG C.
In order to achieve the above-mentioned object of the invention, further, the present invention provides a kind of enhancing of polyphenyl thioether material is special profound
Military rock fiber, the polyphenyl thioether material enhance special basalt fibre and are prepared by above-mentioned preparation method；Pass through
Obtained polyphenyl thioether material prepared by above-mentioned preparation method enhances special basalt fibre, and surface roughness is big and is grafted with big
Active group is measured, the chemical bonding and mechanical riveted ability between basalt fibre and polyphenyl thioether material are strong, with polyphenylene sulfide
The compatibility of material is good, largely can add and apply in polyphenyl thioether material.
Compared with prior art, beneficial effects of the present invention：
1, polyphenyl thioether material of the present invention enhances the preparation method of special basalt fibre, using size to basalt fibre
It ties up precursor and carries out quick modification, so that fiber surface roughness is increased and be grafted a large amount of active groups, contribute to polyphenylene sulfide
Material carries out chemical bonding and mechanical riveted on basalt fibre surface, improves phase of the basalt fibre with polyphenyl thioether material
Capacitive.
2, polyphenyl thioether material of the present invention enhances the preparation method of special basalt fibre, directly uses size to fiber
Precursor is modified processing, and the production of fiber and modification are combined into one, production stage is simplified, has saved production cost, contracts
The short production cycle.
3, polyphenyl thioether material of the present invention enhances special basalt fibre, and surface roughness is big and is grafted with a large amount of active groups
Group, the chemical bonding and mechanical riveted ability between basalt fibre and polyphenyl thioether material are strong, the phase with polyphenyl thioether material
Capacitive is good, largely can add and apply in polyphenyl thioether material.
Specific implementation mode
With reference to test example and specific implementation mode, the present invention is described in further detail.But this should not be understood
It is only limitted to embodiment below for the range of the above-mentioned theme of the present invention, it is all that this is belonged to based on the technology that the content of present invention is realized
The range of invention.
Embodiment 1
（1）Basalt ore is crushed into processing, obtains the basalt ore powder that grain size is 0.5mm；
（2）Step 1 is obtained into powder heating, is melted at a temperature of 1250 DEG C, forms spinning melt；
（3）The spinning melt that step 2 obtains is subjected to wire drawing under the speed of 2000m/min, obtains a diameter of 5 μm profound
Military rock fiber precursor；
（4）The basalt fibre precursor that step 3 obtains is subjected to infiltration processing in the size that temperature is 60 DEG C；Infiltration
Agent group becomes：15 parts by weight contain modifying agent that 3 ︰ 2 of Huang Suan Na ︰ Liu Suan ︰ phenol 5 ︰ in mass ratio mix, 50 parts by weight
Ptfe emulsion, the glycerine of 30 parts by weight, the water of 10 parts by weight, the silane coupling agent of 10 parts by weight and 3 parts by weight it is hard
Resin acid methyl esters；
（5）The precursor by infiltration processing that step 4 obtains move back and solves and twists, obtains polyphenyl thioether material enhancing
Special basalt fibre.
Embodiment 2
（1）Basalt ore is crushed into processing, obtains the basalt ore powder that grain size is 1.0mm；
（2）Step 1 is obtained into powder heating, is melted at a temperature of 1350 DEG C, forms spinning melt；
（3）The spinning melt that step 2 obtains is subjected to wire drawing under the speed of 2500m/min, obtains a diameter of 10 μm
Basalt fibre precursor；
（4）The basalt fibre precursor that step 3 obtains is subjected to infiltration processing in the size that temperature is 70 DEG C；Infiltration
Agent group becomes：10 parts by weight contain modifying agent, 60 parts by weight that 2 ︰ 1 of Huang Suan Jia ︰ Liu Suan ︰ nitrophenols 3 ︰ in mass ratio are mixed
Polyacrylate dispersion, the glycerine of 20 parts by weight, the water of 20 parts by weight, the silane coupling agent of 15 parts by weight and 1 parts by weight
Zinc stearate；
（5）The precursor by infiltration processing that step 4 obtains move back and solves and twists, obtains polyphenyl thioether material enhancing
Special basalt fibre.
Embodiment 3
（1）Basalt ore is crushed into processing, obtains the basalt ore powder that grain size is 0.1mm；
（2）Step 1 is obtained into powder heating, is melted at a temperature of 1100 DEG C, forms spinning melt；
（3）The spinning melt that step 2 obtains is subjected to wire drawing under the speed of 3000m/min, obtains a diameter of 3 μm profound
Military rock fiber precursor；
（4）The basalt fibre precursor that step 3 obtains is subjected to infiltration processing in the size that temperature is 80 DEG C；Infiltration
Agent group becomes：20 parts by weight contain modifying agent, 40 parts by weight that 3 ︰ of An base Huang Suan ︰ Liu Suan ︰ amino phenols mass ratioes, 4 ︰ 3 are mixed
Polyacrylate dispersion, the glycerine of 30 parts by weight, the water of 20 parts by weight, the silane coupling agent of 5 parts by weight and 5 parts by weight it is hard
Resin acid methyl esters；
（5）The precursor by infiltration processing that step 4 obtains move back and solves and twists, obtains polyphenyl thioether material enhancing
Special basalt fibre.
Embodiment 4
（1）Basalt ore is crushed into processing, obtains the basalt ore powder that grain size is 2mm；
（2）Step 1 is obtained into powder heating, is melted at a temperature of 1500 DEG C, forms spinning melt；
（3）The spinning melt that step 2 obtains is subjected to wire drawing under the speed of 1500m/min, obtains a diameter of 20 μm
Basalt fibre precursor；
（4）The basalt fibre precursor that step 3 obtains is subjected to infiltration processing in the size that temperature is 50 DEG C；Infiltration
Agent group becomes：10 parts by weight contain modifying agent that 2 ︰ 2 of Huang Suan Jia ︰ Liu Suan ︰ cresols 3 ︰ in mass ratio mix, 40 parts by weight
The tristearin of ptfe emulsion, the glycerine of 20 parts by weight, the water of 10 parts by weight, the silane coupling agent of 5 parts by weight and 5 parts by weight
Sour zinc；
（5）The precursor by infiltration processing that step 4 obtains move back and solves and twists, obtains polyphenyl thioether material enhancing
Special basalt fibre.
Comparative example 1
（1）Basalt ore is crushed into processing, obtains the basalt ore powder that grain size is 0.5mm；
（2）Step 1 is obtained into powder heating, is melted at a temperature of 1250 DEG C, forms spinning melt；
（3）The spinning melt that step 2 obtains is subjected to wire drawing under the speed of 2000m/min, obtains a diameter of 5 μm profound
Military rock fiber precursor；
（4）The basalt fibre precursor that step 3 obtains is subjected to infiltration processing in the size that temperature is 60 DEG C；Infiltration
Agent group becomes：The silane of the ptfe emulsion of 50 parts by weight, the glycerine of 30 parts by weight, the water of 10 parts by weight, 10 parts by weight
The methyl stearate of coupling agent and 3 parts by weight；
（5）The precursor by infiltration processing that step 4 obtains move back and solves and twists, obtains basalt fibre.
Comparative example 2
（1）Basalt ore is crushed into processing, obtains the basalt ore powder that grain size is 0.5mm；
（2）Step 1 is obtained into powder heating, is melted at a temperature of 1250 DEG C, forms spinning melt；
（3）The spinning melt that step 2 obtains is subjected to wire drawing under the speed of 2000m/min, obtains a diameter of 5 μm profound
Military rock fiber precursor；
（4）The basalt fibre precursor that step 3 obtains is subjected to infiltration processing in the size that temperature is 60 DEG C；Infiltration
Agent group becomes：15 parts by weight contain modifying agent that 6 ︰ 2 of Huang Suan Na ︰ Liu Suan ︰ phenol 5 ︰ in mass ratio mix, 50 parts by weight
Ptfe emulsion, the glycerine of 30 parts by weight, the water of 10 parts by weight, the silane coupling agent of 10 parts by weight and 3 parts by weight it is hard
Resin acid methyl esters；
（5）The precursor by infiltration processing that step 4 obtains move back and solves and twists, obtains polyphenyl thioether material enhancing
Special basalt fibre.
Comparative example 3
（1）Basalt ore is crushed into processing, obtains the basalt ore powder that grain size is 0.5mm；
（2）Step 1 is obtained into powder heating, is melted at a temperature of 1250 DEG C, forms spinning melt；
（3）The spinning melt that step 2 obtains is subjected to wire drawing under the speed of 2000m/min, obtains a diameter of 5 μm profound
Military rock fiber precursor；
（4）The basalt fibre precursor that step 3 obtains is subjected to infiltration processing in the size that temperature is 60 DEG C；Infiltration
Agent group becomes：15 parts by weight contain modifying agent that 3 ︰ 2 of Huang Suan Na ︰ Liu Suan ︰ phenol 1 ︰ in mass ratio mix, 50 parts by weight
Ptfe emulsion, the glycerine of 30 parts by weight, the water of 10 parts by weight, the silane coupling agent of 10 parts by weight and 3 parts by weight it is hard
Resin acid methyl esters；
（5）The precursor by infiltration processing that step 4 obtains move back and solves and twists, obtains polyphenyl thioether material enhancing
Special basalt fibre.
Preparation-obtained basalt fibre in above-described embodiment 1-4 and comparative example 1-3 is tested for the property and polyphenyl
Thioether plastics（Tensile strength 58MPa, notch impact strength 32J/m, elongation at break 26%）Enhancing（Basalt fibre dosage is
The 10% of polyphenylene sulfide quality）Experiment, records experimental result, and record data are as follows：
| Number | Tensile strength（MPa） | Elongation at break（%） | Modified polyphenylene sulfide plastic notch impact strength（J/m） | Modified polyphenylene sulfide plastic tensile strength（MPa） | Modified polyphenylene sulfide plastic elongation at break（%） |
| Embodiment 1 | 3800 | 2.6 | 74 | 83 | 47 |
| Embodiment 2 | 3810 | 2.4 | 72 | 81 | 48 |
| Embodiment 3 | 3820 | 2.5 | 73 | 82 | 46 |
| Embodiment 4 | 3840 | 2.5 | 72 | 83 | 47 |
| Comparative example 1 | 3840 | 2.7 | 48 | 72 | 34 |
| Comparative example 2 | 3350 | 1.6 | 51 | 68 | 28 |
| Comparative example 3 | 3620 | 2.3 | 53 | 70 | 31 |
To above-mentioned analysis of experimental data it is found that the basalt being prepared using technical solution of the present invention in embodiment 1-4
Fiber draws Shen intensity and elongation at break good, good with the compatibility of polyphenylene sulfide plastic, and poly-p-phenylene sulfide ether plastics enhancing effect is aobvious
It writes；And the size used in 1 preparation method of comparative example is conventional size, the basalt fibre surface being prepared is smooth,
Active group is few, weak with the chemical bonding of polyphenyl thioether material and mechanical riveted ability with polyphenyl thioether material poor compatibility, right
Polyphenyl thioether material humidification is obviously reduced；The size used in 2 preparation method of comparative example is protected in the present invention
Size component proportion dosage, sulfuric acid dosage is excessive, and size is to basalt fibre surface erosion transition, to basalt fibre
Structure damages, and causes the tensile strength of basalt fibre and elongation at break to significantly reduce, to poly-p-phenylene sulfide ether fiber
Humidification be also remarkably decreased；The size used in 3 preparation method of comparative example is not the size protected in the present invention
Component proportion dosage, sulfonate dosage is too small, and size weakens basalt fibre surface activation, basalt fibre surface
The active group of grafting is few, weak with the chemical bonding ability of polyphenyl thioether material, and the effect of poly-p-phenylene sulfide ether Material reinforcement significantly subtracts
It is weak.
Claims (5)
1. a kind of polyphenyl thioether material enhances the preparation method of special basalt fibre, which is characterized in that include the following steps：
（1）Basalt ore is crushed into processing, obtains basalt ore powder；
（2）Step 1 is obtained into powder heating, melting forms spinning melt；
（3）The spinning melt that step 2 is obtained carries out wire drawing, obtains basalt fibre precursor；
（4）The basalt fibre precursor that step 3 obtains is subjected to infiltration modification with size；
（5）The precursor by infiltration modification that step 4 obtains move back and solves and twists, obtains polyphenyl thioether material enhancing
Special basalt fibre；
The size includes following parts by weight of component：40-60 parts of film forming agent, 5-15 parts of coupling agent, 1-5 part lubricant,
10-20 parts of modifying agent, 30-50 parts of solvent；Modifying agent includes sulfonate, sulfuric acid, the phenols that mass ratio is 3-6 ︰ 2-4 ︰ 1-3
Compound；
The sulfonate is one or more in sodium sulfonate, potassium sulfonate, sulfamic acid；The phenolic compound is phenol, benzene
It is one or more in phenol sodium, cresols, amino phenols, nitrophenols；The film forming agent is ptfe emulsion, polyacrylate breast
One kind in liquid；The coupling agent is the modified silane coupler containing one or more groups in sulfonate radical, ether, carboxyl；
The solvent is the aqueous solution of glycerine.
2. preparation method according to claim 1, which is characterized in that melting temperature control is in 1100-1500 in step 2
℃。
3. preparation method according to claim 1, which is characterized in that basalt fibre precursor diameter control exists in step 3
3-20μm。
4. preparation method according to claim 1, which is characterized in that the control of size temperature is at 50-80 DEG C in step 4.
5. a kind of polyphenyl thioether material enhances special basalt fibre, which is characterized in that be by any one of claim 1-4 institutes
What the preparation method stated was prepared.
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| CN109320962A (en) * | 2018-09-13 | 2019-02-12 | 丹阳市三能电器配件有限公司 | PPS composite material and preparation method for air-conditioning supplementary heating element bracket |
| CN108975731A (en) * | 2018-09-20 | 2018-12-11 | 黄勇 | A kind of preparation method of glass fiber infiltration agent |
| CN112934161A (en) * | 2021-01-28 | 2021-06-11 | 嘉兴京能科技有限责任公司 | Modified corrosion-resistant PEEK filler material for rectifying tower and production method and application thereof |
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