CN108219671A - A kind of bi-component addition type liquid silastic and preparation method thereof - Google Patents
A kind of bi-component addition type liquid silastic and preparation method thereof Download PDFInfo
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- CN108219671A CN108219671A CN201810027071.9A CN201810027071A CN108219671A CN 108219671 A CN108219671 A CN 108219671A CN 201810027071 A CN201810027071 A CN 201810027071A CN 108219671 A CN108219671 A CN 108219671A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The application belongs to silicon rubber technical field, and in particular to a kind of bi-component addition type liquid silastic and preparation method thereof.Bi-component addition type liquid silastic provided by the present invention is included by component A and the mixing cured molding of B component, component A：100 parts of base rubber, 8~18 parts of vinyl-terminated silicone fluid, 1~2 part of tackifier, 0.5 part of platinum catalyst；B component includes：20~70 parts of vinyl-terminated silicone fluid, 30~80 parts of containing hydrogen silicone oil, 0.3~0.5 part of inhibitor；Wherein, the raw material of base rubber includes：100 parts of vinyl-terminated silicone fluid, end-vinyl ethenyl of side chain silicone oil 5~10,40 parts of fume colloidal silica, 10~15 parts of silazane inorganic agent, 0~5 part of siloxane treated agent.Each component acts synergistically, and proportioning is reasonable, increases the firmness that silicon rubber is adhered to fabric surface, improves the tensile strength and tearing strength of silicon rubber, and curingprocess rate is fast, and production efficiency is high.The present invention also provides the preparation method of above-mentioned bi-component addition type liquid silastic, process optimization is easy to operate.
Description
Technical field
The invention belongs to silicon rubber technical fields, and in particular to a kind of bi-component addition type liquid silastic further relates to this
The preparation method of bi-component addition type liquid silastic.
Background technology
Add-on type liquid silicon rubber is important one kind in organic silicon rubber, refers to that vinyl silicone oil is (poly- containing vinyl
Siloxanes) with crosslinking agent containing hydrogen silicone oil (polysiloxanes of silicon-hydrogen bond containing) under the action of platinum group catalyst, in room temperature or heating
Under the conditions of by hydrosilylation formed the elastomer with tridimensional network.With high-low temperature resistant, electric insulating quality,
By-product is not generated during curing, coefficient of thermal expansion is small, and shrinking percentage is small, non-toxic and tasteless, it is non-corrosive the advantages that, be widely used in vapour
The multiple fields such as vehicle, electric appliance, aviation, chemical industry, medicine.However, add-on type liquid silicon rubber is the non-polar rubber of high saturation,
Molecular surface energy is very low, poor with the adhesive property of base material especially fabric after hardening, and silicon rubber is caused easily to be taken off from cloth
The problem of falling.Moreover, because of its relatively low fracture toughness and elongation, it is also easy to showing for colloid fracture occur when involving cloth
As these problems all limit application of the addition-type silicon rubber in ribbon coating silica gel is prepared.
Invention content
In order to solve existing addition-type silicon rubber and adhering fabric poor performance, the silica-gel coating being formed by curing is easily from fabric
The technical issues of surface comes off, the present invention provides a kind of bi-component addition type liquid silastics and preparation method thereof.
The specific technical solution of the present invention is as follows：
A kind of bi-component addition type liquid silastic, by component A and the mixing cured molding of B component, the component A includes：
100 parts of base rubber, 8~15 parts of vinyl-terminated silicone fluid, 1~2 part of tackifier, 0.5 part of platinum catalyst；
The B component includes：20~70 parts of vinyl-terminated silicone fluid, 30~80 parts of containing hydrogen silicone oil, inhibitor 0.3~0.5
Part；
The raw material of the base rubber includes：100 parts of vinyl-terminated silicone fluid, end-vinyl ethenyl of side chain silicone oil 5~10, gas
40 parts of phase method white carbon, 10~15 parts of silazane inorganic agent, 0~5 part of siloxane treated agent.
Preferably, the tackifier are vinyltrimethoxysilane, vinyltriethoxysilane, methyl trimethoxy oxygroup
Silane, γ-glycidoxypropyltrime,hoxysilane, N- β-aminoethyl-γ-aminopropyltrimethoxysilane, γ-(methyl
Acryloyl-oxy) one or more hydrolysates in propyl trimethoxy silicane and gamma-aminopropyl-triethoxy-silane, the water
Solution object is the reaction product of above-mentioned one-component or blending ingredients under the action of acidic catalyst.
Preferably, the range of viscosities of the vinyl-terminated silicone fluid be 5000~100000cP, contents of ethylene 0.05%
~0.5%；
The range of viscosities of the end-vinyl ethenyl of side chain silicone oil be 1000~80000cP, contents of ethylene 0.5%
~5%；
The hydrogen content of the containing hydrogen silicone oil is 0.2%~1.2%.
Preferably, the silazane inorganic agent is hexamethyldisilazane or vinyl silazane；
The siloxane treated agent is dimethyldimethoxysil,ne or dimethyl diethoxysilane.
Preferably, complex compound of the platinum catalyst for chloroplatinic acid and divinyl tetramethyl disiloxane, platinum content
For 500~10000ppm.
Preferably, the inhibitor is 1- acetenyl -1- cyclohexanol and the mixture of 2- methyl -3- crotonylene alcohol；Work as suppression
When preparation is mixture, mixing quality ratio is (1~5):1.
The present invention also provides the preparation methods of above-mentioned bi-component addition type liquid silastic, include the following steps：
A) by the mixture of the vinyl-terminated silicone fluid and end-vinyl ethenyl of side chain silicone oil and fume colloidal silica, silicon
Azane inorganic agent, siloxane treated agent and water are mixing, and are warming up to 145~155 DEG C and vacuumize, obtain the base rubber；
B) base rubber, vinyl-terminated silicone fluid, tackifier and platinum catalyst are mixed, obtains the A components；
C) vinyl-terminated silicone fluid, containing hydrogen silicone oil and 1- acetenyl -1- cyclohexanol are mixed, obtains the B component；
D) it is the component A and B component is mixing cured to get the bi-component addition type liquid silastic.
Preferably, the addition of the step a) water is 3~4 parts by weight；
Described be blended in kneader carries out, and incorporation time is 3~5h.
Preferably, described are blended in planetary stirring machine of step b) carries out；
Rotating speed is 25~35rpm, and the time is 50~70min.
Preferably, the step d) solidification temperatures are at 50 DEG C or more；Further, the weight ratio of the component A and B component
For (9~11):1.
Therefore, the fabric coating silicon rubber that Pass through above-mentioned technical proposal obtains is bi-component addition type liquid silastic, by A
Component and the mixing cured molding of B component, component A include：100 parts of base rubber, 8~18 parts of vinyl-terminated silicone fluid, 1~2 part of tackifier,
0.5 part of platinum catalyst；B component includes：20~70 parts of vinyl-terminated silicone fluid, 30~80 parts of containing hydrogen silicone oil, inhibitor 0.3~
0.5 part；Wherein, the raw material of base rubber includes：100 parts of vinyl-terminated silicone fluid, end-vinyl ethenyl of side chain silicone oil 5~10, gas phase
40 parts of method white carbon, 10~15 parts of silazane inorganic agent, 0~5 part of siloxane treated agent.
The present invention is greatly improved using vinyl-terminated silicone fluid as main component and abutting end vinyl sidechain vinyl silicone oil
The tensile strength and tearing strength of silicon rubber.Meanwhile the acid water that the tackifier that use of inventive formulation are organo-silicon coupling agent
Product is solved, can be chemically bonded with the hydroxyl of fabric surface, and there is good intermiscibility with liquid silastic and ooze
Permeability can be combined with fabric table securely, and then considerably increase the firmness that silicon rubber is adhered to fabric surface, vulcanization speed
Degree is fast, greatly increases the efficiency of production.
The present invention also provides the preparation method of above-mentioned bi-component addition type liquid silastic, process optimizations, with the present invention
Formula is with the use of the comprehensive performance for being greatly improved fabric coating silicon rubber of the present invention.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the specific technical solution of the present invention is clearly and completely described, is shown
So, described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.Based on the reality in the present invention
Apply example, those of ordinary skill in the art's all other embodiments obtained without making creative work all belong to
In the scope of protection of the invention.
Embodiment 1
1st, by the vinyl-terminated silicone fluid that 100 parts of viscosity are 20000mpa.s and the end-vinyl that 5 parts of viscosity is 1000mpa.s
Ethenyl of side chain silicone oil is added in kneader and is stirred evenly, and is then 300m by 40 parts of specific surface areas2The vapor phase method hard charcoal of/g
Black, 12 parts of silazane inorganic agents and 3 parts of water are added in kneading machine stir 3h in four times, then heat to 150 DEG C of heat treatment 2h,
Vacuum 2h again, discharging cross three-roll grinder, obtain base rubber.
2nd, 100 parts of base rubbers are taken, vinyl-terminated silicone fluid, 1 part of tackifier and platinum that 8 parts of viscosity are 20000mpa.s is added in and urges
0.5 part of agent (vinyl chromium complex 2000ppm) stirs 1h with 30rpm in planetary mixer and obtains component A to uniform.
3rd, it is 60 parts of vinyl-terminated silicone fluid, the containing hydrogen silicone oil 40 parts (hydrogen contents 0.5%) of 5000mpa.s and suppression by viscosity
0.36 part of alcohol stirs evenly to obtain B component to preparation 1- acetenyl 1- rings in high speed dispersor.
In use, by component A and B component by weight 10:1 mixing, is then coated on textile surface, is dried at 120 DEG C
Roasting 5min, you can to obtain certain thickness silica-gel coating, the liquid silastic is impermeable, strong with fabric surface cohesive force, interior
It is poly- to destroy.
Wherein, the silazane inorganic agent employed in the present embodiment is hexamethyldisilazane；Tackifier are methyl trimethoxy
Oxysilane and water are by weight 100:15 are mixed, and after reaction 5h under the action of acidic catalyst, remove low molecule
Obtained hydrolysate.Platinum catalyst is chloroplatinic acid complex compound, preferably chloroplatinic acid and divinyl tetramethyl disiloxane
Complex compound, platinum content are 500~10000ppm.
It is detected by experiment, the hardness for measuring the silica-gel coating is 40 degree, and tensile strength 5.1mpa, elongation reaches
330%, tearing strength 12KN/m, it is 66 to spring back.
Embodiment 2
1st, by the vinyl-terminated silicone fluid that 100 parts of viscosity are 10000mpa.s and the end-vinyl that 5 parts of viscosity is 1000mpa.s
Ethenyl of side chain silicone oil is added in kneader and is stirred evenly, and is then 300m by 40 parts of specific surface areas2The vapor phase method hard charcoal of/g
Black, 10 parts of silazane inorganic agents, 2 parts of siloxane treated agent and 3.5 parts of water add in 3h is stirred in kneading machine in four times, then heat up
Three-roll grinder is crossed, obtains base rubber to 150 DEG C of heat treatment 2h, then vacuum 2h, discharging.
2nd, 100 parts of base rubbers are taken, vinyl-terminated silicone fluid, 1 part of tackifier and platinum that 8 parts of viscosity are 10000mpa.s is added in and urges
0.5 part of agent (vinyl chromium complex 2000ppm) stirs 1h with 30rpm in planetary mixer and obtains component A to uniform.
3rd, it is 20 parts of vinyl-terminated silicone fluid, the containing hydrogen silicone oil 80 parts (hydrogen contents 0.25%) of 2000mpa.s and suppression by viscosity
0.36 part of alcohol stirs evenly to obtain B component to preparation 1- acetylene basic ring in high speed dispersor.
In use, by component A and B component by weight 9:1 mixing, is then coated on textile surface, is toasted at 60 DEG C
30min, you can to obtain certain thickness silica-gel coating, the liquid silastic is impermeable, strong with fabric surface cohesive force, cohesion
It destroys.
Wherein, the silazane inorganic agent employed in the present embodiment is hexamethyldisilazane, and siloxane treated agent is two
Methyldiethoxysilane, tackifier are the acidic hydrolysis object of vinyltriethoxysilane.Platinum catalyst is chloroplatinic acid network
The complex compound of object, preferably chloroplatinic acid and divinyl tetramethyl disiloxane is closed, platinum content is 500~10000ppm.
It is detected by experiment, the hardness for measuring the silica-gel coating is 32 degree, and tensile strength 5.2mpa, elongation reaches
320%, tearing strength 10KN/m, it is 57 to spring back.
Embodiment 3
1st, 100 parts of viscosity are added for the vinyl-terminated silicone fluid of 20000mpa.s and 5 parts of end-vinyl ethenyl of side chain silicone oil
Enter in kneader, be then 300m by 40 parts of specific surface areas2The fume colloidal silica of/g, 10 parts of silazane inorganic agents, 4 parts of silica
Alkane inorganic agent and 3.5 parts of water add in 3h is stirred in kneading machine in four times, then heat to 150 DEG C of heat treatment 2h, then vacuum 2h, mistake
Three-roll grinder obtains base rubber.
2nd, 100 parts of base rubbers are taken, add in vinyl-terminated silicone fluid, 1.5 parts of tackifier and platinum that 15 parts of viscosity are 10000mpa.s
0.5 part of Au catalyst (vinyl chromium complex 2000ppm) stirs 1h with 30rpm in planetary mixer and obtains component A to uniform.
3rd, it is 70 parts of vinyl-terminated silicone fluid, the containing hydrogen silicone oil 30 parts (hydrogen contents 0.8%) of 2000mpa.s and suppression by viscosity
0.4 part of alcohol stirs evenly to obtain B component to preparation 1- acetylene basic ring in high speed dispersor.
In use, by component A and B component by weight 11:1 mixing, is then coated on textile surface, is dried at 100 DEG C
Roasting 15min, you can to obtain certain thickness silica-gel coating, the silicon rubber is impermeable, and strong with fabric surface cohesive force, cohesion is broken
It is bad.
Wherein, the silazane inorganic agent employed in the present embodiment is 9 parts of hexamethyldisilazane and 1 part of tetramethyl diethyl
The mixture of alkenyl silazane；Siloxane treated agent is dimethyldimethoxysil,ne；Tackifier are methyltrimethoxysilane
With the acidic hydrolysis object of ethylene trimethoxy silane.Platinum catalyst is chloroplatinic acid complex compound, preferably chloroplatinic acid and divinyl
The complex compound of base tetramethyl disiloxane, platinum content are 500~10000ppm.
It is detected by experiment, the hardness for measuring the silica-gel coating is 39 degree, and tensile strength 7.12mpa, elongation reaches
472%, tearing strength 17.6, it is 66% to spring back.
Embodiment 4
1st, by the vinyl-terminated silicone fluid that 100 parts of viscosity are 20000mpa.s and the end-vinyl that 5 parts of viscosity is 3000mpa.s
Ethenyl of side chain silicone oil is added in kneader and is stirred evenly, and is then 300m by 40 parts of specific surface areas2The vapor phase method hard charcoal of/g
Black, 12 parts of silazane inorganic agents, 1 part of vinyl silazane inorganic agent, 1 part of siloxane treated agent and 3.5 parts of water add in four times
3h is stirred in kneading machine, then heats to 150 DEG C of heat treatment 2h, then vacuum 2h, discharging cross three-roll grinder, obtain base rubber.
2nd, 100 parts of base rubbers are taken, add in vinyl-terminated silicone fluid, 1 part of tackifier and platinum that 12 parts of viscosity are 50000mpa.s
0.5 part of catalyst (vinyl chromium complex 2000ppm) stirs 1h with 30rpm in planetary mixer and obtains component A to uniform.
3rd, it is 50 parts of vinyl-terminated silicone fluid, the containing hydrogen silicone oil 50 parts (hydrogen contents 0.5%) of 2000mpa.s and suppression by viscosity
0.5 part of alcohol stirs evenly to obtain B component to preparation 1- acetylene basic ring in high speed dispersor.
In use, by component A and B component by weight 9:1 mixing, is then coated on textile surface, is toasted at 80 DEG C
20min, you can to obtain certain thickness coating, the silicon rubber is impermeable, strong with fabric surface cohesive force, cohesional failure.
Wherein, the silazane inorganic agent employed in the present embodiment is hexamethyldisilazane and tetramethyl divinyl silicon
The mixture of azane；Siloxane treated agent is dimethyl diethoxysilane；Tackifier are the water of vinyltrimethoxysilane
Solve object.Complex compound of the platinum catalyst for chloroplatinic acid complex compound, preferably chloroplatinic acid and divinyl tetramethyl disiloxane, platinum
Content is 500~10000ppm.
It is detected by experiment, the hardness for measuring the fabric silica gel is 38 degree, and tensile strength 5.5mpa, elongation reaches
280%, tearing strength 11KN/m, it is 65 to spring back.
Embodiment 5
1st, by the vinyl-terminated silicone fluid that 100 parts of viscosity are 10000mpa.s and the end ethylene that 5 parts of viscosity are 50000mpa.s
Base side chain vinyl silicone oil is added in kneader and is stirred evenly, and is then 300m by 40 parts of specific surface areas2The vapor phase method hard charcoal of/g
Black, 12 parts of silazane inorganic agents, 2 parts of siloxane treated agent and 3 parts of water add in 3h is stirred in kneading machine in four times, then heat to
150 DEG C, 2h vacuum 2h are heat-treated, three-roll grinder is crossed, obtains base rubber.
2nd, 100 parts of base rubbers are taken, add in vinyl-terminated silicone fluid, 1 part of tackifier and platinum that 18 parts of viscosity are 10000mpa.s
0.5 part of catalyst (vinyl chromium complex 2000ppm) stirs 1h with 30rpm in planetary mixer and obtains component A to uniform.
3rd, it is 35 parts of vinyl-terminated silicone fluid, the containing hydrogen silicone oil 65 parts (hydrogen contents 0.36%) of 3000mpa.s and suppression by viscosity
0.5 part of alcohol stirs evenly to obtain B component to preparation 1- acetylene basic ring in high speed dispersor.
In use, by component A and B component by weight 10:1 mixing, is then coated on textile surface, is dried at 95 DEG C
Roasting 15min, you can to obtain certain thickness coating, the silicon rubber is impermeable, strong with fabric surface cohesive force, cohesional failure.
Wherein, the silazane inorganic agent employed in the present embodiment is hexamethyldisilazane, and siloxane treated agent is two
Methyldiethoxysilane, hydrolysate of the tackifier for vinyltriethoxysilane and methyl trimethoxy oxygroup.Platinum catalyst
For the complex compound of chloroplatinic acid complex compound, preferably chloroplatinic acid and divinyl tetramethyl disiloxane, platinum content for 500~
10000ppm。
It is detected by experiment, the hardness for measuring the fabric silica gel is 32 degree, and tensile strength 5.2mpa, elongation reaches
320%, tearing strength 10KN/m, it is 57 to spring back.
Embodiment 6
Fabric coating silicon rubber prepared by Example 1 to embodiment 5 carries out performance detection, and two kinds of commercially available bi-components is taken to add
The outer sample 1 of molding liquid silicon rubber and outer sample 2 are compareed as reference substance, and table 1 is performance test results.
Table 1
Claims (10)
1. a kind of bi-component addition type liquid silastic, by component A and the mixing cured molding of B component, which is characterized in that the A
Component includes：100 parts of base rubber, 8~18 parts of vinyl-terminated silicone fluid, 1~2 part of tackifier, 0.5 part of platinum catalyst；
The B component includes：20~70 parts of vinyl-terminated silicone fluid, 30~80 parts of containing hydrogen silicone oil, 0.3~0.5 part of inhibitor；
The raw material of the base rubber includes：100 parts of vinyl-terminated silicone fluid, end-vinyl ethenyl of side chain silicone oil 5~10, vapor phase method is white
40 parts of carbon black, 10~15 parts of silazane inorganic agent, 0~5 part of siloxane treated agent.
2. bi-component addition type liquid silastic according to claim 1, which is characterized in that the tackifier are vinyl
Trimethoxy silane, vinyltriethoxysilane, methyltrimethoxysilane, γ-glycidoxypropyl group trimethoxy silicon
Alkane, N- β-aminoethyl-γ-aminopropyltrimethoxysilane, γ-(methacryloxypropyl) propyl trimethoxy silicane and γ-ammonia
One or more hydrolysates in propyl-triethoxysilicane.
3. bi-component addition type liquid silastic according to claim 1, which is characterized in that the vinyl-terminated silicone fluid
Range of viscosities is 5000~100000cP, and contents of ethylene is 0.05%~0.5%；
The range of viscosities of the end-vinyl ethenyl of side chain silicone oil is 1000~80000cP, contents of ethylene for 0.5%~
5%；
The hydrogen content of the containing hydrogen silicone oil is 0.2%~1.2%.
4. bi-component addition type liquid silastic according to claim 1, which is characterized in that the silazane inorganic agent is
Hexamethyldisilazane or vinyl silazane；
The siloxane treated agent is dimethyldimethoxysil,ne or dimethyl diethoxysilane.
5. bi-component addition type liquid silastic according to claim 1, which is characterized in that the platinum catalyst is chlorine
The complex compound of platinic acid and divinyl tetramethyl disiloxane, platinum content are 500~10000ppm.
6. bi-component addition type liquid silastic according to claim 1, which is characterized in that the inhibitor is 1- acetylene
The mixture of base -1- cyclohexanol and 2- methyl -3- crotonylene alcohol.
7. the preparation method of bi-component addition type liquid silastic, feature exist described in a kind of claim 1 to 6 any one
In including the following steps：
A) by the mixture of the vinyl-terminated silicone fluid and end-vinyl ethenyl of side chain silicone oil and fume colloidal silica, silazane
Inorganic agent, siloxane treated agent and water are mixing, and are warming up to 145~155 DEG C and vacuumize, obtain the base rubber；
B) base rubber, vinyl-terminated silicone fluid, tackifier and platinum catalyst are mixed, obtains the component A；
C) vinyl-terminated silicone fluid, containing hydrogen silicone oil and 1- acetenyl -1- cyclohexanol are mixed, obtains the B component；
D) it is the component A and B component is mixing cured to get the bi-component addition type liquid silastic.
8. preparation method according to claim 7, which is characterized in that the addition of the step a) water is 3~4 weight
Part；
Described be blended in kneader carries out, and incorporation time is 3~5h.
9. preparation method according to claim 7, which is characterized in that step b) is described be blended in planetary stirring machine into
Row；
Rotating speed is 25~35rpm, and the time is 50~70min.
10. preparation method according to claim 1, which is characterized in that the step d) solidification temperatures are at 50 DEG C or more.
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