CN110373034A - A kind of preparation method of high temperature resistance and high strength isolation film - Google Patents
A kind of preparation method of high temperature resistance and high strength isolation film Download PDFInfo
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- C08K2003/2241—Titanium dioxide
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Abstract
The present invention relates to a kind of preparation methods of high temperature resistance and high strength isolation film, belong to isolation technical field of membrane.Reed Leaves are passed through lye by the present invention, acid soak separates the plant fiber component in reed Leaves, graphite powder is added, graphene oxide is generated by hydrogen peroxide oxidation in sulfuric acid solution, make the negatively charged oxygen atom outside ring, reducing property is reinforced, make cellulose, plant fiber dissolution is more abundant, reinforce isolation film internal crosslinking degree, improve the mechanical strength and mechanical strength of isolation film, the present invention prepares nano-titanium dioxide using butyl titanate, titanium dioxide is introduced into isolation film, titanium dioxide molecular structure stabilized itself, heat resistance is good, further strengthen the heat resistance of isolation film, mechanical property and mechanical strength, prepared titanium dioxide has porous structure simultaneously, the enhancing of hole is conducive to reinforce the electric conductivity and contact area of isolation film, to make the electric conductivity of isolation film, heat resistance is strengthened with mechanical strength , have a good application prospect.
Description
Technical field
The present invention relates to a kind of preparation methods of high temperature resistance and high strength isolation film, belong to isolation technical field of membrane.
Background technique
Using polymer as the high molecular products high-temperature molding of substrate after processing is completed, need product and mold quick and smooth
Ground is detached from, to guarantee quality of item and improve manufacture efficiency.For this purpose, needing to increase a kind of material between product and processing mold
Effect is detached to improve.Release agent and isolation film can play the role of this kind, but release agent sprinkling uniformity is poor and appearance
Product and environment are easily stain, isolation film is opposite to improve production efficiency, and minimizes to the pollution of environment.
Common isolation film has PE isolation film and PET isolation film, uses PE/PET plastic film for substrate, its surface into
Row plasma treatment, the processing of painting fluorine or painting silicone oil are handled.Due to the property of polymer itself, PE isolation film can only be resistant to temperature
Degree is not higher than 120 DEG C of low temperature；Though PET isolation film will can significantly shrink generation at 160 DEG C with resistance to 200 DEG C of high temperature
Fold is used only once, and cannot be reused, be caused huge waste.
The isolation film of existing preparation is produced isolation film through extruder, is substituted release agent, mentioned using perfluoroethylene-propylene
High positive benefit.The fusing point of perfluoroethylene-propylene 265 DEG C or more and fluorine content it is higher, the isolation film have preferable high temperature resistant
Performance and demolding performace.The problem is that the isolation film processing conditions is more harsh, and material cost is very high, is suitable for high property
Energy product scope is restricted in the application of general purpose rubber industry.It include polyester film substrate and separation layer there are also isolation film, every
The composition of absciss layer coating is Organosilicon Release Agent, catalyst, crosslinking agent, solvent and antistatic agent component.The composition one of interleaving agent
As be made of organic siliconresin, crosslinking agent, curing accelerator and organic solvent.Production method be coated on polyester base material it is organic
Silicon interleaving agent is dried to obtain isolation film product.Organic siliconresin is a kind of linear polymeric resin, after being coated on substrate surface
It can migrate, influence anti-adhesion effects, crosslinking agent has been used to make to carry out appropriately crosslinked formation network knot when interleaving agent is dry thus
Structure.The isolation film has preferable effect for the disposable demoulding of heat product and cost is also more cheap.The problem is that
Polyester film substrate is due to the defect of processing technology, and high temperature isolation is using once will generating many gauffers, again because of being heat-shrinked
When secondary use a large amount of wrinkle, the appearance and service performance of the product of influence can be formed in product surface.
Such as a kind of isolation film of related patent and its production technology, using perfluoroethylene-propylene, under the conditions of 350-395 DEG C,
Isolation film is produced through extruder, release agent is substituted, improves positive benefit.The fusing point of perfluoroethylene-propylene at 265 DEG C or more and
Fluorine content is higher, which has preferable high temperature resistance and demolding performace.The problem is that the isolation film processes item
Part is more harsh, and material cost is very high, is suitable for premium quality product field, is restricted in the application of general purpose rubber industry.
A kind of polyester insulating film of patent, the isolation film include polyester film substrate and separation layer, and the composition of separation layer coating is organosilicon
Interleaving agent, catalyst, crosslinking agent, solvent and antistatic agent component.The composition of interleaving agent generally by organic siliconresin, crosslinking agent,
Curing accelerator and organic solvent composition.The isolation film has preferable effect and cost for the disposable demoulding of heat product
Also more cheap.The problem is that defect of the polyester film substrate due to processing technology, high temperature isolation is using once will be because
A large amount of wrinkle can be formed in product surface when generating many gauffers to be heat-shrinked, reuse, the appearance of the product of influence and
Service performance.
Therefore, inventing the isolation film that a kind of heat-resisting quantity is good and intensity is high has actively meaning to isolation film preparation technical field
Justice.
Summary of the invention
The technical problems to be solved by the invention: bad for current high temperature resistance, mechanical property, mechanical strength be not high
Defect, provide a kind of preparation method of high temperature resistance and high strength isolation film.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of high temperature resistance and high strength isolation film the preparation method comprises the following steps:
Reaction lotion is put into vacuum oven, it is dense under conditions of temperature is 70~74 DEG C, vacuum degree is 110~120Pa
Enriched product is made in the dry 35~45min that contracts, and extruding pelletization in enriched product investment double screw extruder is made and squeezes out product,
By squeeze out product be placed in hot press, temperature be 200~220 DEG C, compacting pressure be 20~22MPa under conditions of compacting 40~
High temperature resistance and high strength isolation film is made after natural cooling by 50min；
React lotion the preparation method comprises the following steps:
(1) it weighs in butyl titanate, glacial acetic acid and dehydrated alcohol investment beaker, with blender with 1200~1300r/min's
Revolving speed stirs, and the hydrochloric acid that dimethylformamide and mass fraction are 10~12% is added in whipping process into beaker, is mixed
Mixed glue solution is made after 50~52h；
(2) by mixed glue solution with react suspension investment reaction kettle in be uniformly mixed obtain prefabricated mixed liquor, into reaction kettle
The N-methylmorpholine aqueous solution that mass fraction is 15~17% is added, increases reactor temperature to 70~74 DEG C, constant temperature stands 80
Reaction lotion is made in~90min；
React suspension the preparation method comprises the following steps:
(1) it weighs and is crushed in the reed Leaves investment pulverizer of 600~800g, the reed Leaves crushed are put into beaker, matter is used
The sodium hydroxide solution that amount score is 6~8% impregnates the reed Leaves crushed, and placing the beaker bath temperature is 60~64 DEG C
In water-bath, constant temperature impregnates 4~5h, and mixing suspension is made；
(2) graphite powder is put into beaker, and 60~80min is mixed with the revolving speed of 900~950r/min with blender and is made
Mixed serum is put into three-necked flask to be uniformly mixed to be made and be mixed by mixed serum with the sulfuric acid solution that mass fraction is 80~84%
Close liquid；
(3) three-necked flask is placed in ice-water bath, it is molten that the hydrogen peroxide that mass fraction is 18~20% is added dropwise into three-necked flask
Three-necked flask is placed in sonic oscillation instrument by liquid, and reaction solution is made in 2~3h of oscillation under conditions of frequency is 35~37kHz, to
The alumina powder of reaction solution quality 10~12% is added in three-necked flask, reaction suspension is made after standing 3~4h.
Temperature in double screw extruder is 130~140 DEG C, and revolving speed is 80~100r/min.
It reacts in the preparation method of lotion according to parts by weight, the butyl titanate is 8~10 parts, glacial acetic acid is
2.4~2.6 parts, the salt that dehydrated alcohol is 14~16 parts, dimethylformamide is 0.4~0.6 part, mass fraction is 10~12%
Acid is 3.0~3.4 parts.
React lotion preparation method in mixed glue solution with the mass ratio for react suspension be 1:3.
It is water-soluble to react the N-methylmorpholine that the mass fraction being added in the preparation method of lotion into reaction kettle is 15~17%
The quality of liquid is the 10~12% of prefabricated mixed liquor quality.
The quality for reacting the graphite powder put into the preparation method of suspension into beaker is the 10 of mixing suspension quality
~12%.
Reacting the mass ratio of sulfuric acid solution that mixed serum is 80~84% with mass fraction in the preparation method of suspension is
3:5。
It is molten to react the hydrogen peroxide that the mass fraction being added dropwise in the preparation method of suspension into three-necked flask is 18~20%
The quality of liquid is the 20~22% of mixed liquor quality, and the quality for the alumina powder being added into three-necked flask is reaction solution quality
10~12%.
The method have the benefit that:
The present invention first crushes reed Leaves, is heated and is impregnated with lye, and graphite powder is added after immersion and is mixed to prepare with sulfuric acid mixed
Liquid is closed, then to hydrogenperoxide steam generator sonic oscillation is added in mixed liquor, aluminium ion is introduced after oscillation and is mixed to prepare and reacts suspended
Then butyl titanate and glacial acetic acid, dehydrated alcohol are mixed, hydrochloric acid, dimethylformamide are added in whipping process by liquid
It is mixed with mixed glue solution, finally mixes mixed glue solution with suspension is reacted, N-methylmorpholine aqueous solution pyroreaction is added,
High temperature resistance and high strength isolation film is obtained using vacuum concentration, extruding pelletization, hot pressing, reed Leaves are passed through lye, acid by the present invention
Liquid impregnates the plant fiber component in separation reed Leaves, and graphite powder is added and generates oxidation stone by hydrogen peroxide oxidation in sulfuric acid solution
Black alkene is adsorbed on reed plant fiber, improves the mechanical strength of fiber, and plant fiber is carbonized in the environment of sulfuric acid, raw
At carbon fiber, carbon fiber helps to improve the electric conductivity of isolation film, is fitted into graphene oxide in carbon fiber, more further strengthens
Electric conductivity, simultaneous oxidation graphene are also dispersed in isolation film, can improve the electric conductivity of isolation film, this hair comprehensively
It is bright also to utilize N-methylmorpholine aqueous dissolution reed Leaves, the N-O key having in N-methylmorpholine aqueous solution, N-O key fracture chance
Water binding performance hydrogen bond makes the negatively charged oxygen atom outside ring, and reducing property is reinforced, and makes cellulose, plant fiber dissolution more
Sufficiently, each molecule in more group bonding isolation films is generated, reinforces isolation film internal crosslinking degree, improves the mechanics of isolation film
Intensity and mechanical strength, the present invention prepare nano-titanium dioxide using butyl titanate, and titanium dioxide is introduced into isolation film, and two
Titanium oxide molecular structure stabilized itself, heat resistance is good, and the heat resistance, mechanical property and machinery for further strengthening isolation film are strong
Degree, while prepared titanium dioxide has porous structure, the enhancing of hole is conducive to reinforce the electric conductivity of isolation film and connect
Contacting surface product, so that the electric conductivity of isolation film, heat resistance and mechanical strength be made to be strengthened, has a good application prospect.
Specific embodiment
It weighs and is crushed in the reed Leaves investment pulverizer of 600~800g, the reed Leaves crushed are put into beaker, matter is used
The sodium hydroxide solution that amount score is 6~8% impregnates the reed Leaves crushed, and placing the beaker bath temperature is 60~64 DEG C
In water-bath, constant temperature impregnates 4~5h, and mixing suspension is made；Mixing suspension quality 10~12% is put into above-mentioned beaker
Graphite powder is mixed 60~80min with blender with the revolving speed of 900~950r/min and mixed serum is made, by mixed serum
It puts into three-necked flask to be uniformly mixed with the sulfuric acid solution 3:5 in mass ratio that mass fraction is 80~84% and mixed liquor is made；By three
Mouth flask is placed in ice-water bath, and the mass fraction that mixed liquor quality 20~22% is added dropwise in Xiang Shangshu three-necked flask is 18~20%
Three-necked flask is placed in sonic oscillation instrument by hydrogenperoxide steam generator, and 2~3h system is vibrated under conditions of frequency is 35~37kHz
Reaction solution is obtained, the alumina powder of reaction solution quality 10~12% is added into three-necked flask, obtained reaction is hanged after standing 3~4h
Turbid, it is spare；According to parts by weight, 8~10 parts of butyl titanates, 2.4~2.6 parts of glacial acetic acid and 14~16 parts of anhydrous second are weighed
Alcohol is put into beaker, is stirred with blender with the revolving speed of 1200~1300r/min, it is added 0.4 in whipping process into beaker~
The hydrochloric acid that 0.6 part of dimethylformamide and 3.0~3.4 parts of mass fractions are 10~12% is made mixed after 50~52h is mixed
Close glue；By above-mentioned mixed glue solution with it is spare react be uniformly mixed in suspension 1:3 in mass ratio investment reaction kettle obtain it is pre-
The N-methylmorpholine water that the mass fraction of prefabricated mixed liquor quality 10~12% is 15~17% is added into reaction kettle for mixed liquor processed
Solution increases reactor temperature to 70~74 DEG C, and constant temperature stands 80~90min, and reaction lotion is made；By above-mentioned reaction lotion
It puts into vacuum oven, 35~45min is concentrated and dried under conditions of temperature is 70~74 DEG C, vacuum degree is 110~120Pa
Be made enriched product, by enriched product put into double screw extruder in temperature be 130~140 DEG C, revolving speed be 80~100r/
Extruding pelletization, which is made, under conditions of min squeezes out product, will squeeze out product and is placed in hot press, is 200~220 DEG C in temperature, pressure
Pressure processed suppresses 40~50min under conditions of being 20~22MPa, high temperature resistance and high strength isolation film is made after natural cooling.
Example 1
React the preparation of suspension:
It weighs and is crushed in the reed Leaves investment pulverizer of 600g, the reed Leaves crushed are put into beaker, are with mass fraction
6% sodium hydroxide solution impregnates the reed Leaves crushed, places the beaker in the water-bath that bath temperature is 60 DEG C, constant temperature leaching
4h is steeped, mixing suspension is made；
The graphite powder that mixing suspension quality 10% is put into above-mentioned beaker is stirred with blender with the revolving speed mixing of 900r/min
It mixes 60min and mixed serum is made, the sulfuric acid solution 3:5 in mass ratio that mixed serum and mass fraction are 80% is put into three mouthfuls of burnings
Obtained mixed liquor is uniformly mixed in bottle；
Three-necked flask is placed in ice-water bath, the mass fraction that mixed liquor quality 20% is added dropwise in Xiang Shangshu three-necked flask is 18%
Three-necked flask is placed in sonic oscillation instrument by hydrogenperoxide steam generator, and reaction is made in oscillation 2h under conditions of frequency is 35kHz
The alumina powder of reaction solution quality 10% is added into three-necked flask for liquid, and reaction suspension is made after standing 3h, spare；
React the preparation of lotion:
According to parts by weight, it weighs in 8 parts of butyl titanates, 2.4 parts of glacial acetic acid and 14 parts of dehydrated alcohol investment beakers, with stirring
Device is stirred with the revolving speed of 1200r/min, and 0.4 part of dimethylformamide and 3.0 parts of quality point is added in whipping process into beaker
Mixed glue solution is made after 50h is mixed in the hydrochloric acid that number is 10%；
Above-mentioned mixed glue solution is uniformly mixed in suspension 1:3 in mass ratio investment reaction kettle with spare reacting and obtains prefabricated mix
Liquid is closed, the N-methylmorpholine aqueous solution that the mass fraction of prefabricated mixed liquor quality 10% is 15% is added into reaction kettle, is increased anti-
Answer temperature in the kettle to 70 DEG C, constant temperature stands 80min, and reaction lotion is made；
The preparation of high temperature resistance and high strength isolation film:
Above-mentioned reaction lotion is put into vacuum oven, is concentrated and dried under conditions of temperature is 70 DEG C, vacuum degree is 110Pa
Enriched product is made in 35min, by enriched product put into double screw extruder in temperature be 130 DEG C, revolving speed be 80r/min item
Extruding pelletization, which is made, under part squeezes out product, will squeeze out product and is placed in hot press, is 200 DEG C in temperature, compacting pressure is 20MPa
Under conditions of suppress 40min, high temperature resistance and high strength isolation film is made after natural cooling.
Example 2
React the preparation of suspension:
It weighs and is crushed in the reed Leaves investment pulverizer of 700g, the reed Leaves crushed are put into beaker, are with mass fraction
7% sodium hydroxide solution impregnates the reed Leaves crushed, places the beaker in the water-bath that bath temperature is 62 DEG C, constant temperature leaching
4.5h is steeped, mixing suspension is made；
The graphite powder that mixing suspension quality 11% is put into above-mentioned beaker is stirred with blender with the revolving speed mixing of 920r/min
It mixes 70min and mixed serum is made, the sulfuric acid solution 3:5 in mass ratio that mixed serum and mass fraction are 82% is put into three mouthfuls of burnings
Obtained mixed liquor is uniformly mixed in bottle；
Three-necked flask is placed in ice-water bath, the mass fraction that mixed liquor quality 21% is added dropwise in Xiang Shangshu three-necked flask is 19%
Three-necked flask is placed in sonic oscillation instrument by hydrogenperoxide steam generator, and reaction is made in oscillation 2.5h under conditions of frequency is 36kHz
The alumina powder of reaction solution quality 11% is added into three-necked flask for liquid, and reaction suspension is made after standing 3.5h, spare；
React the preparation of lotion:
According to parts by weight, it weighs in 9 parts of butyl titanates, 2.5 parts of glacial acetic acid and 15 parts of dehydrated alcohol investment beakers, with stirring
Device is stirred with the revolving speed of 1250r/min, and 0.5 part of dimethylformamide and 3.5 parts of quality point is added in whipping process into beaker
Mixed glue solution is made after 51h is mixed in the hydrochloric acid that number is 11%；
Above-mentioned mixed glue solution is uniformly mixed in suspension 1:3 in mass ratio investment reaction kettle with spare reacting and obtains prefabricated mix
Liquid is closed, the N-methylmorpholine aqueous solution that the mass fraction of prefabricated mixed liquor quality 11% is 16% is added into reaction kettle, is increased anti-
Answer temperature in the kettle to 72 DEG C, constant temperature stands 85min, and reaction lotion is made；
The preparation of high temperature resistance and high strength isolation film:
Above-mentioned reaction lotion is put into vacuum oven, is concentrated and dried under conditions of temperature is 72 DEG C, vacuum degree is 115Pa
Enriched product is made in 40min, by enriched product put into double screw extruder in temperature be 135 DEG C, revolving speed be 90r/min item
Extruding pelletization, which is made, under part squeezes out product, will squeeze out product and is placed in hot press, is 210 DEG C in temperature, compacting pressure is 21MPa
Under conditions of suppress 45min, high temperature resistance and high strength isolation film is made after natural cooling.
Example 3
React the preparation of suspension:
It weighs and is crushed in the reed Leaves investment pulverizer of 800g, the reed Leaves crushed are put into beaker, are with mass fraction
8% sodium hydroxide solution impregnates the reed Leaves crushed, places the beaker in the water-bath that bath temperature is 64 DEG C, constant temperature leaching
5h is steeped, mixing suspension is made；
The graphite powder that mixing suspension quality 12% is put into above-mentioned beaker is stirred with blender with the revolving speed mixing of 950r/min
It mixes 80min and mixed serum is made, the sulfuric acid solution 3:5 in mass ratio that mixed serum and mass fraction are 84% is put into three mouthfuls of burnings
Obtained mixed liquor is uniformly mixed in bottle；
Three-necked flask is placed in ice-water bath, the mass fraction that mixed liquor quality 22% is added dropwise in Xiang Shangshu three-necked flask is 20%
Three-necked flask is placed in sonic oscillation instrument by hydrogenperoxide steam generator, and reaction is made in oscillation 3h under conditions of frequency is 37kHz
The alumina powder of reaction solution quality 12% is added into three-necked flask for liquid, and reaction suspension is made after standing 4h, spare；
React the preparation of lotion:
According to parts by weight, it weighs in 10 parts of butyl titanates, 2.6 parts of glacial acetic acid and 16 parts of dehydrated alcohols investment beakers, with stirring
It mixes device to stir with the revolving speed of 1300r/min, 0.6 part of dimethylformamide and 3.4 parts of quality is added in whipping process into beaker
Mixed glue solution is made after 52h is mixed in the hydrochloric acid that score is 12%；
Above-mentioned mixed glue solution is uniformly mixed in suspension 1:3 in mass ratio investment reaction kettle with spare reacting and obtains prefabricated mix
Liquid is closed, the N-methylmorpholine aqueous solution that the mass fraction of prefabricated mixed liquor quality 12% is 17% is added into reaction kettle, is increased anti-
Answer temperature in the kettle to 74 DEG C, constant temperature stands 90min, and reaction lotion is made；
The preparation of high temperature resistance and high strength isolation film:
Above-mentioned reaction lotion is put into vacuum oven, is concentrated and dried under conditions of temperature is 74 DEG C, vacuum degree is 120Pa
Enriched product is made in 45min, and it is 140 DEG C that enriched product, which is put into double screw extruder in temperature, and revolving speed is 100r/min
Under the conditions of extruding pelletization be made squeeze out product, by squeeze out product be placed in hot press, temperature be 220 DEG C, compacting pressure be
50min is suppressed under conditions of 22MPa, and high temperature resistance and high strength isolation film is made after natural cooling.
Comparative example 1: it is essentially identical with the preparation method of example 2, it has only the difference is that lacking reaction suspension.
Comparative example 2: it is essentially identical with the preparation method of example 2, it has only the difference is that lacking reaction lotion.
Comparative example 3: the high temperature resistance and high strength isolation film of Shanxi company production.
The test of isolation film ionic conductivity: isolation film and two panels stainless steel substrates are formed into button cell, electrolyte is injected, connects
Enter electrochemical workstation, test the AC impedance of the button cell, frequency range is 1Hz~50000Hz, frequency sweep 5Hz, simulation
Circuit is R (CR), and the ionic conductivity of isolation film is calculated by fitting AC impedance.
Tensile strength test is detected using battery isolating film instron.
1 isolation film performance measurement result of table
| Test item | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Fusing-off temperature (DEG C) | 255 | 258 | 260 | 190 | 180 | 200 |
| Ionic conductivity × 10-5(S/cm2) | 1.40 | 1.41 | 1.42 | 1.11 | 0.95 | 1.15 |
| Tensile strength (MPa) (200 DEG C × 3h) | 28.7 | 29.0 | 29.2 | 15.6 | 17.8 | 19.4 |
Good according to above-mentioned detection data high temperature resistance and high strength isolation film heat-resisting quantity produced by the present invention, fusing-off temperature is high,
Conductivity is high, good conductivity, and tensile strength is high, and mechanical property is good, has broad application prospects.
The foregoing is merely preferred modes of the invention, are not intended to limit the invention, all in spirit and original of the invention
Within then, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of preparation method of high temperature resistance and high strength isolation film, it is characterised in that specific preparation step are as follows:
Reaction lotion is put into vacuum oven, it is dense under conditions of temperature is 70~74 DEG C, vacuum degree is 110~120Pa
Enriched product is made in the dry 35~45min that contracts, and extruding pelletization in enriched product investment double screw extruder is made and squeezes out product,
By squeeze out product be placed in hot press, temperature be 200~220 DEG C, compacting pressure be 20~22MPa under conditions of compacting 40~
High temperature resistance and high strength isolation film is made after natural cooling by 50min；
The specific preparation step of the reaction lotion are as follows:
(1) it weighs in butyl titanate, glacial acetic acid and dehydrated alcohol investment beaker, with blender with 1200~1300r/min's
Revolving speed stirs, and the hydrochloric acid that dimethylformamide and mass fraction are 10~12% is added in whipping process into beaker, is mixed
Mixed glue solution is made after 50~52h；
(2) by mixed glue solution with react suspension investment reaction kettle in be uniformly mixed obtain prefabricated mixed liquor, into reaction kettle
The N-methylmorpholine aqueous solution that mass fraction is 15~17% is added, increases reactor temperature to 70~74 DEG C, constant temperature stands 80
Reaction lotion is made in~90min；
The specific preparation step of the reaction suspension are as follows:
(1) it weighs and is crushed in the reed Leaves investment pulverizer of 600~800g, the reed Leaves crushed are put into beaker, matter is used
The sodium hydroxide solution that amount score is 6~8% impregnates the reed Leaves crushed, and placing the beaker bath temperature is 60~64 DEG C
In water-bath, constant temperature impregnates 4~5h, and mixing suspension is made；
(2) graphite powder is put into beaker, and 60~80min is mixed with the revolving speed of 900~950r/min with blender and is made
Mixed serum is put into three-necked flask to be uniformly mixed to be made and be mixed by mixed serum with the sulfuric acid solution that mass fraction is 80~84%
Close liquid；
(3) three-necked flask is placed in ice-water bath, it is molten that the hydrogen peroxide that mass fraction is 18~20% is added dropwise into three-necked flask
Three-necked flask is placed in sonic oscillation instrument by liquid, and reaction solution is made in 2~3h of oscillation under conditions of frequency is 35~37kHz, to
The alumina powder of reaction solution quality 10~12% is added in three-necked flask, reaction suspension is made after standing 3~4h.
2. a kind of preparation method of high temperature resistance and high strength isolation film according to claim 1, it is characterised in that: described is double
Temperature in screw extruder is 130~140 DEG C, and revolving speed is 80~100r/min.
3. a kind of preparation method of high temperature resistance and high strength isolation film according to claim 1, it is characterised in that: reaction lotion
Specific preparation step (1) in it is preferred according to parts by weight, the butyl titanate is 8~10 parts, glacial acetic acid be 2.4~
2.6 parts, the hydrochloric acid that dehydrated alcohol is 14~16 parts, dimethylformamide is 0.4~0.6 part, mass fraction is 10~12% be
3.0~3.4 parts.
4. a kind of preparation method of high temperature resistance and high strength isolation film according to claim 1, it is characterised in that: reaction lotion
Specific preparation step (2) described in mixed glue solution with the mass ratio for reacting suspension be 1:3.
5. a kind of preparation method of high temperature resistance and high strength isolation film according to claim 1, it is characterised in that: reaction lotion
Specific preparation step (2) described in the mass fraction that is added into reaction kettle be 15~17% N-methylmorpholine aqueous solution
Quality be prefabricated mixed liquor quality 10~12%.
6. a kind of preparation method of high temperature resistance and high strength isolation film according to claim 1, it is characterised in that: reaction is suspended
The quality of the graphite powder put into described in the specific preparation step (2) of liquid into beaker be mixing suspension quality 10~
12%。
7. a kind of preparation method of high temperature resistance and high strength isolation film according to claim 1, it is characterised in that: reaction is suspended
The mass ratio for the sulfuric acid solution that mixed serum described in the specific preparation step (2) of liquid and mass fraction are 80~84% is 3:
5。
8. a kind of preparation method of high temperature resistance and high strength isolation film according to claim 1, it is characterised in that: reaction is suspended
The hydrogenperoxide steam generator that the mass fraction being added dropwise described in the specific preparation step (3) of liquid into three-necked flask is 18~20%
Quality be the 20~22% of mixed liquor quality, the quality of the alumina powder being added into three-necked flask is reaction solution quality
10~12%.
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Citations (3)
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| CN1623895A (en) * | 2004-11-16 | 2005-06-08 | 清华大学 | Method for mfg. low sulfur expansive graphite by oxydol sulfate |
| CN104787750A (en) * | 2014-01-16 | 2015-07-22 | 中国科学院宁波材料技术与工程研究所 | Graphene and preparation method thereof |
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| CN1623895A (en) * | 2004-11-16 | 2005-06-08 | 清华大学 | Method for mfg. low sulfur expansive graphite by oxydol sulfate |
| CN104787750A (en) * | 2014-01-16 | 2015-07-22 | 中国科学院宁波材料技术与工程研究所 | Graphene and preparation method thereof |
| CN107437630A (en) * | 2016-05-26 | 2017-12-05 | 上海恩捷新材料科技股份有限公司 | A kind of lithium battery isolation membrane and its production and use |
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