CN107778779A - A kind of preparation method of high-temp resisting high-humidity resisting mold glue - Google Patents
A kind of preparation method of high-temp resisting high-humidity resisting mold glue Download PDFInfo
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- CN107778779A CN107778779A CN201711150827.0A CN201711150827A CN107778779A CN 107778779 A CN107778779 A CN 107778779A CN 201711150827 A CN201711150827 A CN 201711150827A CN 107778779 A CN107778779 A CN 107778779A
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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
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
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Abstract
The invention belongs to mold glue processing technique field, and in particular to a kind of preparation method of high-temp resisting high-humidity resisting mold glue, including batch mixing suction filtration, hot-pressing processing and the several steps of obtained mold glue.The present invention has advantages below compared with prior art:Pass through hot pressing after raw material is filtered under vacuum in the present invention, help to make coordination plasticizing between raw material, prepared mold glue percent thermal shrinkage substantially reduces, with stronger heat endurance, contribute to the raising of product surface flatness, extend the mold use life-span, preparation method is easily controlled, suitable for promoting the use of.
Description
Technical field
The invention belongs to mold glue processing technique field, and in particular to a kind of preparation method of high-temp resisting high-humidity resisting mold glue.
Background technology
Silica gel dedicated for production technology product mould is referred to as mold glue, typically with room temperature vulcanized silicone rubber (abbreviation RTV)
Manufacture, RTV is a kind of macromolecular elastomer, and it is the synthetic material using silicon atom and oxygen atom as skeleton, on each silicon atom
It is a kind of fibrous polymer polymer with Si-O-Si chain belts containing 1~2 organic group (mainly methyl).Cause
This, RTV has the following properties that:Good chemical stability, nontoxic, non-corrosiveness;Good fluidity, mould can be full of automatically;Can
Curingprocess rate is controlled, is vulcanized under room temperature normal pressure, good release property easy to operation;Simulation quality is strong, and decorative pattern is true to nature;Molding speed
It hurry up, mould can be made into general 20 hours.
But found during long-term use, under the conditions of hot and humid, the RTV moulds of existing mold glue manufacture
Percent thermal shrinkage is larger, and dimensional stability is poor, and heat resistance difference have impact on the decorative pattern fineness and outward appearance of manufactured product, and lead
Cause die life shorter, substantially increase the production cost of enterprise.
The content of the invention
The purpose of the present invention is to be directed to the problem of existing, there is provided a kind of preparation method of high-temp resisting high-humidity resisting mold glue.
The present invention is achieved by the following technical solutions:A kind of preparation method of high-temp resisting high-humidity resisting mold glue, including with
Lower content:
(1)By weight, 8-12 parts PPG, 4-7 parts modified molecular screen, 15-20 parts talcum powder, 4-8 part gas phases are taken
Silica, 12-15 parts octadecyl carbamate, the mixing of 1-3 parts benzene sulfonic acid, the ultrasonic disperse in ethanol solution
30-40 minutes, then filtered in the condition that vacuum is 0.045-0.065MPa, stop taking out when filtering out there is no ethanol
Filter, much filtrate is taken out, it is 10-15% to be dried to water content under conditions of being 40-50 DEG C in temperature;
(2)Added in above-mentioned dried object equivalent to 6-8 part Methyl Hydrogen Polysiloxane Fluids, in temperature be 55-65 DEG C after stirring
Under the conditions of heat 18-25 minutes, the then hot pressing 40-60 point under conditions of pressure is 3.5-4.5MPa, temperature is 120-140 DEG C
Clock, after the completion of naturally cool to room temperature, obtain mix rubber powder it is standby;
(3)Melted after gained mixing rubber powder is mixed with the multifunctional glycidol type epoxy resin of 45-55 parts in single screw extrusion machine
Melt it is compound, temperature be 55-65 DEG C under conditions of solidification obtain mold glue.
As further improvement of these options, the step(1)Ultrasonic frequency is 45- during middle ultrasonic disperse
65kHz。
As further improvement of these options, the hydrogen content of the Methyl Hydrogen Polysiloxane Fluid is 1.2-1.6%, viscosity is
200-400mPa。
As further improvement of these options, the preparation method of the modified molecular screen be by molecular sieve with equivalent to
The absolute ethyl alcohol mixing of 4-6 times of its weight, ultrasonic disperse 20-30 minutes, is then added equivalent to molecular sieve 4.5-7.8%
Ammonium persulfate and 1.2-1.8% chlorosulfonic acid, temperature be 45-55 DEG C under conditions of stirring reaction 4-6 hours, Ran Hou
Centrifuged under conditions of 1000-1200 revs/min, obtain solid product, after being washed 3-5 times with absolute ethyl alcohol, in 120-140
Vacuum drying 2-4 hours produce under conditions of DEG C.
As further improvement of these options, described PPG is 7 by weight ratio:5:1 polyoxygenated third
The alcohol ether of allyl three, polytetrahydrofuran diol and rosin polyester polyhydric-alcohol mix.
The present invention has advantages below compared with prior art:By hot after raw material is filtered under vacuum in the present invention
Pressure, help to make coordination plasticizing between raw material, prepared mold glue percent thermal shrinkage substantially reduces, and has stronger thermostabilization
Property, contribute to the raising of product surface flatness, extend the mold use life-span, preparation method is easily controlled, and is made suitable for promoting
With.
Embodiment
Embodiment 1
A kind of preparation method of high-temp resisting high-humidity resisting mold glue, including herein below:
(1)By weight, take 10 parts of PPGs, 6 parts of modified molecular screens, 17 parts of talcum powder, 6 parts of aerosils,
14 parts of octadecyl carbamates, 2 parts of benzene sulfonic acid mixing, ultrasonic disperse 35 minutes, ultrasonic disperse in ethanol solution
When ultrasonic frequency be 55kHz, then vacuum be 0.055MPa condition filtered, stop when being filtered out there is no ethanol
Only filter, take out much filtrate, it is 12% to be dried to water content under conditions of being 45 DEG C in temperature;
(2)Equivalent to 7 parts Methyl Hydrogen Polysiloxane Fluids are added in above-mentioned dried object, after stirring under conditions of temperature is 60 DEG C
Heating 20 minutes, then hot pressing 50 minutes under conditions of pressure is 4MPa, temperature is 130 DEG C, after the completion of naturally cool to room
Temperature, it is standby to obtain mixing rubber powder;
(3)It is multiple in single screw extrusion machine melting after gained mixing rubber powder is mixed with 50 parts of multifunctional glycidol type epoxy resin
Close, solidify under conditions of being 60 DEG C in temperature and obtain mold glue.
Wherein, the hydrogen content of the Methyl Hydrogen Polysiloxane Fluid be 1.4%, viscosity 300mPa;The preparation of the modified molecular screen
Method is mixes molecular sieve with absolute ethyl alcohol of 5 times equivalent to its weight, ultrasonic disperse 25 minutes, then adds equivalent to dividing
The ammonium persulfate and 1.5% chlorosulfonic acid of son sieve weight 6.2%, stirring reaction 5 hours, Ran Hou under conditions of being 50 DEG C in temperature
Centrifuged under conditions of 1100 revs/min, obtain solid product, after washing 4 times with absolute ethyl alcohol, under conditions of 130 DEG C
Vacuum drying produces for 3 hours;Described PPG is 7 by weight ratio:5:1 polyoxypropylene glycerol ether, poly- tetrahydrochysene
Furans glycol and rosin polyester polyhydric-alcohol mix.
By ASTM D696-2003, using ZRPY-300 thermomechanical analyzers, STA-PT1000 thermal gravimetric analyzers, detection
The heat resistance of mold glue is 627 DEG C in the present embodiment, and linear expansion coefficient is 1.9 × 10-6, linear expansion coefficient is 3.4 × 10-6。
Embodiment 2
A kind of preparation method of high-temp resisting high-humidity resisting mold glue, including herein below:
(1)By weight, 8 parts of PPGs, 7 parts of modified molecular screens, 15 parts of talcum powder, 8 parts of aerosils, 12 are taken
Part octadecyl carbamate, 3 parts of benzene sulfonic acids mixing, ultrasonic disperse 40 minutes in ethanol solution, during ultrasonic disperse
Ultrasonic frequency is 45kHz, is then filtered in the condition that vacuum is 0.065MPa, stopped when being filtered out there is no ethanol
Filter, take out much filtrate, it is 15% to be dried to water content under conditions of being 40 DEG C in temperature;
(2)Equivalent to 8 parts Methyl Hydrogen Polysiloxane Fluids are added in above-mentioned dried object, after stirring under conditions of temperature is 65 DEG C
Heating 18 minutes, then hot pressing 60 minutes under conditions of pressure is 3.5MPa, temperature is 140 DEG C, after the completion of naturally cool to
Room temperature, it is standby to obtain mixing rubber powder;
(3)It is multiple in single screw extrusion machine melting after gained mixing rubber powder is mixed with 45 parts of multifunctional glycidol type epoxy resin
Close, solidify under conditions of being 65 DEG C in temperature and obtain mold glue.
Wherein, the hydrogen content of the Methyl Hydrogen Polysiloxane Fluid be 1.2%, viscosity 400mPa;The preparation of the modified molecular screen
Method is mixes molecular sieve with absolute ethyl alcohol of 4 times equivalent to its weight, ultrasonic disperse 30 minutes, then adds equivalent to dividing
The ammonium persulfate and 1.2% chlorosulfonic acid of son sieve weight 4.5%, stirring reaction 4 hours, Ran Hou under conditions of being 55 DEG C in temperature
Centrifuged under conditions of 1000 revs/min, obtain solid product, after washing 5 times with absolute ethyl alcohol, under conditions of 120 DEG C
Vacuum drying produces for 4 hours;Described PPG is 7 by weight ratio:5:1 polyoxypropylene glycerol ether, poly- tetrahydrochysene
Furans glycol and rosin polyester polyhydric-alcohol mix.
By ASTM D696-2003, using ZRPY-300 thermomechanical analyzers, STA-PT1000 thermal gravimetric analyzers, detection
The heat resistance of mold glue is 627 DEG C in the present embodiment, and linear expansion coefficient is 1.8 × 10-6, linear expansion coefficient is 3.2 × 10-6。
Embodiment 3
A kind of preparation method of high-temp resisting high-humidity resisting mold glue, including herein below:
(1)By weight, take 12 parts of PPGs, 4 parts of modified molecular screens, 20 parts of talcum powder, 4 parts of aerosils,
15 parts of octadecyl carbamates, 1 part of benzene sulfonic acid mixing, ultrasonic disperse 30 minutes, ultrasonic disperse in ethanol solution
When ultrasonic frequency be 65kHz, then vacuum be 0.045MPa condition filtered, stop when being filtered out there is no ethanol
Only filter, take out much filtrate, it is 10% to be dried to water content under conditions of being 50 DEG C in temperature;
(2)Equivalent to 6 parts Methyl Hydrogen Polysiloxane Fluids are added in above-mentioned dried object, after stirring under conditions of temperature is 55 DEG C
Heating 25 minutes, then hot pressing 40 minutes under conditions of pressure is 4.5MPa, temperature is 120 DEG C, after the completion of naturally cool to
Room temperature, it is standby to obtain mixing rubber powder;
(3)It is multiple in single screw extrusion machine melting after gained mixing rubber powder is mixed with 55 parts of multifunctional glycidol type epoxy resin
Close, solidify under conditions of being 55 DEG C in temperature and obtain mold glue.
Wherein, the hydrogen content of the Methyl Hydrogen Polysiloxane Fluid be 1.6%, viscosity 200mPa;The preparation of the modified molecular screen
Method is mixes molecular sieve with absolute ethyl alcohol of 6 times equivalent to its weight, ultrasonic disperse 20 minutes, then adds equivalent to dividing
The ammonium persulfate and 1.8% chlorosulfonic acid of son sieve weight 7.8%, stirring reaction 6 hours, Ran Hou under conditions of being 45 DEG C in temperature
Centrifuged under conditions of 1200 revs/min, obtain solid product, after washing 3 times with absolute ethyl alcohol, under conditions of 140 DEG C
Vacuum drying produces for 2 hours;Described PPG is 7 by weight ratio:5:1 polyoxypropylene glycerol ether, poly- tetrahydrochysene
Furans glycol and rosin polyester polyhydric-alcohol mix.
By ASTM D696-2003, using ZRPY-300 thermomechanical analyzers, STA-PT1000 thermal gravimetric analyzers, detection
The heat resistance of mold glue is 627 DEG C in the present embodiment, and linear expansion coefficient is 2.1 × 10-6, linear expansion coefficient is 3.5 × 10-6。
Claims (5)
1. a kind of preparation method of high-temp resisting high-humidity resisting mold glue, it is characterised in that including herein below:
(1)By weight, 8-12 parts PPG, 4-7 parts modified molecular screen, 15-20 parts talcum powder, 4-8 part gas phases are taken
Silica, 12-15 parts octadecyl carbamate, the mixing of 1-3 parts benzene sulfonic acid, the ultrasonic disperse in ethanol solution
30-40 minutes, then filtered in the condition that vacuum is 0.045-0.065MPa, stop taking out when filtering out there is no ethanol
Filter, much filtrate is taken out, it is 10-15% to be dried to water content under conditions of being 40-50 DEG C in temperature;
(2)Added in above-mentioned dried object equivalent to 6-8 part Methyl Hydrogen Polysiloxane Fluids, in temperature be 55-65 DEG C after stirring
Under the conditions of heat 18-25 minutes, the then hot pressing 40-60 point under conditions of pressure is 3.5-4.5MPa, temperature is 120-140 DEG C
Clock, after the completion of naturally cool to room temperature, obtain mix rubber powder it is standby;
(3)Melted after gained mixing rubber powder is mixed with the multifunctional glycidol type epoxy resin of 45-55 parts in single screw extrusion machine
Melt it is compound, temperature be 55-65 DEG C under conditions of solidification obtain mold glue.
A kind of 2. preparation method of high-temp resisting high-humidity resisting mold glue as claimed in claim 1, it is characterised in that the step(1)In
Ultrasonic frequency is 45-65kHz during ultrasonic disperse.
A kind of 3. preparation method of high-temp resisting high-humidity resisting mold glue as claimed in claim 1, it is characterised in that the methyl hydrogen silicon
The hydrogen content of oil is 1.2-1.6%, viscosity 200-400mPa.
A kind of 4. preparation method of high-temp resisting high-humidity resisting mold glue as claimed in claim 1, it is characterised in that the modified molecular screen
Preparation method for molecular sieve is mixed with absolute ethyl alcohol of 4-6 times equivalent to its weight, ultrasonic disperse 20-30 minutes, then
The chlorosulfonic acid of the ammonium persulfate and 1.2-1.8% equivalent to molecular sieve 4.5-7.8% is added, in the bar that temperature is 45-55 DEG C
Stirring reaction 4-6 hours, then centrifuge under conditions of 1000-1200 revs/min under part, obtain solid product, with nothing
Water-ethanol wash 3-5 time after, under conditions of 120-140 DEG C vacuum drying 2-4 hours produce.
A kind of 5. preparation method of high-temp resisting high-humidity resisting mold glue as claimed in claim 1, it is characterised in that described polyether polyols
Alcohol is 7 by weight ratio:5:1 polyoxypropylene glycerol ether, polytetrahydrofuran diol and rosin polyester polyhydric-alcohol mixes.
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Citations (1)
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CN104177775A (en) * | 2014-07-30 | 2014-12-03 | 宁国市冠宇模具有限公司 | Epoxy resin mold having relatively long service life |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN104177775A (en) * | 2014-07-30 | 2014-12-03 | 宁国市冠宇模具有限公司 | Epoxy resin mold having relatively long service life |
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Application publication date: 20180309 |