CN106893142A - Surface coating has expansible graphite and its manufacture method, the polymer of titania aerogel - Google Patents
Surface coating has expansible graphite and its manufacture method, the polymer of titania aerogel Download PDFInfo
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- CN106893142A CN106893142A CN201710141441.7A CN201710141441A CN106893142A CN 106893142 A CN106893142 A CN 106893142A CN 201710141441 A CN201710141441 A CN 201710141441A CN 106893142 A CN106893142 A CN 106893142A
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- mixed liquor
- expansible graphite
- surface coating
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
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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
- C08L2201/02—Flame or fire retardant/resistant
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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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- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- General Chemical & Material Sciences (AREA)
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- Paints Or Removers (AREA)
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Abstract
The invention provides expansible graphite and its manufacture method that a kind of Surface coating has titania aerogel, by in expansible graphite Surface coating layer of titanium dioxide aeroge, on the one hand the heat conduction efficiency of particle is reduced, the amount that the heat generated during material combustion returns to matrix is on the other hand reduced;The expansible graphite prepared by the method, expansion multiplying power is high, and thermal conductivity factor is low so that expansible graphite has heat endurance and anti-flammability higher, can effectively expand the use scope of expansible graphite as a kind of nontoxic high molecular weight flame retardant.
Description
Technical field
The present invention relates to expansible graphite technical field, there is titanium dioxide airsetting in particular to a kind of Surface coating
The expansible graphite and its manufacture method of glue, polymer.
Background technology
At present, expansible graphite has certain fire resistance, but its flame retarding efficiency is relatively low in application process, in related skill
In art, the method for improving its flame retarding efficiency is to carry out microcapsule coated on its surface, although improve to a certain extent can be swollen
The expansion multiplying power of swollen graphite, but the shell thermal conductivity factor of microcapsule coated is high, the expansible graphite addition of traditional microcapsules cladding
The thermal conductivity factor of material can be improved in matrix, the amount for causing the combustion heat generated in combustion process to return to matrix increases.
The content of the invention
It is contemplated that at least solving one of technical problem present in prior art or correlation technique.
Therefore, first purpose of the present invention is to propose that a kind of Surface coating has the expansible graphite of titania aerogel
Manufacture method.
Second object of the present invention is to propose that a kind of Surface coating has the expansible graphite of titania aerogel.
Third object of the present invention is to propose a kind of polymer.
In view of this, first purpose of the invention, has titanium dioxide gas the invention provides a kind of Surface coating
The manufacture method of the expansible graphite of gel, including:The expansible graphite of scheduled volume is added in the water of scheduled volume, is mixed
Close liquid;Mixed liquor is disperseed after the first scheduled duration to pour into heatable container and continue stirring;Heating mixed liquor is to first pre-
Constant temperature degree;To the TiO 2 precursor of addition scheduled volume in mixed liquor, and continue to stir the second scheduled duration;To in mixed liquor
The acetic acid of predetermined concentration is added, mixed liquor is adjusted to acidity, and continue to stir the 3rd scheduled duration;Mixed liquor is cooled to room
Temperature, to the sodium carbonate liquor that predetermined concentration is added in mixed liquor, mixed liquor is adjusted to alkalescence;Heating mixed liquor is to second predetermined
Temperature, and continue to be cooled to room temperature after stirring the 4th scheduled duration;Mixed liquor is put into freeze drying box, by freeze drying box
Cryogenic temperature be set to the 3rd predetermined temperature, persistently freeze the 5th scheduled duration;By the cryogenic temperature of freeze drying box with
One predetermined speed is promoted to the 4th predetermined temperature, persistently freezes the 6th scheduled duration;By the cryogenic temperature of freeze drying box with
Two predetermined speeds are promoted to the 5th predetermined temperature, persistently freeze the 7th scheduled duration.
Surface coating provided herein has the manufacture method of the expansible graphite of titania aerogel, by can
Expanded graphite Surface coating layer of titanium dioxide aeroge, on the one hand reduces the heat conduction efficiency of particle, on the other hand reduces material
The heat generated in fuel combustion process returns to the amount of matrix;The expansible graphite prepared by the method, expansion multiplying power is high, heat conduction system
Number it is low so that expansible graphite have heat endurance and anti-flammability higher, can as a kind of nontoxic high molecular weight flame retardant,
Effectively expand the use scope of expansible graphite.
In addition, the Surface coating in the above-mentioned technical proposal of present invention offer has the expansible graphite of titania aerogel
Manufacture method can also have following additional technical feature:
In the above-mentioned technical solutions, it is preferable that water is 100 parts;Expansible graphite is 5 to 40 parts;TiO 2 precursor
It is 10 to 60 parts.
In the technical scheme, add by by the TiO 2 precursor of 5 to 40 parts of expansible graphite and 10 to 60 parts
Enter into 100 parts of water, it is ensured that three kinds of material proportions are uniform, it is to avoid a certain material is excessive, effectively less material wave
Take, improve the utilization rate of material, reduce manufacturing cost.
In any of the above-described technical scheme, it is preferable that expansible graphite is graininess, the particle diameter of expansible graphite be more than or
Equal to 50 μm, and less than or equal to 200 μm.
In the technical scheme, by using the graininess expansible graphite that particle diameter is 50 μm to 200 μm so that inflatable
Graphite can be coated sufficiently by titania aerogel, be effectively improved its anti-flammability.
In any of the above-described technical scheme, it is preferable that the first scheduled duration be more than or equal to 30min, and less than or wait
In 120min;Second scheduled duration is more than or equal to 30min, and less than or equal to 120min;3rd scheduled duration be more than or
Equal to 60min, and less than or equal to 180min;4th scheduled duration is more than or equal to 60min, and is less than or equal to
180min;5th scheduled duration is more than or equal to 180min, and less than or equal to 300min;6th scheduled duration is more than or waits
In 180min, and less than or equal to 300min;7th scheduled duration is more than or equal to 60min, and is less than or equal to
90min;First predetermined temperature is more than or equal to 50 DEG C, and less than or equal to 80 DEG C;Second predetermined temperature is more than or equal to 40
DEG C, and less than or equal to 70 DEG C;3rd predetermined temperature is -150 DEG C;4th predetermined temperature is -100 DEG C;5th predetermined temperature
It is -50 DEG C;First predetermined speed is 10 DEG C/min;Second predetermined speed is 10 DEG C/min.
In any of the above-described technical scheme, it is preferable that the 7th scheduled duration is 60min;Second predetermined temperature is more than or waits
In 60 DEG C, and less than or equal to 70 DEG C.
In any of the above-described technical scheme, it is preferable that TiO 2 precursor is at least following one or more combination:Four
Titanium chloride, butyl titanate and titanium sulfate.
In any of the above-described technical scheme, it is preferable that to the acetic acid that predetermined concentration is added in mixed liquor, mixed liquor is adjusted
It is specially to acidity:To the acetic acid that concentration is 10% is added in mixed liquor, ph value of mixture is adjusted to 4 to 6;To in mixed liquor
The sodium carbonate liquor of predetermined concentration is added, mixed liquor is adjusted to alkalescence and is specially to the carbon that addition concentration in mixed liquor is 10%
Acid sodium solution, ph value of mixture is adjusted to 8 to 11.
In any of the above-described technical scheme, it is preferable that pour into heatable container after mixed liquor is disperseed into the first scheduled duration
In and continue stirring be specially by mixed liquor by being poured into after the scheduled duration of Ultrasound Instrument ultrasonic disperse first in there-necked flask and persistently
Stirring.
In the technical scheme, by Ultrasound Instrument dispersion mixing solution, the dispersion effect to mixed solution is effectively improved
Really, it is ensured that subsequently have the preparation of the expansible graphite of titania aerogel to Surface coating.
Second purpose of the invention, the invention provides a kind of Surface coating have a titania aerogel can be swollen
Swollen graphite, the manufacturer for having the expansible graphite of titania aerogel by the Surface coating described in any of the above-described technical scheme
Method is fabricated by, therefore, the expansible graphite that the Surface coating has titania aerogel has any of the above-described technical scheme institute
The Surface coating stated has whole beneficial effects of the manufacture method of the expansible graphite of titania aerogel.
3rd purpose of the invention, the invention provides a kind of polymer, includes such as above-mentioned technical scheme institute
The Surface coating stated has the expansible graphite of titania aerogel;Therefore, the polymer has described in above-mentioned technical proposal
Surface coating has whole beneficial effects of the expansible graphite of titania aerogel;Polymer is polyolefin, polyester, asphalt mixtures modified by epoxy resin
Fat, rubber or fiber.
Additional aspect of the invention and advantage will be set forth in part in the description, and will partly become from the following description
Obtain substantially, or recognized by practice of the invention.
Brief description of the drawings
Of the invention above-mentioned and/or additional aspect and advantage will become from description of the accompanying drawings below to embodiment is combined
Substantially and be readily appreciated that, wherein:
Fig. 1 shows that Surface coating according to an embodiment of the invention has the expansible graphite of titania aerogel
Manufacture method flow chart.
Specific embodiment
It is below in conjunction with the accompanying drawings and specific real in order to be more clearly understood that the above objects, features and advantages of the present invention
Mode is applied to be further described in detail the present invention.It should be noted that in the case where not conflicting, the implementation of the application
Feature in example and embodiment can be mutually combined.
Many details are elaborated in the following description in order to fully understand the present invention, but, the present invention may be used also
Implemented with being different from other modes described here using other, therefore, protection scope of the present invention is not by described below
Specific embodiment limitation.
Referring to Fig. 1 describe that described according to some embodiments of the invention Surface coating has a titania aerogel can be swollen
Swollen graphite manufacture method, Surface coating have the expansible graphite and polymer of titania aerogel.
In first aspect present invention embodiment, as shown in figure 1, having titanium dioxide the invention provides a kind of Surface coating
The manufacture method of the expansible graphite of aeroge, including:Step 102, scheduled volume is added to by the expansible graphite of scheduled volume
In water, mixed liquor is obtained;Step 104, mixed liquor is disperseed after the first scheduled duration to pour into heatable container and continue stirring;
Step 106, heating mixed liquor to the first predetermined temperature;Step 108, to the titanium dioxide forerunner that scheduled volume is added in mixed liquor
Body, and continue to stir the second scheduled duration;Step 110, in mixed liquor add predetermined concentration acetic acid, by mixed liquor adjust to
Acidity, and continue to stir the 3rd scheduled duration;Step 112, room temperature is cooled to by mixed liquor, to adding predetermined concentration in mixed liquor
Sodium carbonate liquor, mixed liquor is adjusted to alkalescence;Step 114, heating mixed liquor continues stirring the to the second predetermined temperature
Room temperature is cooled to after four scheduled durations;Step 116, mixed liquor is put into freeze drying box, by the freezing temperature of freeze drying box
Degree is set to the 3rd predetermined temperature, persistently freezes the 5th scheduled duration;Step 118, by the cryogenic temperature of freeze drying box with
One predetermined speed is promoted to the 4th predetermined temperature, persistently freezes the 6th scheduled duration;Step 120, by the freezing of freeze drying box
Temperature is promoted to the 5th predetermined temperature with the second predetermined speed, persistently freezes the 7th scheduled duration.
In this embodiment, by expansible graphite Surface coating layer of titanium dioxide aeroge, on the one hand reducing grain
The heat conduction efficiency of son, on the other hand reduces the amount that the heat generated during material combustion returns to matrix;Prepared by the method
Expansible graphite, expansion multiplying power is high, and thermal conductivity factor is low so that expansible graphite has heat endurance and anti-flammability higher,
The use scope of expansible graphite can be effectively expanded as a kind of nontoxic high molecular weight flame retardant.As shown in table 1, will
The expansible graphite that Surface coating has titania aerogel is added to polyurethane, compared with original polyurethane or general with adding
Logical expansible graphite is compared, and its limited oxygen index is remarkably improved, that is to say, that its anti-flammability is significantly improved.
Table 1
In one embodiment of the invention, it is preferable that water is 100 parts;Expansible graphite is 5 to 40 parts;Titanium dioxide
Presoma is 10 to 60 parts.
In this embodiment, added by by the TiO 2 precursor of 5 to 40 parts of expansible graphite and 10 to 60 parts
Into 100 parts of water, it is ensured that three kinds of material proportions are uniform, it is to avoid a certain material is excessive, effectively less waste of material,
The utilization rate of material is improve, manufacturing cost is reduced.
In one embodiment of the invention, it is preferable that expansible graphite is graininess, the particle diameter of expansible graphite is more than
Or equal to 50 μm, and less than or equal to 200 μm.
In this embodiment, by using the graininess expansible graphite that particle diameter is 50 μm to 200 μm so that inflatable stone
Ink can be coated sufficiently by titania aerogel, be effectively improved its anti-flammability.
In one embodiment of the invention, it is preferable that the first scheduled duration be more than or equal to 30min, and less than or
Equal to 120min;Second scheduled duration is more than or equal to 30min, and less than or equal to 120min;3rd scheduled duration is more than
Or equal to 60min, and less than or equal to 180min;4th scheduled duration is more than or equal to 60min, and is less than or equal to
180min;5th scheduled duration is more than or equal to 180min, and less than or equal to 300min;6th scheduled duration is more than or waits
In 180min, and less than or equal to 300min;7th scheduled duration is more than or equal to 60min, and is less than or equal to
90min;First predetermined temperature is more than or equal to 50 DEG C, and less than or equal to 80 DEG C;Second predetermined temperature is more than or equal to 40
DEG C, and less than or equal to 70 DEG C;3rd predetermined temperature is -150 DEG C;4th predetermined temperature is -100 DEG C;5th predetermined temperature
It is -50 DEG C;First predetermined speed is 10 DEG C/min;Second predetermined speed is 10 DEG C/min.
In one embodiment of the invention, it is preferable that the 7th scheduled duration is 60min;Second predetermined temperature be more than or
Equal to 60 DEG C, and less than or equal to 70 DEG C.
In one embodiment of the invention, it is preferable that TiO 2 precursor is at least following one or more combination:
Titanium tetrachloride, butyl titanate and titanium sulfate.
In one embodiment of the invention, it is preferable that to the acetic acid that predetermined concentration is added in mixed liquor, mixed liquor is adjusted
Section to acidity is specially:To the acetic acid that concentration is 10% is added in mixed liquor, ph value of mixture is adjusted to 4 to 6;To mixed liquor
The sodium carbonate liquor of middle addition predetermined concentration, it is 10% that mixed liquor is adjusted to alkaline being specially to concentration is added in mixed liquor
Sodium carbonate liquor, ph value of mixture is adjusted to 8 to 11.
In one embodiment of the invention, it is preferable that disperseing to be poured into after the first scheduled duration by mixed liquor can heat appearance
In device and continue stirring be specially by mixed liquor by pouring into there-necked flask and holding after the scheduled duration of Ultrasound Instrument ultrasonic disperse first
Continuous stirring.
In this embodiment, by Ultrasound Instrument dispersion mixing solution, the dispersion effect to mixed solution is effectively improved,
Ensure that the preparation of the follow-up expansible graphite for having titania aerogel to Surface coating.
In second aspect present invention embodiment, the invention provides a kind of Surface coating have a titania aerogel can
Expanded graphite, the manufacturer for having the expansible graphite of titania aerogel by the Surface coating described in any of the above-described embodiment
Method is fabricated by, therefore, the expansible graphite that the Surface coating has titania aerogel has described in any of the above-described embodiment
Surface coating have titania aerogel expansible graphite manufacture method whole beneficial effects.
In third aspect present invention embodiment, the invention provides a kind of polymer, include such as above-mentioned embodiment institute
The Surface coating stated has the expansible graphite of titania aerogel;Therefore, the polymer has the table described in above-described embodiment
Bread is covered with whole beneficial effects of the expansible graphite of titania aerogel;Polymer is polyolefin, polyester, asphalt mixtures modified by epoxy resin
Fat, rubber or fiber.
The preferred embodiments of the present invention are the foregoing is only, is not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.It is all within the spirit and principles in the present invention, made any repair
Change, equivalent, improvement etc., should be included within the scope of the present invention.
Claims (10)
1. a kind of Surface coating has the manufacture method of the expansible graphite of titania aerogel, it is characterised in that including:
The expansible graphite of scheduled volume is added in the water of scheduled volume, mixed liquor is obtained;
Mixed liquor is disperseed after the first scheduled duration to pour into heatable container and continue stirring;
Heat mixed liquor to the first predetermined temperature;
To the TiO 2 precursor of addition scheduled volume in mixed liquor, and continue to stir the second scheduled duration;
To the acetic acid that predetermined concentration is added in mixed liquor, mixed liquor is adjusted to acidity, and continue to stir the 3rd scheduled duration;
Mixed liquor is cooled to room temperature, to the sodium carbonate liquor that predetermined concentration is added in mixed liquor, mixed liquor is adjusted to alkalescence;
Heating mixed liquor continues to be cooled to room temperature after stirring the 4th scheduled duration to the second predetermined temperature;
Mixed liquor is put into freeze drying box, the cryogenic temperature of the freeze drying box is set to the 3rd predetermined temperature, held
The 5th scheduled duration of continuous freezing;
The cryogenic temperature of the freeze drying box is promoted to the 4th predetermined temperature with the first predetermined speed, the 6th is persistently freezed pre-
Timing is long;
The cryogenic temperature of the freeze drying box is promoted to the 5th predetermined temperature with the second predetermined speed, the 7th is persistently freezed pre-
Timing is long.
2. Surface coating according to claim 1 has the manufacture method of the expansible graphite of titania aerogel, and it is special
Levy and be,
The water is 100 parts;
The expansible graphite is 5 to 40 parts;
The TiO 2 precursor is 10 to 60 parts.
3. Surface coating according to claim 1 has the manufacture method of the expansible graphite of titania aerogel, and it is special
Levy and be, the expansible graphite is graininess, the particle diameter of the expansible graphite is more than or equal to 50 μm, and less than or wait
In 200 μm.
4. Surface coating according to claim 1 has the manufacture method of the expansible graphite of titania aerogel, and it is special
Levy and be,
First scheduled duration is more than or equal to 30min, and less than or equal to 120min;
Second scheduled duration is more than or equal to 30min, and less than or equal to 120min;
3rd scheduled duration is more than or equal to 60min, and less than or equal to 180min;
4th scheduled duration is more than or equal to 60min, and less than or equal to 180min;
5th scheduled duration is more than or equal to 180min, and less than or equal to 300min;
6th scheduled duration is more than or equal to 180min, and less than or equal to 300min;
7th scheduled duration is more than or equal to 60min, and less than or equal to 90min;
First predetermined temperature is more than or equal to 50 DEG C, and less than or equal to 80 DEG C;
Second predetermined temperature is more than or equal to 40 DEG C, and less than or equal to 70 DEG C;
3rd predetermined temperature is -150 DEG C;
4th predetermined temperature is -100 DEG C;
5th predetermined temperature is -50 DEG C;
First predetermined speed is 10 DEG C/min;
Second predetermined speed is 10 DEG C/min.
5. Surface coating according to claim 4 has the manufacture method of the expansible graphite of titania aerogel, and it is special
Levy and be,
7th scheduled duration is 60min;
Second predetermined temperature is more than or equal to 60 DEG C, and less than or equal to 70 DEG C.
6. Surface coating according to claim 1 has the manufacture method of the expansible graphite of titania aerogel, and it is special
Levy and be, the TiO 2 precursor is at least following one or more combination:Titanium tetrachloride, butyl titanate and sulfuric acid
Titanium.
7. Surface coating according to any one of claim 1 to 6 has the system of the expansible graphite of titania aerogel
Make method, it is characterised in that
The acetic acid to addition predetermined concentration in mixed liquor, mixed liquor is adjusted to acidity and is specially:Added in mixed liquor
Concentration is 10% acetic acid, and ph value of mixture is adjusted to 4 to 6;
The sodium carbonate liquor to addition predetermined concentration in the mixed liquor, mixed liquor is adjusted to alkalescence and is specially to described
The sodium carbonate liquor that concentration is 10% is added in mixed liquor, ph value of mixture is adjusted to 8 to 11.
8. Surface coating according to any one of claim 1 to 6 has the system of the expansible graphite of titania aerogel
Make method, it is characterised in that described to disperse to be poured into heatable container after the first scheduled duration and lasting Stirring device by mixed liquor
Body be by mixed liquor by being poured into there-necked flask after the scheduled duration of Ultrasound Instrument ultrasonic disperse first and continue stirring.
9. a kind of Surface coating has the expansible graphite of titania aerogel, it is characterised in that by such as claim 1 to 8
Any one of the Surface coating manufacture method that has the expansible graphite of titania aerogel be fabricated by.
10. a kind of polymer, it is characterised in that including Surface coating as claimed in claim 9 has titania aerogel
Expansible graphite;
The polymer is polyolefin, polyester, epoxy resin, rubber or fiber.
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CN201710141441.7A CN106893142A (en) | 2017-03-10 | 2017-03-10 | Surface coating has expansible graphite and its manufacture method, the polymer of titania aerogel |
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CN201710141441.7A CN106893142A (en) | 2017-03-10 | 2017-03-10 | Surface coating has expansible graphite and its manufacture method, the polymer of titania aerogel |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108390002A (en) * | 2018-03-05 | 2018-08-10 | 奚正华 | A kind of preparation method of the lithium battery diaphragm reinforcing material based on pyrophyllite-titania aerogel |
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CN108390002A (en) * | 2018-03-05 | 2018-08-10 | 奚正华 | A kind of preparation method of the lithium battery diaphragm reinforcing material based on pyrophyllite-titania aerogel |
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