CN106751560A - A kind of polybutylene terephthalate (PBT) Material reinforcement basalt fibre sizing agent special and preparation method thereof - Google Patents
A kind of polybutylene terephthalate (PBT) Material reinforcement basalt fibre sizing agent special and preparation method thereof Download PDFInfo
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- CN106751560A CN106751560A CN201611072796.7A CN201611072796A CN106751560A CN 106751560 A CN106751560 A CN 106751560A CN 201611072796 A CN201611072796 A CN 201611072796A CN 106751560 A CN106751560 A CN 106751560A
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- 229920001707 polybutylene terephthalate Polymers 0.000 title claims abstract description 137
- -1 polybutylene terephthalate Polymers 0.000 title claims abstract description 88
- 229920002748 Basalt fiber Polymers 0.000 title claims abstract description 75
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 72
- 239000000463 material Substances 0.000 title claims abstract description 72
- 230000002787 reinforcement Effects 0.000 title claims abstract description 36
- 238000004513 sizing Methods 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 239000007822 coupling agent Substances 0.000 claims abstract description 9
- 239000000314 lubricant Substances 0.000 claims abstract description 9
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical class O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 claims abstract 4
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims abstract 3
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims abstract 3
- 239000011259 mixed solution Substances 0.000 claims description 44
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 34
- HPEUJPJOZXNMSJ-UHFFFAOYSA-N Methyl stearate Chemical group CCCCCCCCCCCCCCCCCC(=O)OC HPEUJPJOZXNMSJ-UHFFFAOYSA-N 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- CAMHHLOGFDZBBG-UHFFFAOYSA-N epoxidized methyl oleate Natural products CCCCCCCCC1OC1CCCCCCCC(=O)OC CAMHHLOGFDZBBG-UHFFFAOYSA-N 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- 125000004185 ester group Chemical group 0.000 claims description 3
- 229920000058 polyacrylate Polymers 0.000 claims description 3
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 2
- 150000004756 silanes Chemical class 0.000 claims description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims 3
- VKEQBMCRQDSRET-UHFFFAOYSA-N Methylone Chemical compound CNC(C)C(=O)C1=CC=C2OCOC2=C1 VKEQBMCRQDSRET-UHFFFAOYSA-N 0.000 claims 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical group [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 1
- 235000010290 biphenyl Nutrition 0.000 claims 1
- 239000004305 biphenyl Substances 0.000 claims 1
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims 1
- 239000011574 phosphorus Substances 0.000 claims 1
- 229910052698 phosphorus Inorganic materials 0.000 claims 1
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 claims 1
- 239000000835 fiber Substances 0.000 abstract description 22
- 239000000126 substance Substances 0.000 abstract description 8
- 230000008595 infiltration Effects 0.000 abstract description 5
- 238000001764 infiltration Methods 0.000 abstract description 5
- 230000003746 surface roughness Effects 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 12
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 8
- 239000002253 acid Substances 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 8
- 239000011734 sodium Substances 0.000 description 8
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 7
- 229910000077 silane Inorganic materials 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 230000002708 enhancing effect Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000000839 emulsion Substances 0.000 description 5
- 150000002689 maleic acids Chemical class 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 150000002148 esters Chemical class 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000004033 plastic Substances 0.000 description 4
- 229920003023 plastic Polymers 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000007380 fibre production Methods 0.000 description 3
- 239000003365 glass fiber Substances 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- 229920001155 polypropylene Polymers 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000002657 fibrous material Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000003607 modifier Substances 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- RYDFXSRVZBYYJV-ODZAUARKSA-N (z)-but-2-enedioic acid;sodium Chemical compound [Na].OC(=O)\C=C/C(O)=O RYDFXSRVZBYYJV-ODZAUARKSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 241001163600 Bathylaco nigricans Species 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 125000005396 acrylic acid ester group Chemical group 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 229920006253 high performance fiber Polymers 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920000874 polytetramethylene terephthalate Polymers 0.000 description 1
- QPMDWIOUHQWKHV-TYYBGVCCSA-M potassium;(e)-but-2-enedioate;hydron Chemical compound [H+].[K+].[O-]C(=O)\C=C\C([O-])=O QPMDWIOUHQWKHV-TYYBGVCCSA-M 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- KUCOHFSKRZZVRO-UHFFFAOYSA-N terephthalaldehyde Chemical compound O=CC1=CC=C(C=O)C=C1 KUCOHFSKRZZVRO-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/10—Silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a kind of polybutylene terephthalate (PBT) Material reinforcement basalt fibre sizing agent special and preparation method thereof, size of the present invention includes 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 solvents；The modifying agent includes the hypophosphites that mass ratio is the ︰ 46 of 24 ︰ 13, highly basic, maleate；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 the chemical bonding between basalt fibre and polybutylene terephthalate (PBT) material and mechanical riveted ability, the compatibility of basalt fibre and polybutylene terephthalate (PBT) material is improve, popularization and application of the basalt fibre in polybutylene terephthalate (PBT) Material reinforcement field are promoted.
Description
Technical field
The present invention relates to basalt fibre size field, and in particular to a kind of polybutylene terephthalate (PBT) material increases
Strong basalt fibre sizing agent special 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 from after high-temperature fusion by spinning technique.Basalt continuous fiber is not only stablized
Property is good, but also with various excellent properties such as electrical insulating property, anticorrosive, flame resistant, high temperature resistant, and, basalt fibre
The discarded object that production technology is produced is few, and environmental pollution is small, directly can be 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 been obtained extensively
Application.
Polybutylene terephthalate (PBT) (abbreviation PBT）Also known as polytetramethylene terephthalate, it is by benzene two
The polyester that formic acid and BDO polycondensation are made.One of most important thermoplastic polyester, five large-engineering plastics, with heat resistance
The advantages of good, good toughness, endurance, self-lubricating, low-friction coefficient；But because ester group is active in polybutylene terephthalate (PBT)
Property it is good, cause polybutylene terephthalate (PBT) material exist intolerant to strong acid, highly basic, it is flammable, under high temperature decompose defect, because
This, it is many when in use not use pure polybutylene terephthalate (PBT) material, polybutylene terephthalate (PBT) material needs
Can just be applied after carrying out the composite modified treatment of enhancing such as fire-retardant, corrosion-resistant, high temperature resistant.Now to poly terephthalic acid fourth two
The fiber-reinforced modified main use glass fiber material of alcohol ester material is modified treatment, and modified effect is notable, but glass fibers
Dimension production cost is high, environmental pollution is big, seriously limits the application of compound polybutylene terephthalate (PBT) material, and exploitation is a kind of
With low cost, environmental protection, the new fiber materials of excellent performance substitute glass fibre to polybutylene terephthalate (PBT) material
The problem that material is modified treatment is badly in need of being resolved.Therefore, it is possible to, it is envisioned that nontoxic, pollution-free, wide material sources, performance is excellent
The enhancing that basalt fibre that is different, having stablized is used for polybutylene terephthalate (PBT) material will improve poly- to benzene two from now on
The new trend of formic acid butanediol ester material property.But due to existing basalt fibre self structure and stable performance, fiber surface
Smooth, surface-active site is few, causes basalt fibre to be difficult in modifying process and polybutylene terephthalate (PBT) material
Chemical bonding and mechanical riveted form the entirety of unified stabilization, i.e., basalt fibre is in polybutylene terephthalate (PBT) material
It is to be individually present in material, the modified humidification to polybutylene terephthalate (PBT) material is relatively weak, enhancing effect is not very
Ideal, 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 which fiber surface is chemically treated, increase fiber feature, therefore, using leaching
Profit agent is modified treatment to fibrous material, will fiber production and it is modified unite two into one, section simplifies production stage, saving
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
Basalt fibre high is feasible with the compatibility of polybutylene terephthalate (PBT) material, may advantageously facilitate basalt fibre and exists
Popularization and application in polybutylene terephthalate (PBT) Material reinforcement field.
The content of the invention
It is an object of the invention to overcome existing basalt fibre size to improve basalt fibre with poly- to benzene two
The defect of formic acid butanediol ester material compatibility, there is provided a kind of polybutylene terephthalate (PBT) strengthens the special leaching of basalt fibre
Profit agent and preparation method thereof；Contain modifying agent in size of the present invention, fiber surface is entered while infiltration by modifying agent
Row is modified, increases fiber surface roughness and is grafted a large amount of active groups, so as to improve basalt fibre with poly- terephthaldehyde
Chemical bonding and mechanical riveted ability between sour butanediol ester material, improve basalt fibre and poly terephthalic acid fourth two
The compatibility of alcohol ester material, promoting popularization of the basalt fibre in polybutylene terephthalate (PBT) Material reinforcement field should
With.
In order to realize foregoing invention purpose, the invention provides a kind of polybutylene terephthalate (PBT) Material reinforcement Black Warrior
Rock fiber sizing agent special, including following parts by weight of component：40-60 parts of film forming agent, 5-15 parts of coupling agent, 1-5 parts of lubrication
Agent, 10-20 parts of modifying agent, 30-50 parts of solvent.
Above-mentioned a kind of polybutylene terephthalate (PBT) Material reinforcement basalt fibre sizing agent special, wherein described changes
Property agent include the Ci Lin Suan Yan ︰ Qiang Jian ︰ maleate mixtures that 2-4 ︰ 1-3 ︰ 4-6 are mixed in mass ratio；It is described to change
Property agent composition can quickly to basalt fibre surface corrosion, activation, formation rough surface and be grafted a large amount of active groups, make fibre
Dimension table face forms a large amount of avtive spots and active group, so that basalt fibre can be carried out with polybutylene terephthalate (PBT)
Chemical bonding and mechanical riveted；Described mechanical riveted refer to matrix material by shrinkage stress pack tightly rough surface fiber and
The frictional engagement of generation；Preferably, described modifying agent includes the ︰ 5 of Ci Lin Suan Yan ︰ Qiang Jian ︰ maleates 3 ︰ in mass ratio 2
The mixture for mixing.
Above-mentioned a kind of polybutylene terephthalate (PBT) Material reinforcement basalt fibre sizing agent special, wherein described is secondary
Phosphate is dimethyl hypophosphites, ethylmethylphosphiniacid acid salt, methyl n-propyl hypophosphites, dimethylamino methane base hypophosphorous acid
One or more of salt, benzene-Isosorbide-5-Nitrae-dimethyl hypophosphites, aminomethyl phenyl hypophosphites or diphenyl hypophosphites.
Above-mentioned a kind of polybutylene terephthalate (PBT) Material reinforcement basalt fibre sizing agent special, wherein described is strong
Alkali be NaOH, potassium hydroxide in one or two.
A kind of polybutylene terephthalate (PBT) Material reinforcement basalt fibre sizing agent special is stated, wherein described suitable fourth
Enedioic acid salt be maleic acid sodium, maleic acid potassium in one or two.
A kind of polybutylene terephthalate (PBT) Material reinforcement basalt fibre sizing agent special, each component in modifying agent
Collective effect under, with quickly forming rough surface to basalt fibre surface corrosion and be grafted a large amount of energy in fiber surface
With the effect of the active group of polybutylene terephthalate (PBT) chemical bonding so that basalt fibre pass through the size
Treatment after, not only with more preferable toughness and lubricity, be conducive to the post-production of basalt fibre, moreover it is possible to improve basalt
Fiber carries out the ability of chemical bonding and mechanical riveted with polybutylene terephthalate (PBT), that is, improve basalt fibre and gather
The compatibility of mutual-phenenyl two acid bromide two alcohol ester；Size of the present invention promotes basalt fibre in polybutylene terephthalate (PBT)
Extensive use in Material reinforcement field.
A kind of above-mentioned polybutylene terephthalate (PBT) Material reinforcement basalt fibre sizing agent special, wherein it is described into
Film is polyacrylate dispersion；Film forming agent can form membrane structure on basalt fibre surface well, increase basalt fibre
Toughness, and the compatibility of basalt fibre and polybutylene terephthalate (PBT) material can be improved.
Above-mentioned a kind of polybutylene terephthalate (PBT) Material reinforcement basalt fibre sizing agent special, wherein described idol
Connection agent is to contain one or more modified silane coupler of group in ester group, alkyl, carboxyl；The silane coupler can with it is profound
Silicon atom coupling, can be coupled with polybutylene terephthalate (PBT) material again in military rock fiber, and coupling effect is best.
Above-mentioned a kind of polybutylene terephthalate (PBT) Material reinforcement basalt fibre sizing agent special, wherein described profit
Lubrication prescription is the one kind in methyl stearate and zinc stearate.
Above-mentioned a kind of polybutylene terephthalate (PBT) Material reinforcement basalt fibre sizing agent special, wherein described is molten
Agent is the aqueous solution of ethanol；Ethanol and the volume ratio of water are 1-3 ︰ 1 in the aqueous solution of the ethanol；Preferably, ethanol is water-soluble
Ethanol and the volume ratio of water are 2 ︰ 1 in liquid.
Preferably, a kind of polybutylene terephthalate (PBT) Material reinforcement basalt fibre sizing agent special, including it is following
Parts by weight of component：50 parts of film forming agent, 10 parts of coupling agent, 3 parts of lubricants, 15 parts of modifying agent, 40 parts of solvents.
In order to realize foregoing invention purpose, further, the invention provides a kind of polybutylene terephthalate (PBT) material
The preparation method of material enhancing basalt fibre sizing agent special, comprises the following steps：
（1）Modifying agent solvent is dissolved to form mixed solution A；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 is added to be well mixed in mixed solution B and forms mixed solution C；
（3）The mixed solution C defoaming treatment that step 2 is obtained obtains polybutylene terephthalate (PBT) Material reinforcement basalt fibre
Sizing agent special.
A kind of preparation method of above-mentioned polybutylene terephthalate (PBT) Material reinforcement basalt fibre sizing agent special, its
Defoaming treatment described in middle step 3 is physical defoaming；Avoid the generation of introducing or the side reaction of impurity.
A kind of preparation method of polybutylene terephthalate (PBT) Material reinforcement basalt fibre sizing agent special, will be modified
The dilution dissolving of agent is separately processed with the mixed dissolution of film forming agent, coupling agent, lubricant, it is to avoid modifying agent is put when dissolving is diluted
The a large amount of thermal conductivities for going out cause the generation of side reaction, and production orderliness is clear, succinct；The inventive method is simple, reliable, is adapted to poly- to benzene
Extensive, the industrialized production of dioctyl phthalate butanediol ester Material reinforcement basalt fibre sizing agent special.
Compared with prior art, beneficial effects of the present invention：
1st, polybutylene terephthalate (PBT) Material reinforcement basalt fibre sizing agent special of the present invention can be quickly fine to basalt
Dimension surface corrosion, forms rough surface, improves the machinery between basalt fibre and polybutylene terephthalate (PBT) material
Riveted ability.
2nd, polybutylene terephthalate (PBT) Material reinforcement basalt fibre sizing agent special infiltration of the present invention can quickly exist
Fiber surface grafting largely can with the active group of polybutylene terephthalate (PBT) chemical bonding, improve basalt fibre with
Chemical bonding ability between polybutylene terephthalate (PBT) material.
3rd, polybutylene terephthalate (PBT) Material reinforcement basalt fibre sizing agent special of the present invention can improve basalt
Compatibility between fiber and polybutylene terephthalate (PBT) material, promotes basalt fibre in poly terephthalic acid fourth two
Extensive use in alcohol ester Material reinforcement field.
4th, the preparation method letter of polybutylene terephthalate (PBT) Material reinforcement basalt fibre sizing agent special of the present invention
It is single, reliable, it is adapted to extensive, the industrial metaplasia of polybutylene terephthalate (PBT) Material reinforcement basalt fibre sizing agent special
Produce.
Specific embodiment
With reference to test example and specific embodiment, the present invention is described in further detail.But this should not be understood
For the scope of above-mentioned theme of the invention is only limitted to following embodiment, all technologies realized based on present invention belong to this
The scope of invention.
Embodiment 1
（1）By 15 weight portions contain the ︰ 5 of dimethyl Ci Lin Suan Na ︰ Qing Yangization Na ︰ maleic acids sodium 3 ︰ in mass ratio 2 mix and
Into modifying agent form mixed solution A with the water dissolves of the ethanol of 10 weight portions and 10 weight portions；By the polypropylene of 50 weight portions
The acid esters emulsion silane coupler and 3 weight portions that 10 weight portions are added after the ethanol of 10 weight portions and the water dissolves of 10 weight portions
Methyl stearate form mixed solution B；
（2）The mixed solution A that step 1 is obtained is added to be well mixed in mixed solution B and forms mixed solution C；
（3）The mixed solution C defoaming treatment that step 2 is obtained obtains polybutylene terephthalate (PBT) Material reinforcement basalt fibre
Sizing agent special.
Embodiment 2
（1）10 weight portions are contained into benzene-Isosorbide-5-Nitrae-︰ 6 of dimethyl hypophosphorous acid Jia ︰ Qing Yangization Jia ︰ maleic acids potassium 4 ︰ in mass ratio 3
The modifying agent for mixing forms mixed solution A with the ethanol of 5 weight portions and the water dissolves of 5 weight portions；By the poly- of 60 weight portions
Acrylic acid ester emulsion adds the silane coupled of 15 weight portions after being dissolved with the solvent of the water of the ethanol and 10 weight portions of 20 weight portions
The zinc stearate of agent and 1 weight portion forms mixed solution B；
（2）The mixed solution A that step 1 is obtained is added to be well mixed in mixed solution B and forms mixed solution C；
（3）The mixed solution C defoaming treatment that step 2 is obtained obtains polybutylene terephthalate (PBT) Material reinforcement basalt fibre
Sizing agent special.
Embodiment 3
（1）20 weight portions are contained into the ︰ 4 of ethylmethylphosphiniacid acid Na ︰ Qing Yangization Na ︰ maleic acids potassium 2 ︰ in mass ratio 1 to mix
Modifying agent form mixed solution A with the water dissolves of the ethanol of 10 weight portions and 10 weight portions；By poly- the third of 40 weight portions
The olefin(e) acid ester emulsion silane coupler and 5 weight that 5 weight portions are added after the ethanol of 20 weight portions and the water dissolves of 10 weight portions
The methyl stearate of part forms mixed solution B；
（2）The mixed solution A that step 1 is obtained is added to be well mixed in mixed solution B and forms mixed solution C；
（3）The mixed solution C defoaming treatment that step 2 is obtained obtains polybutylene terephthalate (PBT) Material reinforcement basalt fibre
Sizing agent special.
Comparative example 1
（1）By the polyacrylate dispersion of 50 weight portions with adding 10 weights after the ethanol of 20 weight portions and the water dissolves of 20 weight portions
The methyl stearate of the silane coupler and 3 weight portions of measuring part forms mixed solution；
（2）The mixed solution defoaming treatment that step 1 is obtained obtains size.
Comparative example 2
（1）By 15 weight portions contain the ︰ 5 of dimethyl Ci Lin Suan Na ︰ Qing Yangization Na ︰ maleic acids sodium 3 ︰ in mass ratio 5 mix and
Into modifying agent form mixed solution A with the water dissolves of the ethanol of 10 weight portions and 10 weight portions；By the polypropylene of 50 weight portions
The acid esters emulsion silane coupler and 3 weight portions that 10 weight portions are added after the ethanol of 10 weight portions and the water dissolves of 10 weight portions
Methyl stearate form mixed solution B；
（2）The mixed solution A that step 1 is obtained is added to be well mixed in mixed solution B and forms mixed solution C；
（3）The mixed solution C defoaming treatment that step 2 is obtained obtains polybutylene terephthalate (PBT) Material reinforcement basalt fibre
Sizing agent special.
Comparative example 3
（1）By 15 weight portions contain the ︰ 5 of dimethyl Ci Lin Suan Na ︰ Qing Yangization Na ︰ maleic acids sodium 5 ︰ in mass ratio 2 mix and
Into modifying agent form mixed solution A with the water dissolves of the ethanol of 10 weight portions and 10 weight portions；By the polypropylene of 50 weight portions
The acid esters emulsion silane coupler and 3 weight portions that 10 weight portions are added after the ethanol of 10 weight portions and the water dissolves of 10 weight portions
Methyl stearate form mixed solution B；
（2）The mixed solution A that step 1 is obtained is added to be well mixed in mixed solution B and forms mixed solution C；
（3）The mixed solution C defoaming treatment that step 2 is obtained obtains polybutylene terephthalate (PBT) Material reinforcement 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, the basalt fibre that will be obtained carries out performance test and polybutylene terephthalate (PBT) plastics（Tensile strength 78MPa,
Notch impact strength 60J/m, 58 DEG C of heat distortion temperature）Enhancing（Basalt fibre consumption is polybutylene terephthalate (PBT) matter
The 30% of amount）Experiment, records experimental result, and record data is as follows：
| Numbering | Tensile strength （MPa） | Elongation at break （%） | Modified polybutylene terephthalate (PBT) plastics notch shock Intensity（J/m） | Modified polybutylene terephthalate (PBT) plastic tensile is strong Degree（MPa） | Modified polybutylene terephthalate (PBT) heat deformations temperature Degree（℃） |
| Implement Example 1 | 3600 | 2.6 | 123 | 151 | 246 |
| Implement Example 2 | 3610 | 2.4 | 120 | 148 | 245 |
| Implement Example 3 | 3620 | 2.5 | 119 | 150 | 245 |
| Contrast Example 1 | 3740 | 2.7 | 94 | 106 | 224 |
| Contrast Example 2 | 3250 | 1.6 | 86 | 116 | 228 |
| Contrast Example 3 | 3520 | 2.3 | 85 | 109 | 233 |
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 treatment, and the basalt fibre for obtaining draws Shen intensity and elongation at break good, with polybutylene terephthalate (PBT)
Compatibility is good, notable to polybutylene terephthalate (PBT) plastics enhancing effect；And size does not add modified in comparative example 1
Agent, as conventional size, the basalt fibre after being processed with the size is conventional basalt fibre, the basalt fibre with
Poor compatibility between polybutylene terephthalate (PBT) material is notable to the effect of polybutylene terephthalate (PBT) Material reinforcement
Weaken；Do not have in comparative example 2 using the modifier components proportioning consumption protected in the present invention, sodium hydroxide concentration is excessive, leaching
Profit agent is damaged to basalt fibre surface erosion transition to basalt fiber construction, causes the stretching of basalt fibre strong
Degree and elongation at break are significantly reduced, so as to the humidification to polybutylene terephthalate (PBT) fiber is also remarkably decreased；It is right
Do not have in ratio 3 using the modifier components proportioning consumption protected in the present invention, dimethyl sodium hypophosphite consumption is excessive, infiltration
Agent weakens to basalt fibre surface activation, and the active group of basalt fibre surface grafting is few, with poly terephthalic acid
The chemical bonding ability of butanediol ester material, is obviously reduced to the effect of polybutylene terephthalate (PBT) Material reinforcement.
Claims (10)
1. a kind of polybutylene terephthalate (PBT) Material reinforcement basalt fibre sizing agent special, it is characterised in that including with
Lower parts by weight of component：40-60 parts of film forming agent, 5-15 parts of coupling agent, 1-5 parts of lubricant, 10-20 parts of modifying agent, 30-50
The solvent of part；The modifying agent includes that mass ratio is the hypophosphites of 2-4 ︰ 1-3 ︰ 4-6, highly basic, maleate.
2. size according to claim 1, it is characterised in that the modifying agent includes secondary phosphorus that mass ratio is the ︰ 5 of 3 ︰ 2
Hydrochlorate, highly basic, maleate.
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
Coupling agent, 3 parts of lubricants, 15 parts of modifying agent, 40 parts of solvents 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
One or more of phenyl hypophosphites or diphenyl hypophosphites.
5. size according to claim 1, it is characterised in that the highly basic is in NaOH, potassium hydroxide
Plant or two kinds.
6. size according to claim 1, it is characterised in that the film forming agent is polyacrylate dispersion.
7. size according to claim 1, it is characterised in that the coupling agent is containing in ester group, alkyl, carboxyl
The modified silane coupler of kind or various groups.
8. size according to claim 1, it is characterised in that during the lubricant is 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 system of polybutylene terephthalate (PBT) Material reinforcement basalt fibre sizing agent special described in a kind of claim 1
Preparation Method, it is characterised in that comprise the following steps：
（1）Modifying agent solvent is dissolved to form mixed solution A；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 is added to be well mixed in mixed solution B and forms mixed solution C；
（3）The mixed solution C defoaming treatment that step 2 is obtained obtains polybutylene terephthalate (PBT) Material reinforcement basalt fibre
Sizing agent special.
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| CN201611072796.7A CN106751560A (en) | 2016-11-29 | 2016-11-29 | A kind of polybutylene terephthalate (PBT) Material reinforcement basalt fibre sizing agent special and preparation method thereof |
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| CN201611072796.7A CN106751560A (en) | 2016-11-29 | 2016-11-29 | A kind of polybutylene terephthalate (PBT) Material reinforcement basalt fibre sizing agent special and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN119410180A (en) * | 2025-01-06 | 2025-02-11 | 四川省工业环境监测研究院 | A phosphate-based anticorrosive coating |
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