CN106268612A - 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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- CN106268612A CN106268612A CN201610648817.9A CN201610648817A CN106268612A CN 106268612 A CN106268612 A CN 106268612A CN 201610648817 A CN201610648817 A CN 201610648817A CN 106268612 A CN106268612 A CN 106268612A
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- strontium titanate
- barium
- porous
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- 229910052454 barium strontium titanate Inorganic materials 0.000 title claims abstract description 46
- 239000000843 powder Substances 0.000 title claims abstract description 33
- 238000005516 engineering process Methods 0.000 title claims description 10
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 238000002360 preparation method Methods 0.000 claims abstract description 17
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 229910052788 barium Inorganic materials 0.000 claims description 11
- 238000004140 cleaning Methods 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000000151 deposition Methods 0.000 claims description 10
- 230000008021 deposition Effects 0.000 claims description 10
- 229950000845 politef Drugs 0.000 claims description 10
- 239000000376 reactant Substances 0.000 claims description 10
- 229910052712 strontium Inorganic materials 0.000 claims description 10
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 8
- 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
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 7
- 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
- 238000001914 filtration Methods 0.000 claims description 5
- 239000012530 fluid Substances 0.000 claims description 5
- 230000007062 hydrolysis Effects 0.000 claims description 5
- 238000006460 hydrolysis reaction Methods 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 150000002500 ions Chemical class 0.000 claims description 3
- 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 claims description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 230000004044 response Effects 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 24
- 239000000463 material Substances 0.000 abstract description 11
- 238000002156 mixing Methods 0.000 abstract description 10
- 239000002243 precursor Substances 0.000 abstract description 6
- 238000001354 calcination Methods 0.000 abstract description 5
- 239000000919 ceramic Substances 0.000 abstract description 5
- 208000002925 dental caries Diseases 0.000 abstract description 5
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000004088 foaming agent Substances 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 230000008569 process Effects 0.000 description 11
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 7
- 238000013019 agitation Methods 0.000 description 6
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 description 6
- 239000002086 nanomaterial Substances 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 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
- 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
- 230000033001 locomotion Effects 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
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical group O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 239000011148 porous material 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
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 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
- 239000002253 acid Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910001422 barium ion 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
- 230000033228 biological regulation Effects 0.000 description 1
- 229960004424 carbon dioxide Drugs 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 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
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000001802 infusion Methods 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
- QKKWJYSVXDGOOJ-UHFFFAOYSA-N oxalic acid;oxotitanium Chemical compound [Ti]=O.OC(=O)C(O)=O QKKWJYSVXDGOOJ-UHFFFAOYSA-N 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000012704 polymeric precursor Substances 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 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
- 229910001427 strontium ion Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005979 thermal decomposition reaction 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
-
- 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 & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Analytical Chemistry (AREA)
- Ceramic Engineering (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Structural Engineering (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses the preparation method of a kind of micro-nano porous structure barium-strontium titanate powder, particularly under hydrothermal high-temperature admixture, realize the synthesis of micro-nano porous structure barium-strontium titanate powder, in the method for the present invention, two kinds of solution as precursors are respectively placed in two cavitys of tetrafluoroethene two-chamber liner, carry out mixing pyroreaction in time being warmed up to 180 ~ 220 ° of C again.Compared with prior art, not using organic foaming agent in the method course of reaction of the present invention, cost of material is lower, has more preferable environment friendly；React under gentle thermal and hydric environment, it is not necessary to calcination processing, energy resource consumption is low, has good stability and repeatability；Prepared porous barium strontium titanate has the micro-nano secondary structure of uniqueness, has bigger specific surface area, and stability is more preferable, has dimensional homogeneity and the dispersibility of excellence, at function ceramics, is catalyzed and is with a wide range of applications in terms of absorption.
Description
Technical field
The present invention relates to a kind of porous barium strontium titanate raw powder's production technology, particularly relate to a kind of hydrothermal high-temperature mixing method and close
Become the method with micro-nano structure porous barium-strontium titanate powder, belong to inorganic non-metallic field of functional materials.
Background technology
Barium strontium titanate has perovskite structure, is the quite varied inorganic non-metallic functional material of a kind of purposes, and it is main
Advantage includes that Heat stability is good, dielectric loss are low, dielectric constant is high.Owing to, in perovskite structure, positive and negative charge center is not
The generation of coincidence meeting induced spontaneous polarization, the existence of this built in field can effectively facilitate the compound of electron-hole pair, extend
The life-span of carrier.Therefore, barium strontium titanate is as a kind of semi-conducting material, and energy gap 3.2 ~ 3.8 eV is in recent years in photocatalysis
Field has obtained increasing concern, before the aspects such as photocatalysis hydrogen production, photocatalytic degradation Organic substance have wide application
Scape.
In order to meet the barium strontium titanate use requirement in catalysis with adsorbing domain, need to develop that there is large specific surface area
Porous type barium strontium titanate material.Usually, in solid phase method carries out barium-strontium titanate ceramic preparation process, by adding organic
Infusion, such as polymethyl methacrylate (PMMA, Polymethyl methacrylate), polyvinyl alcohol (Polyvinyl
Alcohol, PVA), polyvinyl butyral resin (Polyvinyl butyral, PVB), triethanolamine
(Triethanolamine, TEA) etc., thus prepared 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 CNT or graphite, utilize height
In temperature calcination process, the production of carbon dioxide forms Micro porosity.But, the formation of porous ceramics is micro-along with pottery itself
Seeing leakiness, the microcellular structure specific surface area of gained is the highest.In order to increase specific surface area, it is necessary to carry out nanoscale metatitanic acid
The preparation of strontium barium powder body.But, nano-powder itself has a disadvantage that it is easily to reunite, and this will make the specific surface of itself
Amass and greatly reduce, be unfavorable for the performance of performance.
Micro-nano structure belongs to the orderly aggregate of secondary of nano material, and on the one hand it can retain the high of nano material and live
Property, the most also it is avoided that reunion disadvantageous for performance.In terms of barium strontium titanate, development has the powder body tool of micro-nano porous structure
Significant.There is researcher by thermal decomposition barium titanium oxalate [barium titanyl oxalate, BaTiO (C2O4)2·
4H2O] carry out the preparation of the powder body of porous barium strontium titanate, it is substantially to utilize organic decomposition generation two in calcination process
Carbonoxide, thus formed pore space structure (Journal of the American Ceramic Society,2009,92,3132–3134).Additionally, use sol-gel process to prepare the process of porous Sr titanate powder
In, by adding triethanolamine (Triethanolamine, TEA), the size in aperture is controlled by the addition of regulation TEA
System (Chem.Mater., 2000, 12 (9), 2590–2596).Brazil scholar A. Ries etc. uses polymer
Precursor process (Polymeric precursor method, PPM) is prepared for the barium strontium titanate of component ratio Ba/Sr=80/20
Porous powder.Later stage calcination processing process makes particle size uniformity poor, agglomeration more serious (Materials Characterization, 2003, 50, 217– 221).So far, also there is a small amount of Chinese patent open
The preparation method of strontium titanates/barium loose structure is (such as: the preparation side of a kind of strontium titanate film having spherical grain accumulated porous structure
Method, CN 102390935A;A kind of preparation method of porous balls of strontium titanate, CN 101092244A).But, said method is made
Standby porous strontium titanates/barium belongs to the unsound block materials of microstructure, and specific surface area is the abundantest, uniformity
Difference.
Summary of the invention
Technical problem
Present invention aim to address the deficiencies in the prior art, propose to prepare under a kind of hydrothermal condition porous barium-strontium titanate powder
Method, the porous barium strontium titanate powder specific-surface area detection prepared by the method is big, size uniform, good dispersion.
Technical scheme
In order to solve above-mentioned technical problem, a kind of porous barium strontium titanate raw powder's production technology of the present invention, it is characterised in that
Comprise the following steps:
Step one: according to barium strontium titanate molecular formula Ba1-x Sr x TiO3Middle barium and the component ratio of strontiumx, whereinx=0 ~ 1.0, claim
Take BaCl2With Sr (NO3)2, preparation obtains the aqueous solution 20ml that Ba and Sr total ion concentration is 0.16 mol/L；State then up
Adding appropriate potassium hydroxide in solution as mineralizer, stirring 30min treats that it fully dissolves and to be uniformly mixed to get mixing molten
Liquid, then the mixed solution of gained is transferred to first intracavity of politef two-chamber liner；
Step 2: according to the ratio of (Ba+Sr)/Ti=4 in whole reaction system, weighs the butyl titanate of respective quality, then
It is added thereto to a small amount of deionized water and dilute nitric acid solution, to suppress tetrabutyl titanate hydrolysis, the solution then will prepared
It is transferred to second intracavity of politef two-chamber liner；
Step 3: the polytetrafluoroethyllining lining of step 2 inserted in stainless steel high temperature reactor, seals and is disposed vertically in water
In oven heat, oven temperature is increased to 180 ~ 220 ° of C；
Step 4: when intensification reaches 180 ~ 220 ° of C, make reactor be constantly in rollover states, make stainless steel high temperature reactor two
The reaction raw materials of individual intracavity is sufficiently mixed, and cools to room temperature with the furnace, obtain reactant after question response 15 ~ 20 h；
Step 5: reactant step 4 obtained carries out sucking filtration cleaning treatment, obtains white depositions, through deionized water and nothing
Water-ethanol cleans for several times, until cleanout fluid pH value is 7；
Step 6: the white depositions after cleaning carries out 24h dried under the conditions of 80 ° of C, obtains porous barium strontium titanate
Powder body.
In the method for the present invention, it is respectively placed in two of tetrafluoroethene two-chamber liner as two kinds of solution of precursors
In cavity, carry out again mixing pyroreaction in time being warmed up to 180 ~ 220 ° of C.
Beneficial effect
Compared with prior art, the method for the present invention has the advantages that
(1) not using organic foaming agent in course of reaction, cost of material is lower, has more preferable environment friendly；
(2) reacting under gentle thermal and hydric environment, it is not necessary to calcination processing, energy resource consumption is low, have good stability and
Repeatable；
(3) the porous barium strontium titanate prepared by have uniqueness micro--receive secondary structure, there is bigger specific surface area, stability
More preferably, there is dimensional homogeneity and the dispersibility of excellence.
Prepared by the present invention, porous barium-strontium titanate powder has preferably constructing property compared to block materials, makes pottery in function
Porcelain, it is catalyzed and absorption aspect is with a wide range of applications.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of first embodiment of the invention gained porous barium-strontium titanate powder；
Fig. 2 is the field emission scanning electron microscope (FE-SEM) of second embodiment of the invention gained porous barium-strontium titanate powder
Photo；
Fig. 3 is the field emission scanning electron microscope (FE-SEM) of third embodiment of the invention gained porous barium-strontium titanate powder
Photo.
Detailed description of the invention
It is further elucidated with substantive features and the marked improvement of the present invention below by embodiment, but the present invention is only limitted to absolutely not
Embodiment described in described embodiment.The all deformation directly derived by present disclosure or associate, all should recognize
For being protection scope of the present invention.
Embodiment one:
The present embodiment is a kind of porous barium strontium titanate raw powder's production technology, comprises the following steps:
Step one: according to the barium strontium titanate (Ba of required preparation1-x Sr x TiO3, BST) in amount ratio Ba/ of material of barium and strontium
Sr=1, weighs the barium chloride (BaCl of 0.08mol/L2) and the strontium nitrate [Sr (NO of 0.08mol/L3)2], prepare Ba and Sr ion
Total concentration is aqueous solution 20 ml of 0.16 mol/L.State in solution the mineralizer potassium hydroxide adding 2.0mol/L then up
(KOH), stir 30 min until its fully dissolve and uniformly mixing after, above-mentioned mixed solution is transferred in politef two-chamber
One of them intracavity of lining；
Step 2: be that 0.04 mol/L weighs butyl titanate according to Ti ratio in whole reaction system, is then added thereto to
A small amount of deionized water and dilute nitric acid solution, thus suppress the hydrolysis of butyl titanate, the solution then preparation obtained shifts
Another intracavity to politef two-chamber liner；
Step 3: by being placed with step one, the polytetrafluoroethyllining lining of reaction precursor liquid solution that step 2 obtains insert rustless steel
In pyroreaction still, in order to avoid the mixing of two intracavity reaction raw materials, in remaining politef in seal process
Lining is in plumbness；The pyroreaction still of good seal is disposed vertically in hydro-thermal baking oven, sets temperature control program, by baking oven
Temperature is increased to 200 ° of C；
Step 4: when reaction temperature arrives 200 ° of C, reactor is fixed on mechanical agitation axle, opens mechanical agitation axle control
Device processed, allows reactor make 360 ° of rotary motions in perpendicular along with shaft, in this process, in tetrafluoroethene two-chamber
The raw material of two intracavity of lining will be sufficiently mixed and react.After carrying out 16h high temperature hybrid reaction under the conditions of 200 ° of C, with stove
It is cooled to room temperature, obtains reactant；
Step 5: reactant step 4 obtained carries out sucking filtration cleaning treatment, obtains white depositions, and utilizes deionized water
Repeatedly clean with dehydrated alcohol, until the pH=7 of cleanout fluid；
Step 6: the white depositions after cleaning carries out 24h dried under the conditions of 80 ° of C, obtains porous barium strontium titanate powder
Body.
X-ray diffraction technology is used prepared porous barium-strontium titanate powder to be carried out crystal structure analysis, such as Fig. 1 institute
Showing can have perovskite structure by this product, diffraction maximum is to coincide with standard card JCPDS:35-0734.As can be seen here, institute
Obtaining barium strontium titanate porous powder and have good crystallinity, purity is higher.
Embodiment two:
The present embodiment is a kind of porous barium strontium titanate raw powder's production technology, comprises the steps:
Step one: according to the barium strontium titanate (Ba of required preparation1-x Sr x TiO3, BST) in amount ratio Ba/ of material of barium and strontium
Sr=5/3, weighs the barium chloride (BaCl of 0.10mol/L2) and the strontium nitrate [Sr (NO of 0.06mol/L3)2], preparation Ba and Sr from
Sub-total concentration is aqueous solution 20 ml of 0.16 mol/L.State in solution the mineralizer hydroxide adding 2.0mol/L then up
Potassium (KOH), stir 30 min until its fully dissolve and uniformly mixing after, above-mentioned mixed solution is transferred to politef two-chamber
One intracavity of liner；
Step 2: be that 0.04 mol/L weighs butyl titanate according to Ti ratio in whole reaction system, is then added thereto to
A small amount of deionized water and dilute nitric acid solution, thus suppress the hydrolysis of butyl titanate, then the solution of preparation is transferred to certainly
Another intracavity of the politef two-chamber liner of system；
Step 3: by being placed with step one, the polytetrafluoroethyllining lining of reaction precursor liquid solution that step 2 obtains insert rustless steel
In pyroreaction still, in order to avoid the mixing of reaction raw materials in two cavitys of polytetrafluoroethyllining lining, in seal process all the time
Polytetrafluoroethyllining lining is kept to be in plumbness.The pyroreaction still of good seal is disposed vertically in hydro-thermal baking oven, sets
Temperature control program, is increased to 200 ° of C by oven temperature；
Step 4: when reaction temperature arrives 200 ° of C, reactor is fixed on mechanical agitation axle, opens mechanical agitation axle control
Device processed, allows reactor make 360 ° of rotary motions in perpendicular along with shaft.In this process, polytetrafluoroethyllining lining
Raw material in two cavitys will be sufficiently mixed and react, after carrying out 16h high temperature hybrid reaction under the conditions of 200 ° of C, with stove
It is cooled to room temperature, obtains reactant；
Step 5: the reactant of gained is carried out sucking filtration cleaning treatment, obtains white depositions, utilizes deionized water and anhydrous second
Alcohol cleans repeatedly, until the pH=7 of cleanout fluid；
Step 6: the white depositions after cleaning carries out 24h dried under the conditions of 80 ° of C, obtains porous barium strontium titanate powder
Body.
Use field emission scanning electron microscope (FE-SEM) that prepared porous barium-strontium titanate powder is carried out microcosmic shape
Looks are analyzed, as in figure 2 it is shown, the barium-strontium titanate powder prepared by the method has pore space structure, individual particle is by multiple nanometers
Grain composition, this micro--secondary structure of receiving presents good dispersibility.
Embodiment three:
The present embodiment relates to a kind of porous barium strontium titanate raw powder's production technology, comprises the steps:
Step one: according to the barium strontium titanate (Ba of required preparation1-x Sr x TiO3, BST) in amount ratio Ba/ of material of barium and strontium
Sr=1/3, weighs the barium chloride (BaCl of 0.04mol/L2) and the strontium nitrate [Sr (NO of 0.12mol/L3)2], preparation A position ion is dense
Degree (Ba+Sr) is aqueous solution 20 ml of 0.16 mol/L.State in solution the mineralizer hydroxide adding 2.0mol/L then up
Potassium (KOH), stir 30 min until its fully dissolve and uniformly mixing after, above-mentioned mixed solution is transferred to politef two-chamber
One intracavity of liner；
Step 2: be that 0.04 mol/L weighs butyl titanate according to Ti ratio in whole reaction system, is then added thereto to
A small amount of deionized water and dilute nitric acid solution, thus suppress the hydrolysis of butyl titanate.Then it is transferred to gather by the solution of preparation
Another intracavity of tetrafluoroethene two-chamber liner；
Step 3: by being placed with step one, the polytetrafluoroethyllining lining of reaction precursor liquid solution that step 2 obtains insert rustless steel
In pyroreaction still, in order to avoid the mixing of reaction raw materials in two cavitys of polytetrafluoroethyllining lining, in seal process all the time
Polytetrafluoroethyllining lining is kept to be in plumbness.The pyroreaction still of good seal is disposed vertically in hydro-thermal baking oven, sets
Temperature control program, is increased to 200 ° of C by oven temperature；
Step 4: when reaction temperature arrives 200 ° of C, reactor is fixed on mechanical agitation axle, opens mechanical agitation axle control
Device processed, allows reactor make 360 ° of rotary motions in perpendicular along with shaft.In this process, polytetrafluoroethyllining lining
Raw material in two cavitys will be sufficiently mixed and react.After carrying out 16h high temperature hybrid reaction under the conditions of 200 ° of C, with stove
It is cooled to room temperature, obtains reactant；
Step 5: the reactant of gained is carried out sucking filtration cleaning treatment, obtains white depositions, utilizes deionized water and anhydrous second
Alcohol cleans repeatedly, until the pH=7 of cleanout fluid；
Step 6: the white depositions after cleaning carries out 24h dried under the conditions of 80 ° of C, obtains porous barium strontium titanate powder
Body.
Field emission scanning electron microscope (FE-SEM) is used prepared powder body to be carried out Morphology analysis, such as Fig. 3
Shown in, the barium-strontium titanate powder prepared by the method has loose structure, particle size uniformity, favorable dispersibility.
Claims (1)
1. a porous barium strontium titanate raw powder's production technology, it is characterised in that comprise the following steps:
Step one: according to barium strontium titanate molecular formula Ba1-x Sr x TiO3Middle barium and the component ratio of strontiumx, whereinx=0 ~ 1.0, weigh
BaCl2With Sr (NO3)2, preparation obtains the aqueous solution 20ml that Ba and Sr total ion concentration is 0.16 mol/L；State molten then up
Liquid adds appropriate potassium hydroxide and treats that it fully dissolves and is uniformly mixed to get mixed solution as mineralizer, stirring 30min,
The mixed solution of gained is transferred to first intracavity of politef two-chamber liner again；
Step 2: according to the ratio of (Ba+Sr)/Ti=4 in whole reaction system, weighs the butyl titanate of respective quality, then
It is added thereto to a small amount of deionized water and dilute nitric acid solution, to suppress tetrabutyl titanate hydrolysis, the solution then will prepared
It is transferred to second intracavity of politef two-chamber liner；
Step 3: the polytetrafluoroethyllining lining of step 2 inserted in stainless steel high temperature reactor, seals and is disposed vertically in water
In oven heat, oven temperature is increased to 180 ~ 220 ° of C；
Step 4: when intensification reaches 180 ~ 220 ° of C, make reactor be constantly in rollover states, make stainless steel high temperature reactor two
The reaction raw materials of individual intracavity is sufficiently mixed, and cools to room temperature with the furnace, obtain reactant after question response 15 ~ 20 h；
Step 5: reactant step 4 obtained carries out sucking filtration cleaning treatment, obtains white depositions, through deionized water and nothing
Water-ethanol cleans for several times, until cleanout fluid pH value is 7；
Step 6: the white depositions after cleaning carries out 24h dried under the conditions of 80 ° of C, obtains porous barium strontium titanate
Powder body.
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| CN113600169A (en) * | 2021-06-08 | 2021-11-05 | 电子科技大学长三角研究院(湖州) | Solid solution photocatalyst for photocatalytic oxidation degradation of toluene and preparation method thereof |
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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 |