CN106700102A - Polyphenylene sulfide reinforced composite material and preparing method thereof - Google Patents
Polyphenylene sulfide reinforced composite material and preparing method thereof Download PDFInfo
- Publication number
- CN106700102A CN106700102A CN201611139169.0A CN201611139169A CN106700102A CN 106700102 A CN106700102 A CN 106700102A CN 201611139169 A CN201611139169 A CN 201611139169A CN 106700102 A CN106700102 A CN 106700102A
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- polyphenylene sulfide
- preparation
- composite
- basalt fibre
- basalt
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/54—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
- 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
- C08K9/02—Ingredients treated with inorganic 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
-
- 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
- C08K9/10—Encapsulated ingredients
-
- 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
- C08J2381/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen, or carbon only; Polysulfones; Derivatives of such polymers
- C08J2381/02—Polythioethers; Polythioether-ethers
Abstract
The invention discloses a polyphenylene sulfide reinforced composite material and a preparing method thereof. The preparing method comprises the steps of conducting modified treatment and recombination on basalt fiber. By conducting modified treatment on the basalt fiber containing phosphoric acid, and finally conducting coupling and recombination on the modified basalt fiber and polyphenylene sulfide under the action of a coupling agent, the polyphenylene sulfide reinforced composite material with better compatibility of basalt fiber and the polyphenylene sulfide material is obtained. The basalt fiber plays a better role in reinforcing polyphenylene sulfide so that the composite material can have greater performance, and thus the preparing method thereof is beneficial to application and popularization of the polyphenylene sulfide reinforced composite material in various fields.
Description
Technical field
The present invention relates to polyphenyl thioether composite material field, and in particular to a kind of polyphenylene sulfide strengthens composite and its system
Preparation Method.
Background technology
Polyphenylene sulfide English is abbreviated as PPS, is a kind of novel high-performance thermoplastic resin, with high mechanical strength, resistance to height
Temperature, chemical proofing, fire retardant, heat endurance are good, excellent electrical properties the advantages of;But because polyphenylene sulfide crystallinity is high, cause
There is the low defect of poor toughness, impact strength in polyphenyl thioether material, therefore, do not use pure polyphenylene sulfide material when in use
Material, polyphenyl thioether material needs just be applied after carrying out the composite modified treatment of enhancing such as toughness reinforcing, increase 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 treatment, change
Property effect is significant, but glass fibre and carbon fiber production cost is high, environmental pollution big seriously limits composite polyphenylene sulfide material
Application.
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.
Therefore, glass is substituted using nontoxic, pollution-free, wide material sources, excellent performance, the basalt fiber material stablized
Glass fiber and carbon fiber poly-p-phenylene sulfide ether material are strengthened, and polyphenylene sulfide enhancing composite is polyphenylene sulfide obtained from
The new direction of enhancing composite development.But because basalt fibre is inorganic material, and polyphenylene sulfide is the organic material of macromolecule
Material, both compatibility extreme differences, and basalt fibre self structure and stable performance, fiber surface is smooth, surface-active site is few,
Basalt fibre is caused to be more difficult to carry out chemical bonding and mechanical riveted, i.e. basalt with polyphenyl thioether material in modifying process
Fiber is to be individually present in polyphenyl thioether material, poly-p-phenylene sulfide ether Material reinforcement effect on driving birds is not good, polyphenylene sulfide enhancing composite wood
The poor-performing of material.
The content of the invention
It is an object of the invention to overcome polyphenylene sulfide to strengthen the defect of composite property difference, there is provided a kind of polyphenylene sulfide
Enhancing composite and preparation method thereof;The inventive method is modified treatment by the basalt fibre containing barium phosphate,
Finally it is coupled with polyphenylene sulfide in the presence of coupling agent, is combined, so as to obtains basalt fibre and polyphenyl thioether material
The more preferable polyphenyl thioether composite material of compatibility, basalt fibre poly-p-phenylene sulfide ether humidification more preferably, makes the composite
Can be more excellent, be conducive to polyphenyl thioether composite material in the popularization and application of every field.
In order to realize foregoing invention purpose, the invention provides the preparation method that a kind of polyphenylene sulfide strengthens composite,
Comprise the following steps:
(1)Modification:Basalt fibre is carried out into immersion treatment with modifier A, is inserted after taking-up in modifying agent B, heating is anti-
Should completely after, take out dry treated basalt fiber;
(2)It is compound:Treated basalt fiber and polyphenyl thioether material, coupling agent are carried out into Combined Processing, polyphenylene sulfide increasing is obtained
Strong composite.
A kind of above-mentioned polyphenylene sulfide strengthens the preparation method of composite, short including basalt wherein described in step 1
One or more in fiber, basalt long fiber, continuous basalt fiber, basalt fiber cotton.
Contain barium phosphate in described basalt fibre;Contain the key of phosphate radical, phosphate radical and organic group in barium phosphate
Connect ability strong, the polarity of basalt fibre and organic material can be reduced, increase the compatibility with organic material;Preferably, it is described
Basalt fibre contain the barium phosphate of mass percent 0.1-2.0%;Most preferably, described basalt fibre contains quality
The barium phosphate of percentage 0.3-0.8%.
Described modifier A is the benzole soln of diphenyl disulfide.
Described modifying agent B is the mixed solution of lewis acid and inorganic acid;Preferably, the lewis acid is chlorination
One or more in aluminium, iron chloride, boron trifluoride;The inorganic acid is the one kind or many in sulfuric acid, hydrochloric acid, phosphoric acid, nitric acid
Kind;The pH value of described modifying agent B is 1-4, and solution acidic is higher, and the modified effect to basalt fibre is better.
The time that described basalt fibre soaks in modifier A is 1-3h, in immersion process, the hexichol in solution
Disulfide is uniformly adhered to basalt fibre surface under the adsorption effect of basalt fibre, and soak time is too short, inhales
The coupon scale of construction is not enough, and long soaking time, the production cycle is oversize, and effect is also without being obviously improved.
The temperature of the heating response is 50-80 DEG C, and the reaction time is 5-20min, and temperature is too high, and the reaction time is long,
Excessively, polymer molecular weight is excessive, is unfavorable for the modification to basalt fibre for polycondensation reaction;Most preferably, the heating
The temperature of reaction is 60 DEG C, and the reaction time is 10min, and reaction effect is good, and energy resource consumption is low, and the time is short.
A kind of above-mentioned polyphenylene sulfide strengthens the preparation method of composite, and the coupling agent wherein described in step 2 is silane
Coupling agent.
The consumption of the treated basalt fiber can strengthen composite according to polyphenylene sulfide will in different application field
Ask and be adjusted, it is preferred that the treated basalt fiber consumption is the 1-20% of polyphenylene sulfide material.
In the preparation method step 2 of the polyphenylene sulfide enhancing composite, auxiliary agent can also be added;The auxiliary agent includes
One or more in dispersant, antiseptic, antistatic additive, fire retardant, age resister, UV resistant agent;The kind of the auxiliary agent
Class can strengthen composite and require to carry out specific aim adjustment addition in different application field according to polyphenylene sulfide.
Described Combined Processing refers to that will pre-process basalt fibre and polyphenyl thioether material by process meanses
Bonding is learned, basalt fibre is formed unified overall method with polyphenyl thioether material.
A kind of polyphenylene sulfide strengthens the preparation method of composite, preparation method of the present invention first with basalt fibre table
Face adsorption capacity adsorbs on basalt fibre surface diphenyl disulfide monomer material, then the monomer that will be adsorbed by polycondensation reaction
Aggregate into the polymer of certain molecular weight, and make it bonded with the barium phosphate on basalt fibre surface, so that the bag of stabilization
Basalt fibre surface is overlayed on, the compatibility of basalt fibre and polyphenylene sulfide is dramatically increased;Finally by Combined Processing, make profound
Military rock fiber carries out composite strengthening and obtains the more excellent polyphenylene sulfide enhancing composite of performance, present invention side with polyphenylene sulfide
Method is simple, convenient, and being adapted to polyphenylene sulfide strengthens industrialization, the large-scale production of composite.
In order to realize foregoing invention purpose, further, the invention provides a kind of polyphenylene sulfide enhancing composite;Institute
State polyphenylene sulfide enhancing composite to be prepared by above-mentioned preparation method, the composite that above-mentioned preparation method is obtained
Bonded power is strong between middle polyphenylene sulfide and basalt fibre, is not likely to produce phase separation, and compatibility is good, basalt fiber poly-p-phenylene sulfide ether
Humidification dramatically increase, the performance of composite is also significantly improved.
Compared with prior art, beneficial effects of the present invention:
1st, preparation method of the present invention can dramatically increase basalt fibre and polyphenylene sulfide by the modification to basalt fibre
Compatibility, basalt fibre and polyphenylene sulfide is carried out composite strengthening, to obtain the more excellent polyphenylene sulfide enhancing of performance compound
Material.
2nd, the composite property that preparation method of the present invention is prepared is excellent, and method is simple, convenient, is adapted to polyphenylene sulfide
Strengthen industrialization, the large-scale production of composite.
3rd, bonded power is strong between polyphenylene sulfide and basalt fibre in composite of the present invention, is not likely to produce phase separation, phase
Capacitive is good, and the humidification of basalt fiber poly-p-phenylene sulfide ether is dramatically increased, and the performance of composite is also significantly improved.
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)Modification:The benzole soln of the basalt fibre diphenyl disulfide containing the barium phosphate of mass percent 0.8% is entered
Row immersion treatment 2h, inserts in the mixed solution of aluminium chloride that pH value is 2 and sulfuric acid after taking-up, is reacted after being heated to 60 DEG C
After 10min, dry treated basalt fiber is taken out;
(2)It is compound:By the polyphenyl thioether material of the treated basalt fiber of 10 weight portions and 90 weight portions, the silane of 2 weight portions
Coupling agent carries out Combined Processing, obtains polyphenylene sulfide enhancing composite.
Embodiment 2
(1)Modification:The benzole soln of the basalt fibre diphenyl disulfide containing the barium phosphate of mass percent 2.0% is entered
Row immersion treatment 1h, inserts in the mixed solution of iron chloride that pH value is 1 and hydrochloric acid after taking-up, is reacted after being heated to 50 DEG C
After 20min, dry treated basalt fiber is taken out;
(2)It is compound:By the polyphenyl thioether material of the treated basalt fiber of 10 weight portions and 90 weight portions, the silane of 2 weight portions
Coupling agent carries out Combined Processing, obtains polyphenylene sulfide enhancing composite.
Embodiment 3
(1)Modification:The benzole soln of the basalt fibre diphenyl disulfide containing the barium phosphate of mass percent 0.1% is entered
Row immersion treatment 3h, inserts in the mixed solution of boron trifluoride that pH value is 4 and nitric acid after taking-up, is reacted after being heated to 80 DEG C
After 5min, dry treated basalt fiber is taken out;
(2)It is compound:By the polyphenyl thioether material of the treated basalt fiber of 10 weight portions and 90 weight portions, the silane of 2 weight portions
Coupling agent carries out Combined Processing, obtains polyphenylene sulfide enhancing composite.
Embodiment 4
(1)Modification:The benzole soln of the basalt fibre diphenyl disulfide containing the barium phosphate of mass percent 0.3% is entered
Row immersion treatment 2h, inserts in the mixed solution of boron trifluoride that pH value is 3 and phosphoric acid after taking-up, is reacted after being heated to 50 DEG C
After 15min, dry treated basalt fiber is taken out;
(2)It is compound:By the polyphenyl thioether material of the treated basalt fiber of 10 weight portions and 90 weight portions, the silane of 2 weight portions
Coupling agent carries out Combined Processing, obtains polyphenylene sulfide enhancing composite.
Comparative example 1
(1)Modification:Conventional basalt fibre is carried out into immersion treatment 2h with the benzole soln of diphenyl disulfide, is inserted after taking-up
During pH value is 2 aluminium chloride and the mixed solution of sulfuric acid, after reacting 10min after being heated to 60 DEG C, the dry Black Warrior that must be modified is taken out
Rock fiber;
(2)It is compound:By the polyphenyl thioether material of the treated basalt fiber of 10 weight portions and 90 weight portions, the silane of 2 weight portions
Coupling agent carries out Combined Processing, obtains polyphenylene sulfide enhancing composite.
Comparative example 2
By the polyphenyl thioether material of the basalt fibre containing the barium phosphate of mass percent 1.0% of 10 weight portions and 90 weight portions,
The silane coupler of 2 weight portions carries out Combined Processing, obtains polyphenylene sulfide enhancing composite.
Comparative example 3
The conventional basalt fibre of 10 weight portions is entered with the polyphenyl thioether material of 90 weight portions, the silane coupler of 2 weight portions
Row Combined Processing, obtains polyphenylene sulfide enhancing composite.
Preparation-obtained polyphenylene sulfide enhancing composite in above-described embodiment 1-4 and comparative example 1-3 is carried out into performance
Test experiments record experimental result, and record data is as follows:(Polyphenylene sulfide:Tensile strength 58MPa, notch impact strength 32J/m,
Elongation at break 26%)
Numbering | Polyphenylene sulfide strengthens composite notch impact strength(J/m) | Polyphenylene sulfide strengthens composite tensile strength(MPa) | Polyphenylene sulfide strengthens fracture of composite materials elongation(%) |
Embodiment 1 | 58 | 94 | 59 |
Embodiment 2 | 55 | 95 | 62 |
Embodiment 3 | 57 | 96 | 56 |
Embodiment 4 | 56 | 93 | 63 |
Comparative example 1 | 47 | 78 | 46 |
Comparative example 2 | 46 | 76 | 48 |
Comparative example 3 | 39 | 68 | 32 |
Above-mentioned analysis of experimental data is understood, the polyphenylene sulfide prepared using technical solution of the present invention in embodiment 1-4 is increased
The notch impact strength of composite, tensile strength, elongation at break have and are obviously improved by force;And in the preparation method of comparative example 1
The basalt fibre of use does not contain barium phosphate, modified fiber and polyphenyl thioether material poor compatibility, with polyphenyl thioether material
Chemical bonding ability, polyphenylene sulfide enhancing composite property significantly reduce;It is not modified in the preparation method of comparative example 2
Treatment, the chemical bonding with polyphenyl thioether material is less able, and polyphenylene sulfide enhancing composite property is significantly reduced;Comparative example
Directly it is combined using conventional basalt fibre in 3 preparation methods, the humidification of poly-p-phenylene sulfide ether is worst.
Claims (10)
1. a kind of polyphenylene sulfide strengthens the preparation method of composite, it is characterised in that comprise the following steps:
(1)Modification:Basalt fibre is carried out into immersion treatment with modifier A, is inserted after taking-up in modifying agent B, heating is anti-
Should completely after, take out dry treated basalt fiber;
(2)It is compound:Treated basalt fiber and polyphenyl thioether material, coupling agent are carried out into Combined Processing, polyphenylene sulfide increasing is obtained
Strong composite;
Contain barium phosphate in described basalt fibre;Described modifier A is the benzole soln of diphenyl disulfide;Described is modified
Agent B is the mixed solution of lewis acid and inorganic acid.
2. preparation method according to claim 1, it is characterised in that described basalt fibre contains mass percent
The barium phosphate of 1.0-2.0%.
3. preparation method according to claim 2, it is characterised in that described basalt fibre contains mass percent
The barium phosphate of 0.3-0.8%.
4. preparation method according to claim 1, it is characterised in that the lewis acid is aluminium chloride, iron chloride, trifluoro
Change one or more in boron.
5. preparation method according to claim 1, it is characterised in that the inorganic acid is sulfuric acid, hydrochloric acid, phosphoric acid, nitric acid
In one or more.
6. preparation method according to claim 1, it is characterised in that described modifying agent B solution pH value is 1-4.
7. preparation method according to claim 1, it is characterised in that basalt fibre soaks in modifier A in step 1
Time be 1-3h.
8. preparation method according to claim 1, it is characterised in that the temperature of heating response is 50-80 DEG C in step 1,
Reaction time is 5-20min.
9. preparation method according to claim 1, it is characterised in that treated basalt fiber consumption is polyphenyl in step 2
The 1-20% of sulfide material weight.
10. a kind of polyphenylene sulfide strengthens composite, it is characterised in that the composite is any by claim 1-9
What preparation method was prepared.
Priority Applications (1)
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CN201611139169.0A CN106700102A (en) | 2016-12-12 | 2016-12-12 | Polyphenylene sulfide reinforced composite material and preparing method thereof |
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CN201611139169.0A CN106700102A (en) | 2016-12-12 | 2016-12-12 | Polyphenylene sulfide reinforced composite material and preparing method thereof |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107945960A (en) * | 2017-10-31 | 2018-04-20 | 四川力智久创知识产权运营有限公司 | A kind of tension polyphenylene sulfide cable |
CN110669339A (en) * | 2019-10-28 | 2020-01-10 | 青岛科技大学 | High-strength impact-resistant polyphenylene sulfide/basalt fiber composite material |
-
2016
- 2016-12-12 CN CN201611139169.0A patent/CN106700102A/en not_active Withdrawn
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107945960A (en) * | 2017-10-31 | 2018-04-20 | 四川力智久创知识产权运营有限公司 | A kind of tension polyphenylene sulfide cable |
CN110669339A (en) * | 2019-10-28 | 2020-01-10 | 青岛科技大学 | High-strength impact-resistant polyphenylene sulfide/basalt fiber composite material |
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Application publication date: 20170524 |