CN108239399A - A kind of preparation method of high temperature resistant glass fibre reinforced plastic - Google Patents

A kind of preparation method of high temperature resistant glass fibre reinforced plastic Download PDF

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CN108239399A
CN108239399A CN201810084160.7A CN201810084160A CN108239399A CN 108239399 A CN108239399 A CN 108239399A CN 201810084160 A CN201810084160 A CN 201810084160A CN 108239399 A CN108239399 A CN 108239399A
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parts
glass fibre
reinforced plastic
high temperature
fibre reinforced
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王成友
虞林森
焦正超
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Tongling Four Tong Environmental Technology Co Ltd
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Tongling Four Tong Environmental Technology Co Ltd
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L79/00Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
    • C08L79/04Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C08L79/08Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

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  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Reinforced Plastic Materials (AREA)

Abstract

The invention discloses a kind of preparation methods of high temperature resistant glass fibre reinforced plastic, are related to frp process technical field;The preparation of high temperature resistant glass fibre reinforced plastic includes the following steps:(1) prepared by pyroceram steel substrate;(2) high temperature resistant glass fibre reinforced plastic is aged;The present invention prepares high temperature resistant glass fibre reinforced plastic with thermal stability and irradiation stability, it is light and hard, it is non-conductive, performance is stablized, high mechanical strength, impact resistance, high temperature resistant, it is corrosion-resistant, recycle less, use material safety, preparation process is convenient, by techniques such as base material preparation, ageings in high temperature resistant glass fibre reinforced plastic preparation process, extend high temperature resistant glass fibre reinforced plastic service life, improve the safety in utilization of fiberglass, stability.

Description

A kind of preparation method of high temperature resistant glass fibre reinforced plastic
Technical field:
The present invention relates to frp process technical fields, and in particular to a kind of preparation method of high temperature resistant glass fibre reinforced plastic.
Background technology:
Fiberglass (FRP) is also referred to as GFRP, i.e. fiber-reinforced plastic, refer generally to glass fiber reinforcement unsaturated polyester, Epoxy resin and phenolic resin as matrix resin.Make the reinforced plastics of reinforcing material with glass fibre or its product, appellation is glass fibre Reinforced plastics or for fiberglass, different from tempered glass.
Due to used resin variety difference, have organic toughened glass, fiber glass epoxy, phenolic fiberglass reinforced plastics it is not. Light and hard, non-conductive, performance is stablized, high mechanical strength, recycles less, corrosion-resistant.It can replace steel manufacture machine zero Part and automobile, ship housing etc..
Fiberglass scientific name fibre reinforced plastics are commonly called as FRP (Fiber Reinforced Plastics), i.e. fiber reinforcement Composite plastic.Glass fiber reinforced composite plastics (GFRP), fibre reinforced composite plastic are divided into according to the fiber difference of use (CFRP), boron fibre enhancing composite plastic etc..It is using glass fibre and its product (glass cloth, band, felt, yarn etc.) as enhancing Material makees a kind of composite material of basis material with synthetic resin.Fibre reinforced composites are by reinforcing fiber and matrix group Into.The diameter very little of fiber (or whisker), generally at 10 μm hereinafter, defect is less and smaller, breaking strain is about 3/1000ths It is fragile material within ten, easy damaged, fracture and is corroded.Matrix for fiber, intensity, modulus will it is low very It is more, but big strain can be withstood, it is toughness material often with viscoplasticity and elastoplasticity.
Invention content:
The technical problems to be solved by the invention are to provide a kind of preparation method of high temperature resistant glass fibre reinforced plastic, light and hard, It is non-conductive, performance is stable, high mechanical strength, impact resistance, high temperature resistant, it is corrosion-resistant, recycle it is few.It to be solved using the present invention The technical issues of realized using following technical scheme:
A kind of preparation method of high temperature resistant glass fibre reinforced plastic is as follows including specific technical solution:High temperature resistant glass fibre reinforced plastic includes as follows Number component:
Kh5600.1-0.3 parts of silane coupling agent, 30-40 parts of dimethylacetylamide, 3-18 parts of polyvinyl alcohol, polyvinyl chloride 25-30 parts, 5-11 parts of active oxidation aluminium ball, 2-3 parts of polyethyleneimine, 0.8-1 parts of sldium lauryl sulfate, maleic anhydride 0.7-1 parts, 5-7 parts of octamethylcy-clotetrasiloxane ,-POSS2-3 parts of octaphenyl, 45-68 parts of glass fibre, four silicon of octyl phenyl ring 1-3 parts of oxygen alkane, 37-40 parts of 4,4'- diaminodiphenyl ethers, 6-13 parts of pyromellitic acid anhydride, 7-11 parts of N-Methyl pyrrolidone, 3-4 parts of calcium aluminate, 0.1-0.2 parts of butanethiol tin, 4-6 parts of chlorinated paraffin, 20-25% 3-8 parts of acetum.
A kind of preparation method of high temperature resistant glass fibre reinforced plastic, includes the following steps:
(1) prepared by pyroceram steel substrate:
(a) 10-15% of octamethylcy-clotetrasiloxane weight is taken, is mixed with maleic anhydride, is passed through nitrogen, in 90- Insulation reaction 2-3 hours at 95 DEG C, it is room temperature slowly to reduce temperature, obtains alkaline-sol;
(b) 10-15% of dimethylacetylamide weight is taken, adds in remaining octamethylcy-clotetrasiloxane, octyl phenyl ring Tetrasiloxane, octaphenyl-POSS, stir evenly, are passed through nitrogen, add in above-mentioned alkaline-sol, in 90-95 DEG C of insulated and stirred 30-40 Minute, stopping is passed through nitrogen, keeps the temperature 2-3 hours, and raising temperature is 150-160 DEG C, keeps the temperature 27-30 minutes, cooling, in 60-65 It is dried in vacuo 1-2 hours at DEG C, obtains cross linking polysiloxane;
(c) 4,4'- diaminodiphenyl ethers are added in 3-4 times of its weight, 15-17% sulfuric acid solution, in addition The acetum of 20-25% is stated, stands 1-2 hours, filtering precipitation is washed with deionized water 3-4 times, the vacuum at 60-70 DEG C It is 4-5 hours dry, obtain refined phenylate;
(d) glass fibre and polyvinyl chloride are added in melting furnace and are heated to being completely melt for 1000-1200 DEG C, after will be above-mentioned Refined phenylate, cross linking polysiloxane, polyvinyl alcohol, add in silane coupling agent, stir evenly, and are sent into ice-water bath, are passed through Nitrogen is stirred to react 2-3 hours, and product is added in the distilled water of 30-40 times of its weight by discharging, and room temperature stands 4-5 days, Filtering, obtains precrosslink polyimides polyvinyl chloride;
(e) pyromellitic acid anhydride is added in the absolute ethyl alcohol of 3-5 times of its weight, raising temperature is 80-90 DEG C, is added Enter chlorinated paraffin, polyethyleneimine, insulated and stirred 10-17 minutes, discharging adds in butanethiol tin, stirs to room temperature, obtain amide Alcohol liquid;
(f) above-mentioned precrosslink polyimides polyvinyl chloride, amide alcohol liquid are mixed, raising temperature is 50-60 DEG C, in addition Dimethylacetylamide is stated, 100-200 revs/min is stirred 4-10 minutes, obtains silane-modified amide solution;
(g) above-mentioned active oxidation aluminium ball is added in N-Methyl pyrrolidone, it is 2-3 minutes ultrasonic, obtain alumina dispersion Liquid;
(h) above-mentioned silane-modified amide solution is added in alumina fluid dispersion, adds in above-mentioned sldium lauryl sulfate, surpassed Sound 20-30 minutes, filtering, will be deposited at 76-80 DEG C and be dried in vacuo 3-5 hours, wear into fine powder, 250-260 DEG C of feeding it is true It in empty drying box, heats 6-7 hours, discharging cooling obtains cross-linking modified polyimides;
(i) above-mentioned cross-linking modified polyimides with remaining each raw material is mixed, stirs evenly, be sent to screw extruder In, melting extrusion is cooled down up to the pyroceram steel substrate.
(2) 65-85 DEG C of pyroceram steel substrate holding chamber temperature is subjected to ageing 5-7 days, and will material heating after ageing Material is added in high-pressure bottle into horizontal high voltage batch mixing after 35-50 DEG C, and pressure is 2.5~3.5 times of atmospheric pressure, the temperature of high pressure batch mixing It it is 155-180 DEG C, the time of high pressure batch mixing is 8-10 minutes;Then it adds in extruder and completes melting, batch mixing, the process squeezed out, The machine barrel of extruder includes four areas, and from feed end to extruding end, the temperature in four areas is followed successively by 665-685 DEG C, 820-830 DEG C, 605-610 DEG C, 490-495 DEG C, the machine cylinder pressure of the extruder is 0.06MPa;Finally extruded material is added in entirely certainly Dynamic fiberglass maker, is fabricated to fiberglass.
Ageing in the high temperature resistant glass fibre reinforced plastic preparation method step 2, is as follows:By the high temperature resistant glass fibre reinforced plastic Step 1 prepares glass steel substrate and is aged in constant temperature oven, and when to select Aging Temperature be 65-85 DEG C, digestion time is 7 days, choosing When to select Aging Temperature be 90-105 DEG C, digestion time is 3 days, and when select Aging Temperature be 120-135 DEG C, digestion time is 2 days, When to select Aging Temperature be 150-175 DEG C, digestion time is 1 day.
The advantages of high temperature resistant glass fibre reinforced plastic of the present invention, is:
The present invention introduces polyimides in the strand of polyimides, to the shearing force of cross linking polysiloxane, can incite somebody to action Polysiloxanes is dispersed into smaller particle, can be uniformly coated on the surface of polyimide particle, so as to form hydrophobic layer, So as to improve its dispersing uniformity in the composite;The cross linking polysiloxane of the present invention also has good thermal stability And irradiation stability;The present invention mixes precrosslink polyimides with aluminium nitride suspension, and the composite material of formation combines poly- The respective advantage of acid imide and aluminium nitride has the excellent performances such as high heat conduction, high temperature resistant, low bulk, low dielectric, electrical isolation; The present invention uses a variety of silane-modified materials, effectively raises the mechanical strength of high temperature resistant glass fibre reinforced plastic.
High temperature resistant glass fibre reinforced plastic has efficient waterproof, ageing-resistant, light and hard, non-conductive, performance stabilization, mechanical strength Height, intensity height, impact resistance, high temperature resistant, corrosion-resistant, recycling is few, is easy to get using material is safe and convenient, high temperature resistant glass fibre reinforced plastic By techniques such as base material preparation, ageings in preparation process, extend high temperature resistant glass fibre reinforced plastic service life, improve the use peace of fiberglass Quan Xing, stability.
Specific embodiment:
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below Specific embodiment is closed, the present invention is further explained.
Embodiment 1:
A kind of preparation method of high temperature resistant glass fibre reinforced plastic;
The technical problems to be solved by the invention are realized using following technical scheme:
A kind of preparation method of high temperature resistant glass fibre reinforced plastic is as follows including specific technical solution:High temperature resistant glass fibre reinforced plastic includes as follows Number component:
Kh560-0.3 parts of silane coupling agent, 30 parts of dimethylacetylamide, 3 parts of polyvinyl alcohol, 25 parts of polyvinyl chloride, activity 5 parts of alumina balls, 2 parts of polyethyleneimine, 0.8 part of sldium lauryl sulfate, 0.7 part of maleic anhydride, four silica of prestox ring 5 parts of alkane ,-POSS2 parts of octaphenyl, 58 parts of glass fibre, 1 part of octyl phenyl cyclotetrasiloxane, 4,4'- diaminodiphenyl ethers 37 Part, 6 parts of pyromellitic acid anhydride, 7 parts of N-Methyl pyrrolidone, 3 parts of calcium aluminate, 0.1 part of butanethiol tin, 4 parts of chlorinated paraffin, 4 parts of the acetum of 20-25%.
A kind of preparation method of high temperature resistant glass fibre reinforced plastic, includes the following steps:
(1) prepared by pyroceram steel substrate:
(a) the 10% of octamethylcy-clotetrasiloxane weight is taken, is mixed with maleic anhydride, is passed through nitrogen, at 90-95 DEG C Lower insulation reaction 2 hours, it is room temperature slowly to reduce temperature, obtains alkaline-sol;
(b) the 10% of dimethylacetylamide weight is taken, adds in remaining octamethylcy-clotetrasiloxane, four silicon of octyl phenyl ring Oxygen alkane, octaphenyl-POSS, stir evenly, are passed through nitrogen, add in above-mentioned alkaline-sol, in 90-95 DEG C of insulated and stirred 30 minutes, stop Nitrogen is only passed through, keeps the temperature 2 hours, raising temperature is 150 DEG C, keeps the temperature 27 minutes, cooling, and it is small that 1 is dried in vacuo at 60-65 DEG C When, obtain cross linking polysiloxane;
(c) 4,4'- diaminodiphenyl ethers are added in 3 times of its weight, 15% sulfuric acid solution, add in above-mentioned 20% Acetum, stand 1 hour, filtering, precipitation is washed with deionized water 3 times, is dried in vacuo 4 hours, obtains refined at 60 DEG C Phenylate;
(d) glass fibre and polyvinyl chloride are added in melting furnace and are heated to being completely melt for 1000-1050 DEG C, after will be above-mentioned Refined phenylate, cross linking polysiloxane, polyvinyl alcohol, add in silane coupling agent, stir evenly, and are sent into ice-water bath, are passed through Nitrogen is stirred to react 2 hours, and product is added in the distilled water of 30 times of its weight by discharging, and room temperature stands 4 days, and filtering obtains Precrosslink polyimides polyvinyl chloride;
(e) pyromellitic acid anhydride is added in the absolute ethyl alcohol of 3 times of its weight, raising temperature is 80 DEG C, adds in chlorine Fossil waxes, polyethyleneimine, insulated and stirred 10 minutes, discharging add in butanethiol tin, stir to room temperature, obtain amide alcohol liquid;
(f) above-mentioned precrosslink polyimides polyvinyl chloride, amide alcohol liquid are mixed, raising temperature is 50-55 DEG C, in addition Dimethylacetylamide is stated, 200 revs/min are stirred 5 minutes, obtain silane-modified amide solution;
(g) above-mentioned active oxidation aluminium ball is added in N-Methyl pyrrolidone, ultrasound 3 minutes obtains alumina fluid dispersion;
(h) above-mentioned silane-modified amide solution is added in alumina fluid dispersion, adds in above-mentioned sldium lauryl sulfate, surpassed Sound 30 minutes, filtering, will be deposited at 76-80 DEG C and is dried in vacuo 3 hours, wear into fine powder, be sent into 250-260 DEG C of vacuum drying It in case, heats 6 hours, discharging cooling obtains cross-linking modified polyimides;
(i) above-mentioned cross-linking modified polyimides with remaining each raw material is mixed, stirs evenly, be sent to screw extruder In, melting extrusion is cooled down up to the pyroceram steel substrate.
(2) 75-80 DEG C of pyroceram steel substrate holding chamber temperature is subjected to ageing 7 days, and 50 DEG C will be heated by material after ageing Material is added in into horizontal high voltage batch mixing in high-pressure bottle afterwards, and pressure is 3.5 times of atmospheric pressure, and the temperature of high pressure batch mixing is 180 DEG C, high pressure The time of batch mixing is 10 minutes;Then it adds in extruder and completes melting, batch mixing, the process squeezed out, the machine barrel of extruder includes four A area, from feed end to extruding end, the temperature in four areas is followed successively by 685 DEG C, 830 DEG C, 610 DEG C, 495 DEG C, the extruder Machine cylinder pressure is 0.06MPa;Extruded material is finally added in into full-automatic glass steel maker, is fabricated to fiberglass.
Ageing in the high temperature resistant glass fibre reinforced plastic preparation method step 2, is as follows:By the high temperature resistant glass fibre reinforced plastic Step 1 prepares glass steel substrate and is aged in constant temperature oven, and when to select Aging Temperature be 75-80 DEG C, digestion time is 7 days.
Embodiment 2:
A kind of preparation method of high temperature resistant glass fibre reinforced plastic;
The technical problems to be solved by the invention are realized using following technical scheme:
A kind of preparation method of high temperature resistant glass fibre reinforced plastic, includes the following steps:
(1) prepared by pyroceram steel substrate:
(a) the 12% of octamethylcy-clotetrasiloxane weight is taken, is mixed with maleic anhydride, is passed through nitrogen, at 95 DEG C Insulation reaction 2 hours, it is room temperature slowly to reduce temperature, obtains alkaline-sol;
(b) the 12% of dimethylacetylamide weight is taken, adds in remaining octamethylcy-clotetrasiloxane, four silicon of octyl phenyl ring Oxygen alkane, octaphenyl-POSS, stir evenly, are passed through nitrogen, add in above-mentioned alkaline-sol, in 95 DEG C of insulated and stirreds 40 minutes, stop logical Enter nitrogen, keep the temperature 2 hours, raising temperature is 160 DEG C, keeps the temperature 30 minutes, and cooling is dried in vacuo 2 hours at 65 DEG C, must be crosslinked Polysiloxanes;
(c) 4,4'- diaminodiphenyl ethers are added in 4 times of its weight, 15% sulfuric acid solution, add in above-mentioned 25% Acetum, stand 2 hours, filtering, precipitation is washed with deionized water 3 times, is dried in vacuo 4 hours, obtains refined at 70 DEG C Phenylate;
(d) glass fibre and polyvinyl chloride are added in melting furnace and are heated to being completely melt for 1000-1100 DEG C, after will be above-mentioned Refined phenylate, cross linking polysiloxane, polyvinyl alcohol, add in silane coupling agent, stir evenly, and are sent into ice-water bath, are passed through Nitrogen is stirred to react 3 hours, and product is added in the distilled water of 35 times of its weight by discharging, and room temperature stands 5 days, and filtering obtains Precrosslink polyimides polyvinyl chloride;
(e) pyromellitic acid anhydride is added in the absolute ethyl alcohol of 5 times of its weight, raising temperature is 80-90 DEG C, is added in Chlorinated paraffin, polyethyleneimine, insulated and stirred 17 minutes, discharging add in butanethiol tin, stir to room temperature, obtain amide alcohol liquid;
(f) above-mentioned precrosslink polyimides polyvinyl chloride, amide alcohol liquid are mixed, raising temperature is 60 DEG C, is added in above-mentioned Dimethylacetylamide, 200 revs/min are stirred 10 minutes, obtain silane-modified amide solution;
(g) above-mentioned active oxidation aluminium ball is added in N-Methyl pyrrolidone, ultrasound 3 minutes obtains alumina fluid dispersion;
(h) above-mentioned silane-modified amide solution is added in alumina fluid dispersion, adds in above-mentioned sldium lauryl sulfate, surpassed Sound 30 minutes, filtering, will be deposited at 80 DEG C and is dried in vacuo 4 hours, wear into fine powder, is sent into 260 DEG C of vacuum drying chamber, adds Heat 7 hours, discharging cooling, obtains cross-linking modified polyimides;
(i) above-mentioned cross-linking modified polyimides with remaining each raw material is mixed, stirs evenly, be sent to screw extruder In, melting extrusion is cooled down up to the pyroceram steel substrate.
(2) 80-85 DEG C of pyroceram steel substrate holding chamber temperature is subjected to ageing 6 days, and 50 DEG C will be heated by material after ageing Material is added in into horizontal high voltage batch mixing in high-pressure bottle afterwards, and pressure is 3.5 times of atmospheric pressure, and the temperature of high pressure batch mixing is 180 DEG C, high pressure The time of batch mixing is 10 minutes;Then it adds in extruder and completes melting, batch mixing, the process squeezed out, the machine barrel of extruder includes four A area, from feed end to extruding end, the temperature in four areas is followed successively by 680 DEG C, 825 DEG C, 610 DEG C, 490 DEG C, the extruder Machine cylinder pressure is 0.06MPa;Extruded material is finally added in into full-automatic glass steel maker, is fabricated to fiberglass.
To carrying out experiment investigation respectively in embodiment provided by the invention, embodiment 1 and embodiment 2 are prepared into high temperature resistant glass Glass steel detects, and the results are shown in Table 1;
1 high temperature resistant glass fibre reinforced plastic testing result of table
Wherein water imbibition test method is:It is carried out under the conditions of 20 ± 5 DEG C, 24 ± 0.5h of soaking time, experiment sensibility reciprocal Assay balance for 0.0005g.Sample is taken out from water after immersion for 24 hours, surface is blotted with filter paper, is put into after latter 70 DEG C dry 4h It is cooled to room temperature in drier,
Heat exposure detects:113 ± 1 DEG C of bellows of the material Jing Guo circulation air, after the processing of 168h, high temperature resistant glass fibre reinforced plastic It is distorted or during effect that other are unfavorable, high temperature resistant glass fibre reinforced plastic should not generate rupture.
By the above results show that:The present invention prepares high temperature resistant glass fibre reinforced plastic with thermal stability and irradiation stability, it is light and Firmly, non-conductive, performance is stablized, and high mechanical strength, impact resistance, high temperature resistant, corrosion-resistant, recycling is few.Use material safety, system Standby technique is convenient, by techniques such as base material preparation, ageings in high temperature resistant glass fibre reinforced plastic preparation process, extends high temperature resistant glass fibre reinforced plastic and uses Time limit improves the safety in utilization of fiberglass, stability.
The basic principles, main features and the advantages of the invention have been shown and described above.The technology of the industry Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its Equivalent thereof.

Claims (2)

1. a kind of preparation method of high temperature resistant glass fibre reinforced plastic, it is characterised in that:The preparation method of high temperature resistant glass fibre reinforced plastic, including following step Suddenly:
(1) prepared by pyroceram steel substrate:
(a) 10-15% of octamethylcy-clotetrasiloxane weight is taken, is mixed with maleic anhydride, is passed through nitrogen, at 90-95 DEG C Lower insulation reaction 2-3 hours, it is room temperature slowly to reduce temperature, obtains alkaline-sol;
(b) 10-15% of dimethylacetylamide weight is taken, adds in remaining octamethylcy-clotetrasiloxane, four silicon of octyl phenyl ring Oxygen alkane, octaphenyl-POSS, stir evenly, are passed through nitrogen, add in above-mentioned alkaline-sol, in 90-95 DEG C of insulated and stirred 30-40 minutes, Stopping is passed through nitrogen, keeps the temperature 2-3 hours, and raising temperature is 150-160 DEG C, keeps the temperature 27-30 minutes, and cooling is true at 60-65 DEG C Sky is 1-2 hours dry, obtains cross linking polysiloxane;
(c) 4,4'- diaminodiphenyl ethers are added in 3-4 times of its weight, 15-17% sulfuric acid solution, add in above-mentioned 20- 25% acetum stands 1-2 hours, and precipitation is washed with deionized water 3-4 times, 4- is dried in vacuo at 60-70 DEG C by filtering 5 hours, obtain refined phenylate;
(d) glass fibre and polyvinyl chloride are added in melting furnace and are heated to being completely melt for 1000-1200 DEG C, after above-mentioned will refine Phenylate, cross linking polysiloxane, polyvinyl alcohol add in silane coupling agent, stir evenly, and are sent into ice-water bath, are passed through nitrogen, It being stirred to react 2-3 hours, discharges, product is added in the distilled water of 30-40 times of its weight, room temperature stands 4-5 days, filtering, Obtain precrosslink polyimides polyvinyl chloride;
(e) pyromellitic acid anhydride is added in the absolute ethyl alcohol of 3-5 times of its weight, raising temperature is 80-90 DEG C, adds in chlorine Fossil waxes, polyethyleneimine, insulated and stirred 10-17 minutes, discharging add in butanethiol tin, stir to room temperature, obtain amide alcohol Liquid;
(f) above-mentioned precrosslink polyimides polyvinyl chloride, amide alcohol liquid are mixed, raising temperature is 50-60 DEG C, adds in above-mentioned two Methylacetamide, 100-200 revs/min is stirred 4-10 minutes, obtains silane-modified amide solution;
(g) above-mentioned active oxidation aluminium ball is added in N-Methyl pyrrolidone, it is 2-3 minutes ultrasonic, obtain alumina fluid dispersion;
(h) above-mentioned silane-modified amide solution is added in alumina fluid dispersion, adds in above-mentioned sldium lauryl sulfate, ultrasound 20-30 minutes, filtering will be deposited at 76-80 DEG C and be dried in vacuo 3-5 hours, wear into fine powder, be sent into 250-260 DEG C of vacuum It in drying box, heats 6-7 hours, discharging cooling obtains cross-linking modified polyimides;
(i) above-mentioned cross-linking modified polyimides with remaining each raw material is mixed, stirs evenly, be sent in screw extruder, melt Melt extrusion, cool down up to the pyroceram steel substrate;
(2) 65-85 DEG C of pyroceram steel substrate holding chamber temperature is subjected to ageing 5-7 days, and 35-50 will be heated by material after ageing Material is added in high-pressure bottle into horizontal high voltage batch mixing after DEG C, and pressure is 2.5~3.5 times of atmospheric pressure, and the temperature of high pressure batch mixing is 155-180 DEG C, the time of high pressure batch mixing is 8-10 minutes;Then it adds in extruder and completes melting, batch mixing, the process squeezed out, squeeze The machine barrel for going out machine includes four areas, from feed end to extruding end, the temperature in four areas be followed successively by 665-685 DEG C, 820-830 DEG C, 605-610 DEG C, 490-495 DEG C, the machine cylinder pressure of the extruder is 0.06MPa;Finally extruded material is added in full-automatic Fiberglass maker, is fabricated to fiberglass;
The high temperature resistant glass fibre reinforced plastic includes following number component:
Kh5600.1-0.3 parts of silane coupling agent, 30-40 parts of dimethylacetylamide, 3-18 parts of polyvinyl alcohol, polyvinyl chloride 25-30 Part, 5-11 parts of active oxidation aluminium ball, 2-3 parts of polyethyleneimine, 0.8-1 parts of sldium lauryl sulfate, maleic anhydride 0.7-1 Part, 5-7 parts of octamethylcy-clotetrasiloxane ,-POSS2-3 parts of octaphenyl, 45-68 parts of glass fibre, octyl phenyl cyclotetrasiloxane 1-3 parts, 37-40 parts of 4,4'- diaminodiphenyl ethers, 6-13 parts of pyromellitic acid anhydride, 7-11 parts of N-Methyl pyrrolidone, aluminic acid 3-4 parts of calcium, 0.1-0.2 parts of butanethiol tin, 4-6 parts of chlorinated paraffin, 20-25% 3-8 parts of acetum.
2. the preparation method of high temperature resistant glass fibre reinforced plastic according to claim 1, it is characterised in that:The pyroceram steel Ageing in Preparation Method step 2, is as follows:The high temperature resistant glass fibre reinforced plastic step 1 is prepared into glass steel substrate in constant temperature It is aged in baking oven, when to select Aging Temperature be 65-85 DEG C, digestion time is 7 days, old when to select Aging Temperature be 90-105 DEG C It is 3 days to change the time, and when select Aging Temperature be 120-135 DEG C, digestion time is 2 days, selects Aging Temperature as 150-175 DEG C When, digestion time is 1 day.
CN201810084160.7A 2018-01-29 2018-01-29 A kind of preparation method of high temperature resistant glass fibre reinforced plastic Pending CN108239399A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
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CN110156290A (en) * 2019-05-22 2019-08-23 北京金格玖畅环保科技有限公司 A kind of equipment that microwave method administers oily sludge
CN112078992A (en) * 2020-09-10 2020-12-15 中国石油化工股份有限公司 Composite material and oil storage tank

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1230570A (en) * 1998-04-01 1999-10-06 中国科学院化学研究所 Short staple-containing composite polyimide material and its preparation and use
CN105086445A (en) * 2014-05-16 2015-11-25 黑龙江鑫达企业集团有限公司 Preparation of high temperature resistant polyimide composite material
CN105713387A (en) * 2014-12-05 2016-06-29 黑龙江鑫达企业集团有限公司 Preparation method of thermoplastic polyimide composite material
CN105924742A (en) * 2016-06-22 2016-09-07 安徽电信器材贸易工业有限责任公司 Fiber toughening heat-resistant optical cable material and preparation method thereof
CN106009163A (en) * 2016-06-22 2016-10-12 安徽电信器材贸易工业有限责任公司 Flexible, anti-freezing and heat-resisting optical cable material and preparation method thereof
CN106009166A (en) * 2016-06-22 2016-10-12 安徽电信器材贸易工业有限责任公司 Multi-silane modified heat-resisting optical cable material and preparation method thereof
CN106084394A (en) * 2016-06-22 2016-11-09 安徽电信器材贸易工业有限责任公司 A kind of insulation heat-resistant cable material and preparation method thereof
CN106480533A (en) * 2016-10-09 2017-03-08 西北工业大学 A kind of polymide dielectric heat-conductive composite material and preparation method thereof

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1230570A (en) * 1998-04-01 1999-10-06 中国科学院化学研究所 Short staple-containing composite polyimide material and its preparation and use
CN105086445A (en) * 2014-05-16 2015-11-25 黑龙江鑫达企业集团有限公司 Preparation of high temperature resistant polyimide composite material
CN105713387A (en) * 2014-12-05 2016-06-29 黑龙江鑫达企业集团有限公司 Preparation method of thermoplastic polyimide composite material
CN105924742A (en) * 2016-06-22 2016-09-07 安徽电信器材贸易工业有限责任公司 Fiber toughening heat-resistant optical cable material and preparation method thereof
CN106009163A (en) * 2016-06-22 2016-10-12 安徽电信器材贸易工业有限责任公司 Flexible, anti-freezing and heat-resisting optical cable material and preparation method thereof
CN106009166A (en) * 2016-06-22 2016-10-12 安徽电信器材贸易工业有限责任公司 Multi-silane modified heat-resisting optical cable material and preparation method thereof
CN106084394A (en) * 2016-06-22 2016-11-09 安徽电信器材贸易工业有限责任公司 A kind of insulation heat-resistant cable material and preparation method thereof
CN106480533A (en) * 2016-10-09 2017-03-08 西北工业大学 A kind of polymide dielectric heat-conductive composite material and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110156290A (en) * 2019-05-22 2019-08-23 北京金格玖畅环保科技有限公司 A kind of equipment that microwave method administers oily sludge
CN112078992A (en) * 2020-09-10 2020-12-15 中国石油化工股份有限公司 Composite material and oil storage tank

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