CN109809468A - A kind of preparation method and applications of nano barium phthalate - Google Patents
A kind of preparation method and applications of nano barium phthalate Download PDFInfo
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- CN109809468A CN109809468A CN201811625815.3A CN201811625815A CN109809468A CN 109809468 A CN109809468 A CN 109809468A CN 201811625815 A CN201811625815 A CN 201811625815A CN 109809468 A CN109809468 A CN 109809468A
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- nano barium
- barium phthalate
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention provides a kind of preparation method and applications of nano barium phthalate, the preparation method of nano barium phthalate includes the following steps: to mix titanium-containing compound, peroxide aqueous solution, aqueous solutions of polymers, forms dispersion liquid；It is slowly added to water soluble metallic compound into dispersion liquid, stirs evenly；Alcohol is added, precipitating is generated, is filtered by centrifuge precipitating or pumping and filtering device and isolates sediment, is i.e. Nano titanate presoma；Barium chloride solution is added into Nano titanate presoma, it with solvent acetylacetone,2,4-pentanedione, is carried out after being sufficiently stirred 0.5-1 hours, is transferred in the interior stainless steel cauldron equipped with polytetrafluoroethylliner liner by ultrasonic oscillation, closing is tightened, reaction kettle is put into constant temperature oven and carries out lyate ion exchange；Using filtering, washing, drying obtains nano barium phthalate.The application does not prepare nano barium phthalate by high pressure, high temperature, highly basic, simple process can be used for large-scale industrial production by raw material simple and easy to get.
Description
Technical field
The present invention relates to material chemistry technical field more particularly to a kind of preparation method and applications of nano barium phthalate.
Background technique
Titanate has been widely used in the fields such as battery electrode, piezoelectricity, is the hot spot of Material Field research.Metatitanic acid
The application performance of salt material and its particle size are closely related.For example, nanostructure can reduce the grain diameter of material, when
When applied to battery electrode, it is possible to reduce ion insertion with it is embedding out at a distance from and path, promote the fast charging and discharging of battery
Energy；Nanostructure can also increase the contact surface of the specific surface area of material, adsorbable more conductive agents and increase and electrolyte
Product reduces current density, further promotes the fast charging and discharging performance of material.Therefore, preparation synthesis has the titanium of nanoscale
Hydrochlorate particle will greatly improve the application effect of titanate material.
The method of existing production titanate mainly includes solid-state synthesis and hydro-thermal reaction preparation.
Wherein, solid-state synthetic method generallys use titanium dioxide and carbonate or hydroxide after ball milling mixes, big
It makes annealing treatment and obtains at a high temperature of 800 degrees Celsius.The titanate size that this method is prepared is usually in micro-meter scale, shape
Looks and homogeneity is all bad and purity is not high, so that the best applications effect of titanate material can not be obtained.
The hydrothermal preparing process of nanostructure titanate is usually starting former material with commercial titanium dioxide and sodium hydroxide
Material, prepares sodium titanate by hydro-thermal method, and sodium titanate is immersed in acid solution, has obtained metatitanic acid using ion-exchange；
Titanate predecessor is obtained after then metatitanic acid is mixed with metal salt solution, product makes annealing treatment at different temperatures later, obtains
To titanate products.The preparation method is related to adding sodium hydroxide in the solution, and sodium hydroxide discharges when solution contacts
Very big heat, and preparation process also uses the environment of high temperature and pressure, so that sodium hydroxide is to the hot ability to bear of equipment, anti-
Corrosive requirement is very high, and the wastewater treatment after preparation will also spend certain cost, it is therefore desirable to develop a kind of simple process peace
Entirely, Nano titanate is prepared without high temperature, high pressure, highly basic to be more widely used in battery electrode, piezoelectricity field.
Summary of the invention
To overcome the problems, such as safe preparation process existing in the prior art, the present invention provides a kind of nano barium titanates
The preparation method and applications of barium.
A kind of preparation method of nano barium phthalate, which comprises the steps of:
(1) titanium-containing compound is distributed in pure water at normal temperature；
(2) product of step (1) is mixed with peroxide aqueous solution, aqueous solutions of polymers, forms dispersion liquid；
(3) it is slowly added to water soluble metallic compound into the product of step (2), stirred evenly；
(4) alcohol is added into the product of step (3), generates precipitating, was carried out by centrifuge precipitating or pumping and filtering device
Sediment, i.e. Nano titanate presoma are isolated in filter；
(5) barium chloride solution of 0.5mol/L will be added in the product of step (4), add acetylacetone,2,4-pentanedione solvent, pass through
Ultrasonic oscillation be sufficiently stirred 0.5-1 hours；
(6) mixed liquor of step (5) is transferred in the interior stainless steel cauldron equipped with polytetrafluoroethylliner liner, is tightened
Closing is formed between sealing reaction, and it is anti-with 240-250 DEG C of temperature progress lyate ion exchange that reaction kettle is put into constant temperature oven
2-6 hours between seasonable；
(7) product of step (6) is precipitated using centrifuge or pumping and filtering device is filtered and isolates sediment；
(8) product of step (7) is washed with deionized, is then transferred to microwave drying device, dried, obtained with 60-80 DEG C
To nano barium phthalate.
In a preferred embodiment, titanium-containing compound preferred alcohol titanium, isopropyl titanate, propyl alcohol in step (1)
Titanium, butyl titanate, titanium ethylene glycolate, glycerine titanium, titanium sulfate, titanyl sulfate, titanium tetrachloride and titanium tetrafluoride one kind or
Several combinations.
In a preferred embodiment, titanium dioxide powder alternative steps (1) can also directly be taken in step (2)
Product.
In a preferred embodiment, step (2) peroxide is selected from hydrogen peroxide, carbamide peroxide and peroxide
The combination of one or more of acetic acid.
In a preferred embodiment, peroxide in the titanium source and peroxide aqueous solution in step (2)
Molar ratio is 1:5-1:10.
In a preferred embodiment, the preferred chitosan of polymer in the step (2), guar gum, methyl are fine
Tie up element, ethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, polyvinyl alcohol, polyacrylamide
The content of one in amine and polyethylene glycol oxide or several combinations, polymer is a ten thousandth to 10, preferably in solution
The content of polymer is added as one thousandth to 1 percent.
In a preferred embodiment, the preferred sodium peroxide of water soluble metallic compound, sodium chloride in step (3),
Wherein the concentration of metal ion is 0.5-7mol/L.
In a preferred embodiment, the preferred methanol of alcohol, ethyl alcohol, propyl alcohol, butanol, amylalcohol, second two in step (4)
One of alcohol, propylene glycol, glycerine and polyethylene glycol or several combinations, the volume ratio that alcohol additive amount accounts for solution are
5%-50%, preferred volume ratio 10%-25%.
A kind of application of nano barium phthalate, which comprises the steps of:
S1, it will disperse in deionized water after graphite oxidation, add the nano barium phthalate prepared, be sufficiently mixed；
S2, product will be obtained in S1 and be put into 60-70 DEG C of constant temperature oven or microwave drying device and dry, until not aqueous
Point；
S3, S2 acquisition product is placed in 250 DEG C of calcining furnaces and is sintered 2 hours, receiving for graphene coated can be obtained
Rice barium titanate.
In a preferred embodiment, when nano barium phthalate being added in step S1, also to increase dispersing agent polypropylene
Sour sodium, Sodium Polyacrylate are conducive to the dissolution of nano barium phthalate.
Compared with prior art, the beneficial effects of the present invention are:
(1) the application does not prepare nano barium phthalate by high pressure, high temperature, highly basic by raw material simple and easy to get,
Simple process can be used for large-scale industrial production；
(2) the application uses liquid-phase chemical reaction by whole, and the additives such as surfactant, technique letter is not added
Single, manufactured material structure is uniform and stable；
(3) the application dissolves sodium titanate and barium ions using the supercriticality of acetylacetone,2,4-pentanedione, reduces ion exchange
The reaction temperature and pressure that Shi Bixu is provided, energy consumption needed for reducing reaction, improve production efficiency；
(4) nano barium phthalate is added, obtains the nano barium phthalate of graphene coated at graphene by graphite oxidation, benefit
With the high conductivity of graphene, the conductivity of nano barium phthalate is improved, nano barium phthalate is allowed preferably to be used for battery
The fields such as electrode, piezoelectricity.
Specific embodiment
With reference to embodiments, the present invention will be described in further detail.It should be appreciated that described herein specific
Embodiment only to explain the present invention, is not intended to limit the present invention.
Embodiment 1:
An a kind of preferred embodiment of the preparation method and applications of nano barium phthalate, a kind of preparation of nano barium phthalate
Method includes the following steps:
(1) titanium ethylene glycolate and glycerine titanium are distributed in pure water at normal temperature；
(2) product of step (1) is mixed with carbamide peroxide aqueous solution with the molar ratio of 1:5, adds chitosan water
Solution forms dispersion liquid；
(3) sodium peroxide and sodium chloride mixed liquor of 0.5mol/L are slowly added into the product of step (2), stirring is equal
It is even；
(4) ethyl alcohol for accounting for bulk product 10% is added into the product of step (3), generates precipitating, is separated by centrifuge
Sediment out, i.e. Nano titanate presoma；
(5) barium chloride solution of 0.5mol/L will be added in the product of step (4), add acetylacetone,2,4-pentanedione solvent, pass through
Ultrasonic oscillation be sufficiently stirred 1 hour；
(6) mixed liquor of step (5) is transferred in the interior stainless steel cauldron equipped with polytetrafluoroethylliner liner, is tightened
Closing is formed between sealing reaction, when reaction kettle being put into constant temperature oven carrying out lyate ion exchange reaction with 240 DEG C of temperature
Between 3 hours；
(7) product of step (6) is precipitated using centrifuge or pumping and filtering device is filtered and isolates sediment；
(8) product of step (7) is washed with deionized, is then transferred to microwave drying device, dried, obtained with 70 DEG C
Nano barium phthalate.
An a kind of preferred embodiment of the preparation method and applications of nano barium phthalate, a kind of application of nano barium phthalate,
Include the following steps:
S1, by dispersing in deionized water after graphite oxidation, add the nano barium phthalate and polyacrylic acid prepared
Sodium is sufficiently mixed, and is increased Sodium Polyacrylate as solvent, is more advantageous to nano barium phthalate dissolution；
S2, product will be obtained in S1 and be put into 70 DEG C of constant temperature ovens and dry, until moisture-free；
S3, S2 acquisition product is placed in 250 DEG C of calcining furnaces and is sintered 2 hours, receiving for graphene coated can be obtained
Rice barium titanate.
Embodiment 2:
An a kind of preferred embodiment of the preparation method and applications of nano barium phthalate, a kind of preparation of nano barium phthalate
Method includes the following steps:
(1) brilliant red stone titania powder is mixed with hydrogen peroxide, carbamide peroxide aqueous solution, POLYPROPYLENE GLYCOL aqueous solution
It closes, forms dispersion liquid, wherein the concentration ratio of brilliant red stone titania powder and peroxide is 1:8, and POLYPROPYLENE GLYCOL accounts for solution
The 1% of volume；
(2) sodium chloride is slowly added into the product of step (1), sodium chloride concentration is 5mol/L after mixing evenly；
(3) ethyl alcohol of liquor capacity 15% and the mixed liquor of ethylene glycol are added into the product of step (3), generates precipitating,
Go out sediment, i.e. Nano titanate presoma by centrifuge precipitation and separation；
(4) barium chloride solution of 0.5mol/L will be added in the product of step (4), add acetylacetone,2,4-pentanedione solvent, pass through
Ultrasonic oscillation be sufficiently stirred 0.75 hour；
(5) mixed liquor of step (5) is transferred in the interior stainless steel cauldron equipped with polytetrafluoroethylliner liner, is tightened
Closing is formed between sealing reaction, when reaction kettle being put into constant temperature oven carrying out lyate ion exchange reaction with 250 DEG C of temperature
Between 4 hours；
(6) product of step (6) is precipitated using centrifuge or pumping and filtering device is filtered and isolates sediment；
(7) product of step (7) is washed with deionized, is then transferred to microwave drying device, dried, obtained with 70 DEG C
Nano barium phthalate.
An a kind of preferred embodiment of the preparation method and applications of nano barium phthalate, a kind of application of nano barium phthalate,
Include the following steps:
S1, it will disperse in deionized water after graphite oxidation, add the nano barium phthalate prepared, be sufficiently mixed；
S2, product will be obtained in S1 and be put into 60-70 DEG C of constant temperature oven or microwave drying device and dry, until not aqueous
Point；
S3, S2 acquisition product is placed in 250 DEG C of calcining furnaces and is sintered 2 hours, receiving for graphene coated can be obtained
Rice barium titanate.
In the present embodiment, when nano barium phthalate being added in step S1, also to increase dispersing agent Sodium Polyacrylate, poly- third
Olefin(e) acid sodium is conducive to the dissolution of nano barium phthalate.
The present embodiment does not prepare nano barium phthalate, work by high pressure, high temperature, highly basic by raw material simple and easy to get
Skill is simple, can be used for large-scale industrial production；Liquid-phase chemical reaction is used by whole process, surfactant etc. is not added
Additive, simple process, manufactured material structure are uniform and stable；Titanium is dissolved by the supercriticality using acetylacetone,2,4-pentanedione
Sour sodium and barium ions, the reaction temperature that must be provided when reducing ion exchange and pressure, energy consumption needed for reducing reaction, mention
High efficiency；The present embodiment, at graphene, is added nano barium phthalate, obtains the nanometer of graphene coated by graphite oxidation
Barium titanate improves the conductivity of nano barium phthalate using the high conductivity of graphene, allows nano barium phthalate more preferable
For the fields such as battery electrode, piezoelectricity.
The preferred embodiment of the present invention has shown and described in above description, as previously described, it should be understood that the present invention is not office
It is limited to form disclosed herein, should not be regarded as an exclusion of other examples, and can be used for various other combinations, modification
And environment, and can be carried out within that scope of the inventive concept describe herein by the above teachings or related fields of technology or knowledge
Change.And changes and modifications made by those skilled in the art do not depart from the spirit and scope of the present invention, then it all should be in institute of the present invention
In attached scope of protection of the claims.
Claims (10)
1. a kind of preparation method of nano barium phthalate, which comprises the steps of:
(1) titanium-containing compound is distributed in pure water at normal temperature；
(2) product of step (1) is mixed with peroxide aqueous solution, aqueous solutions of polymers, forms dispersion liquid；
(3) it is slowly added to water soluble metallic compound into the product of step (2), stirred evenly；
(4) it is added alcohol into the product of step (3), generates precipitating, be filtered point by centrifuge precipitating or pumping and filtering device
Separate out sediment, i.e. Nano titanate presoma；
(5) barium chloride solution of 0.5mol/L will be added in the product of step (4), add acetylacetone,2,4-pentanedione solvent, pass through ultrasound
Wave concussion be sufficiently stirred 0.5-1 hours；
(6) mixed liquor of step (5) is transferred in the interior stainless steel cauldron equipped with polytetrafluoroethylliner liner, tightens closing,
It is formed between sealing reaction, reaction kettle is put into constant temperature oven, the lyate ion exchange reaction time is carried out with 240-250 DEG C of temperature
2-6 hours；
(7) product of step (6) is precipitated using centrifuge or pumping and filtering device is filtered and isolates sediment；
(8) product of step (7) is washed with deionized, is then transferred to microwave drying device, dried, received with 60-80 DEG C
Rice barium titanate.
2. a kind of preparation method of nano barium phthalate according to claim 1, it is characterised in that: contain titanizing in step (1)
Close object preferred alcohol titanium, isopropyl titanate, titanium propanolate, butyl titanate, titanium ethylene glycolate, glycerine titanium, titanium sulfate, titanyl sulfate,
One or several kinds of combinations of titanium tetrachloride and titanium tetrafluoride.
3. a kind of preparation method of nano barium phthalate according to claim 1, it is characterised in that: can be in step (2)
Directly take the product of titanium dioxide powder alternative steps (1).
4. a kind of preparation method of nano barium phthalate according to claim 1, it is characterised in that: step (2) peroxide
Combination selected from one or more of hydrogen peroxide, carbamide peroxide and Peracetic acid.
5. a kind of preparation method of nano barium phthalate according to claim 1, it is characterised in that: the titanium source in step (2)
Molar ratio with the peroxide in peroxide aqueous solution is 1:5-1:10.
6. a kind of preparation method of nano barium phthalate according to claim 1, it is characterised in that: in the step (2)
The preferred chitosan of polymer, guar gum, methylcellulose, ethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxypropyl
One in ylmethyl cellulose, polyvinyl alcohol, polyacrylamide and polyethylene glycol oxide or several combinations, the content of polymer are
A ten thousandth adds the content of polymer to 10 as one thousandth to 1 percent preferably in solution.
7. a kind of preparation method of nano barium phthalate according to claim 1, it is characterised in that: water-soluble in step (3)
The preferred sodium peroxide of metallic compound, sodium chloride, wherein the concentration of metal ion is 0.5-7mol/L.
8. a kind of preparation method of nano barium phthalate according to claim 1, it is characterised in that: alcohol is preferred in step (4)
One of methanol, ethyl alcohol, propyl alcohol, butanol, amylalcohol, ethylene glycol, propylene glycol, glycerine and polyethylene glycol or several groups
It closes, the volume ratio that alcohol additive amount accounts for solution is 5%-50%, preferred volume ratio 10%-25%.
9. a kind of application of nano barium phthalate, which comprises the steps of:
S1, it will disperse in deionized water after graphite oxidation, add the nano barium phthalate prepared, be sufficiently mixed；
S2, product will be obtained in S1 and be put into 60-70 DEG C of constant temperature oven or microwave drying device and dry, until moisture-free；
S3, S2 acquisition product is placed in 250 DEG C of calcining furnaces and is sintered 2 hours, the nano-titanium of graphene coated can be obtained
Sour barium.
10. a kind of application of nano barium phthalate, it is characterised in that: when nano barium phthalate being added in step S1, also to increase dispersion
Agent Sodium Polyacrylate, Sodium Polyacrylate are conducive to the dissolution of nano barium phthalate.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113998732A (en) * | 2021-12-10 | 2022-02-01 | 武汉市格勒特新材料有限公司 | Preparation method of barium titanate nano powder |
| US11554966B2 (en) * | 2018-08-30 | 2023-01-17 | Petrochina Company Limited | Nanostructured titanic acid salts and preparation process and use thereof |
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Application publication date: 20190528 |