CN106268612B - A kind of porous barium strontium titanate raw powder's production technology - Google Patents
A kind of porous barium strontium titanate raw powder's production technology Download PDFInfo
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- 229910052454 barium strontium titanate Inorganic materials 0.000 title claims abstract description 43
- 239000000843 powder Substances 0.000 title claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 238000005516 engineering process Methods 0.000 title claims description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 24
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 22
- 229910052788 barium Inorganic materials 0.000 claims description 16
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 15
- 238000004140 cleaning Methods 0.000 claims description 15
- 229910052712 strontium Inorganic materials 0.000 claims description 15
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 12
- -1 polytetrafluoroethylene Polymers 0.000 claims description 12
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000000151 deposition Methods 0.000 claims description 10
- 230000008021 deposition Effects 0.000 claims description 10
- 239000000376 reactant Substances 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 229910010252 TiO3 Inorganic materials 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 229910001626 barium chloride Inorganic materials 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 239000010936 titanium Substances 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims 2
- 238000010931 ester hydrolysis Methods 0.000 claims 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 claims 1
- 229910052719 titanium Inorganic materials 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 23
- 238000002360 preparation method Methods 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 12
- 238000002156 mixing Methods 0.000 abstract description 10
- 239000000919 ceramic Substances 0.000 abstract description 6
- 239000002243 precursor Substances 0.000 abstract description 5
- 238000001354 calcination Methods 0.000 abstract description 4
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 208000002925 dental caries Diseases 0.000 abstract description 3
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 abstract description 3
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000004088 foaming agent Substances 0.000 abstract description 2
- 238000010792 warming Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 230000008569 process Effects 0.000 description 9
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 7
- 238000010907 mechanical stirring Methods 0.000 description 6
- 230000007062 hydrolysis Effects 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 3
- 239000006193 liquid solution Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 3
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 3
- 239000004926 polymethyl methacrylate Substances 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229960004424 carbon dioxide Drugs 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 239000012704 polymeric precursor Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- WOIHABYNKOEWFG-UHFFFAOYSA-N [Sr].[Ba] Chemical compound [Sr].[Ba] WOIHABYNKOEWFG-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- YWJHUQQPWSXFTC-UHFFFAOYSA-H barium(2+) oxalate titanium(4+) Chemical compound [Ti+4].[Ba++].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O YWJHUQQPWSXFTC-UHFFFAOYSA-H 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- QKKWJYSVXDGOOJ-UHFFFAOYSA-N oxalic acid;oxotitanium Chemical compound [Ti]=O.OC(=O)C(O)=O QKKWJYSVXDGOOJ-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/02—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the alkali- or alkaline earth metals or beryllium
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
- C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
- C04B35/465—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates
- C04B35/468—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates
- C04B35/4682—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates based on BaTiO3 perovskite phase
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3213—Strontium oxides or oxide-forming salts thereof
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- Chemical Kinetics & Catalysis (AREA)
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- Ceramic Engineering (AREA)
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- Manufacturing & Machinery (AREA)
- Structural Engineering (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of preparation methods of micro--nano porous structure barium-strontium titanate powder, especially under hydrothermal high-temperature admixture, realize the synthesis of micro--nano porous structure barium-strontium titanate powder, in method of the invention, two kinds of solution as precursors are respectively placed in two cavitys of tetrafluoroethene two-chamber liner, carry out mixing pyroreaction again when being warming up to 180 ~ 220 °C.Compared with prior art, organic foaming agent is not used in method reaction process of the invention, cost of material is lower, has better environment friendly；It is reacted under mild thermal and hydric environment, is not necessarily to calcination processing, low energy consumption is with good stability and repeatable；Prepared porous barium strontium titanate have it is unique it is micro--receive secondary structure, there is bigger specific surface area, stability is more preferable, has excellent dimensional homogeneity and dispersibility, is with a wide range of applications in terms of function ceramics, catalysis and absorption.
Description
Technical field
The present invention relates to a kind of porous barium strontium titanate raw powder's production technologies more particularly to a kind of hydrothermal high-temperature mixing method to close
At the method with the porous barium-strontium titanate powder of micro-nano structure, belong to inorganic non-metallic field of functional materials.
Background technique
Barium strontium titanate has perovskite structure, is a kind of inorganic non-metallic functional material that purposes is very extensive, main
Advantage includes thermal stability is good, dielectric loss is low, dielectric constant is high etc..Since in perovskite structure, positive and negative charge center is not
It is overlapped the generation of meeting induced spontaneous polarization, the presence of this built in field can effectively facilitate the compound of electron-hole pair, extend
The service life of carrier.Therefore, barium strontium titanate is as a kind of semiconductor material, and 3.2 ~ 3.8 eV of forbidden bandwidth is in recent years in photocatalysis
Field has obtained more and more concerns, photocatalysis hydrogen production, in terms of with wide application before
Scape.
In order to meet barium strontium titanate in the requirement of catalysis and adsorbing domain, need to develop with large specific surface area
Porous type barium strontium titanate material.Generally, it is carried out in barium-strontium titanate ceramic preparation process in solid phase method, by adding organic hair
Infusion, such as polymethyl methacrylate (PMMA, Polymethyl methacrylate), polyvinyl alcohol (Polyvinyl
Alcohol, PVA), polyvinyl butyral (Polyvinyl butyral, PVB), triethanolamine
(Triethanolamine, TEA) etc., thus be made porous barium-strontium titanate ceramic (Materials Chemistry and Physics, 2002, 78, 154–159；Journal of Alloys and Compounds, 2015, 636, 93–
96).Also there is researcher by adding inorganic carbon nanotube or graphite, utilize the production shape of carbon dioxide in high-temperature burning process
At Micro porosity.However, microcosmic leakiness of the formation of porous ceramics along with ceramics itself, resulting microcellular structure compare table
Area is not high.In order to increase specific surface area, it is necessary to carry out the preparation of nanoscale barium-strontium titanate powder.But, nano-powder
Itself have a disadvantage that it is to be easy reunion, this greatly reduces the specific surface area for making itself, is unfavorable for the performance of performance.
Micro-nano structure belongs to the secondary orderly aggregate of nano material, and the height that one side can retain nano material is living
Property, while being also avoided that the reunion unfavorable for performance.In terms of barium strontium titanate, developing, there is the powder of micro-nano porous structure to have
It is significant.There is researcher to pass through thermal decomposition barium titanium oxalate [barium titanyl oxalate, BaTiO (C2O4)2·
4H2O] carry out porous barium strontium titanate powder preparation, be substantially to generate two using the decomposition of organic matter in calcination process
Carbonoxide, thus formed hole configurations (Journal of the American Ceramic Society, 2009, 92,
3132–3134).In addition, during preparing porous Sr titanate powder using sol-gel method, by the way that triethanolamine is added
(Triethanolamine, TEA), the size in aperture be controlled by adjusting the additive amount of TEA (Chem. Mater.,
2000, 12 (9), 2590–2596).Brazilian scholar A. Ries etc. uses Via Polymeric Precursor Method (Polymeric
Precursor method, PPM) it is prepared for the barium strontium titanate porous powder of component ratio Ba/Sr=80/20.At later period calcining
Reason process makes particle size uniformity poor, agglomeration it is more serious (Materials Characterization, 2003,
50, 217– 221).So far, also have a small amount of Chinese patent disclose strontium titanates/barium porous structure preparation method (such as:
A kind of preparation method of strontium titanate film having spherical grain accumulated porous structure, CN 102390935A;A kind of porous balls of strontium titanate
Preparation method, CN 101092244A).However, porous strontium titanates/barium prepared by the above method belongs to microstructure not
Fine and close block materials, specific surface area is still not abundant enough, and uniformity is poor.
Summary of the invention
Technical problem
Present invention aim to address the deficiencies in the prior art, propose to prepare porous barium strontium titanate powder under a kind of hydrothermal condition
The method of body, porous barium strontium titanate powder specific-surface area detection prepared by this method is big, of uniform size, good dispersion.
Technical solution
In order to solve the above technical problems, a kind of porous barium strontium titanate raw powder's production technology of the invention, feature
It is, including the following steps:
Step 1: according to barium strontium titanate molecular formula Ba1-x Sr x TiO3The component ratio of middle barium and strontiumx, whereinx=0 ~ 1.0, claim
Take BaCl2With Sr (NO3)2, prepare and obtain the aqueous solution 20ml that Ba and Sr total ion concentration is 0.16 mol/L；It states then up
Suitable potassium hydroxide is added in solution as mineralizer, stirs 30min and waits for that it is sufficiently dissolved and to be uniformly mixed to get mixing molten
Liquid, then by resulting mixed solution be transferred to first of polytetrafluoroethylene (PTFE) two-chamber liner it is intracavitary；
Step 2: according to the ratio of (Ba+Sr)/Ti=4 in entire reaction system, weighing the butyl titanate of corrresponding quality,
Then a small amount of deionized water and dilute nitric acid solution are added thereto, it, then will be prepared to inhibit tetrabutyl titanate hydrolysis
Solution be transferred to polytetrafluoroethylene (PTFE) two-chamber liner second is intracavitary；
Step 3: it by the polytetrafluoroethyllining lining merging stainless steel high temperature reaction kettle of step 2, seals and is disposed vertically
In hydro-thermal baking oven, oven temperature is increased to 180 ~ 220 °C；
Step 4: when heating reaches 180 ~ 220 °C, so that reaction kettle is constantly in rollover states, react stainless steel high temperature
Two intracavitary reaction raw materials of kettle are sufficiently mixed, and are cooled to room temperature with the furnace after reacting 15 ~ 20 h, are obtained reactant；
Step 5: the reactant that step 4 is obtained carries out suction filtration cleaning treatment, obtains white depositions, through deionized water
For several times with washes of absolute alcohol, until cleaning solution pH value is 7；
Step 6: the white depositions after cleaning are dried for 24 hours under the conditions of 80 °C, obtain porous metatitanic acid
Strontium barium powder.
In method of the invention, two kinds of solution as precursors are respectively placed in two of tetrafluoroethene two-chamber liner
In cavity, mixing pyroreaction is carried out again when being warming up to 180 ~ 220 °C.
Beneficial effect
Compared with prior art, method of the invention has the advantages that
(1) organic foaming agent is not used in reaction process, cost of material is lower, has better environment friendly；
(2) it is reacted under mild thermal and hydric environment, is not necessarily to calcination processing, low energy consumption has good stabilization
Property and repeatability；
(3) porous barium strontium titanate prepared by have it is unique it is micro--receive secondary structure, there is bigger specific surface area, surely
It is qualitative more preferable, there is excellent dimensional homogeneity and dispersibility.
Porous barium-strontium titanate powder prepared by the present invention has preferably constructing property compared to block materials, makes pottery in function
Porcelain, catalysis and absorption aspect are with a wide range of applications.
Detailed description of the invention
Fig. 1 is the XRD spectrum of porous barium-strontium titanate powder obtained by first embodiment of the invention；
Fig. 2 is the field emission scanning electron microscope (FE- of porous barium-strontium titanate powder obtained by second embodiment of the invention
SEM) photo；
Fig. 3 is the field emission scanning electron microscope (FE- of porous barium-strontium titanate powder obtained by third embodiment of the invention
SEM) photo.
Specific embodiment
Below by embodiment the substantive features and marked improvement that the present invention is furture elucidated, but the present invention is only limitted to absolutely not
Embodiment described in the embodiment.All deformations for directly being exported or being associated by present disclosure, should all recognize
To be protection scope of the present invention.
Embodiment one:
The present embodiment is a kind of porous barium strontium titanate raw powder's production technology, comprising the following steps:
Step 1: according to the barium strontium titanate (Ba of required preparation1-x Sr x TiO3, BST) in barium and strontium the mass ratio of the material example
Ba/Sr=1 weighs the barium chloride (BaCl of 0.08mol/L2) and 0.08mol/L strontium nitrate [Sr (NO3)2], prepare Ba and Sr from
Sub- total concentration is 20 ml of aqueous solution of 0.16 mol/L.The mineralizer hydroxide that 2.0mol/L is added in solution is stated then up
Potassium (KOH), 30 min of stirring wait for that it is sufficiently dissolved and after evenly mixing, is transferred to polytetrafluoroethylene (PTFE) two-chamber for above-mentioned mixed solution
One of them of liner is intracavitary；
Step 2: being that 0.04 mol/L weighs butyl titanate according to Ti ratio in entire reaction system, then thereto
A small amount of deionized water and dilute nitric acid solution is added, thus inhibit the hydrolysis of butyl titanate, the solution for then obtaining preparation
Another for being transferred to polytetrafluoroethylene (PTFE) two-chamber liner is intracavitary；
Step 3: will be placed with Step 1: the polytetrafluoroethyllining lining for the reaction precursor liquid solution that step 2 obtains is placed in not
In steel pyroreaction kettle of becoming rusty, in order to avoid the mixing of two intracavitary reaction raw materials, polytetrafluoroethyl-ne is remained in seal process
Alkene liner is in plumbness；The pyroreaction kettle being sealed is disposed vertically in hydro-thermal baking oven, temperature control program is set, will dry
The temperature inside the box is increased to 200 °C；
Step 4: when reaction temperature reaches 200 °C, reaction kettle is fixed on mechanical stirring axis, opens mechanical stirring
Axis controller allows reaction kettle to make 360 ° rotation movement in perpendicular with agitating shaft, and in this process, tetrafluoroethene is double
Two intracavitary raw materials of intracavitary lining will be sufficiently mixed and be reacted.After carrying out 16h high temperature hybrid reaction under the conditions of 200 °C,
It cools to room temperature with the furnace, obtains reactant；
Step 5: the reactant that step 4 is obtained carries out suction filtration cleaning treatment, obtains white depositions, and using go from
Sub- water and dehydrated alcohol are cleaned repeatedly, until pH=7 of cleaning solution；
Step 6: the white depositions after cleaning are dried for 24 hours under the conditions of 80 °C, obtain porous strontium titanates
Barium powder.
Crystal structure analysis is carried out to prepared porous barium-strontium titanate powder using X-ray diffraction technology, such as Fig. 1 institute
Show, can the product have perovskite structure, diffraction maximum be with standard card JCPDS:35-0734 coincide.It can be seen that institute
Obtaining barium strontium titanate porous powder has good crystallinity, and purity is higher.
Embodiment two:
The present embodiment is a kind of porous barium strontium titanate raw powder's production technology, is included the following steps:
Step 1: according to the barium strontium titanate (Ba of required preparation1-x Sr x TiO3, BST) in barium and strontium the mass ratio of the material example
Ba/Sr=5/3 weighs the barium chloride (BaCl of 0.10mol/L2) and 0.06mol/L strontium nitrate [Sr (NO3)2], prepare Ba and Sr
Total ion concentration is 20 ml of aqueous solution of 0.16 mol/L.The mineralizer hydrogen-oxygen that 2.0mol/L is added in solution is stated then up
Change potassium (KOH), 30 min of stirring wait for that it sufficiently dissolve and after evenly mixing, and above-mentioned mixed solution is transferred to polytetrafluoroethylene (PTFE) pair
One of intracavitary lining is intracavitary；
Step 2: being that 0.04 mol/L weighs butyl titanate according to Ti ratio in entire reaction system, then thereto
A small amount of deionized water and dilute nitric acid solution is added, to inhibit the hydrolysis of butyl titanate, then shifts the solution of preparation
Another to homemade polytetrafluoroethylene (PTFE) two-chamber liner is intracavitary；
Step 3: will be placed with Step 1: the polytetrafluoroethyllining lining for the reaction precursor liquid solution that step 2 obtains is placed in not
In steel pyroreaction kettle of becoming rusty, in order to avoid the mixing of reaction raw materials in two cavitys of polytetrafluoroethyllining lining, in seal process
Remain that polytetrafluoroethyllining lining is in plumbness.The pyroreaction kettle being sealed is disposed vertically in hydro-thermal baking oven,
Temperature control program is set, oven temperature is increased to 200 °C；
Step 4: when reaction temperature reaches 200 °C, reaction kettle is fixed on mechanical stirring axis, opens mechanical stirring
Axis controller allows reaction kettle to make 360 ° rotation movement in perpendicular with agitating shaft.In this process, polytetrafluoroethylene (PTFE)
Two intracorporal raw materials of chamber of liner will be sufficiently mixed and be reacted, after carrying out 16h high temperature hybrid reaction under the conditions of 200 °C,
It cools to room temperature with the furnace, obtains reactant；
Step 5: resulting reactant is subjected to suction filtration cleaning treatment, white depositions is obtained, utilizes deionized water and nothing
Water-ethanol is cleaned repeatedly, until pH=7 of cleaning solution；
Step 6: the white depositions after cleaning are dried for 24 hours under the conditions of 80 °C, obtain porous strontium titanates
Barium powder.
Microcosmic shape is carried out to prepared porous barium-strontium titanate powder using field emission scanning electron microscope (FE-SEM)
Looks analysis, as shown in Fig. 2, barium-strontium titanate powder prepared by this method has hole configurations, individual particle is by multiple nanometers
Good dispersibility is presented in grain composition, this micro--secondary structure of receiving.
Embodiment three:
The present embodiment is related to a kind of porous barium strontium titanate raw powder's production technology, includes the following steps:
Step 1: according to the barium strontium titanate (Ba of required preparation1-x Sr x TiO3, BST) in barium and strontium the mass ratio of the material example
Ba/Sr=1/3 weighs the barium chloride (BaCl of 0.04mol/L2) and 0.12mol/L strontium nitrate [Sr (NO3)2], prepare A from
Sub- concentration (Ba+Sr) is 20 ml of aqueous solution of 0.16 mol/L.The mineralizer hydrogen that 2.0mol/L is added in solution is stated then up
Potassium oxide (KOH), 30 min of stirring wait for that it is sufficiently dissolved and after evenly mixing, is transferred to polytetrafluoroethylene (PTFE) for above-mentioned mixed solution
One of two-chamber liner is intracavitary；
Step 2: being that 0.04 mol/L weighs butyl titanate according to Ti ratio in entire reaction system, then thereto
A small amount of deionized water and dilute nitric acid solution is added, to inhibit the hydrolysis of butyl titanate.Then the solution of preparation is shifted
Another to polytetrafluoroethylene (PTFE) two-chamber liner is intracavitary；
Step 3: will be placed with Step 1: the polytetrafluoroethyllining lining for the reaction precursor liquid solution that step 2 obtains is placed in not
In steel pyroreaction kettle of becoming rusty, in order to avoid the mixing of reaction raw materials in two cavitys of polytetrafluoroethyllining lining, in seal process
Remain that polytetrafluoroethyllining lining is in plumbness.The pyroreaction kettle being sealed is disposed vertically in hydro-thermal baking oven,
Temperature control program is set, oven temperature is increased to 200 °C；
Step 4: when reaction temperature reaches 200 °C, reaction kettle is fixed on mechanical stirring axis, opens mechanical stirring
Axis controller allows reaction kettle to make 360 ° rotation movement in perpendicular with agitating shaft.In this process, polytetrafluoroethylene (PTFE)
Two intracorporal raw materials of chamber of liner will be sufficiently mixed and be reacted.After carrying out 16h high temperature hybrid reaction under the conditions of 200 °C,
It cools to room temperature with the furnace, obtains reactant；
Step 5: resulting reactant is subjected to suction filtration cleaning treatment, white depositions is obtained, utilizes deionized water and nothing
Water-ethanol is cleaned repeatedly, until pH=7 of cleaning solution；
Step 6: the white depositions after cleaning are dried for 24 hours under the conditions of 80 °C, obtain porous strontium titanates
Barium powder.
Morphology analysis, such as Fig. 3 are carried out to prepared powder using field emission scanning electron microscope (FE-SEM)
Shown, barium-strontium titanate powder prepared by this method has porous structure, particle size uniformity, favorable dispersibility.
Claims (1)
1. a kind of porous barium strontium titanate raw powder's production technology, characterized in that it comprises the following steps:
Step 1: according to barium strontium titanate molecular formula Ba1-xSrxTiO3The component ratio x of middle barium and strontium, wherein x=0.375~
0.75, weigh BaCl2With Sr (NO3)2, prepare and obtain the aqueous solution 20ml that Ba and Sr total ion concentration is 0.16mol/L；Then
Suitable potassium hydroxide is added into above-mentioned solution as mineralizer, stirs 30min and waits for that it sufficiently dissolves and is uniformly mixed to get
Mixed solution, then by resulting mixed solution be transferred to first of polytetrafluoroethylene (PTFE) two-chamber liner it is intracavitary；
Step 2: claim according to the ratio that molar ratio between the amount of the amount and titanium substance of barium in entire reaction system and strontium substance is 4
The butyl titanate of corrresponding quality is taken, a small amount of deionized water and dilute nitric acid solution are then added thereto, to inhibit metatitanic acid four
Butyl ester hydrolysis, then by prepared solution be transferred to second of polytetrafluoroethylene (PTFE) two-chamber liner it is intracavitary；
Step 3: it by the polytetrafluoroethyllining lining merging stainless steel high temperature reaction kettle of step 2, seals and is disposed vertically in water
In oven heat, oven temperature is increased to 180~220 DEG C；
Step 4: when heating reaches 180~220 DEG C, so that reaction kettle is constantly in rollover states, make stainless steel high temperature reaction kettle two
A intracavitary reaction raw materials are sufficiently mixed, and are cooled to room temperature with the furnace after reacting 15~20h, are obtained reactant；
Step 5: the reactant that step 4 is obtained carries out suction filtration cleaning treatment, obtains white depositions, through deionized water and nothing
Water-ethanol cleans for several times, until cleaning solution pH value is 7；
Step 6: the white depositions after cleaning are dried for 24 hours under the conditions of 80 DEG C, obtain porous barium strontium titanate powder
Body.
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Effective date of registration: 20191204 Address after: Baixia District of Nanjing City, Jiangsu province 210017 Camp No. 4 Bauhinia 5 storey building No. 5 Patentee after: Nanjing Yure Material Technology Co., Ltd. Address before: Yudaojie Nanjing 210016 Jiangsu province No. 29 Co-patentee before: Nanjing Yure Material Technology Co., Ltd. Patentee before: Nanjing University of Aeronautics and Astronautics |