CN108435129A - A method of preparing Sr-Ti-In ternary oxide molecular sieves - Google Patents
A method of preparing Sr-Ti-In ternary oxide molecular sieves Download PDFInfo
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- CN108435129A CN108435129A CN201810218888.4A CN201810218888A CN108435129A CN 108435129 A CN108435129 A CN 108435129A CN 201810218888 A CN201810218888 A CN 201810218888A CN 108435129 A CN108435129 A CN 108435129A
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- 239000002808 molecular sieve Substances 0.000 title claims abstract description 27
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 11
- 239000000243 solution Substances 0.000 claims abstract description 33
- 239000000463 material Substances 0.000 claims abstract description 19
- 239000010936 titanium Substances 0.000 claims abstract description 18
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 18
- 230000001476 alcoholic effect Effects 0.000 claims abstract description 17
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 12
- MDFMZCSBYVYIAZ-UHFFFAOYSA-N [Sr].[In] Chemical compound [Sr].[In] MDFMZCSBYVYIAZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000002390 rotary evaporation Methods 0.000 claims abstract description 11
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims abstract description 6
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims abstract description 6
- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical compound N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-UHFFFAOYSA-N 0.000 claims abstract description 6
- 230000032683 aging Effects 0.000 claims abstract description 6
- 235000019257 ammonium acetate Nutrition 0.000 claims abstract description 6
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 235000019441 ethanol Nutrition 0.000 claims abstract description 6
- 229910052738 indium Inorganic materials 0.000 claims abstract description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 6
- 239000010935 stainless steel Substances 0.000 claims abstract description 6
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 6
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 10
- 239000012065 filter cake Substances 0.000 claims description 10
- 239000003643 water by type Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000009833 condensation Methods 0.000 claims description 5
- 230000005494 condensation Effects 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000005485 electric heating Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000004570 mortar (masonry) Substances 0.000 claims description 5
- 229910052573 porcelain Inorganic materials 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 239000012265 solid product Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical class [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 claims description 5
- 239000008399 tap water Substances 0.000 claims description 5
- 235000020679 tap water Nutrition 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 3
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 2
- 239000005695 Ammonium acetate Substances 0.000 abstract 1
- 229940043376 ammonium acetate Drugs 0.000 abstract 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 abstract 1
- 238000003837 high-temperature calcination Methods 0.000 abstract 1
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 abstract 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 abstract 1
- 238000000465 moulding Methods 0.000 abstract 1
- 229910000018 strontium carbonate Inorganic materials 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 230000001699 photocatalysis Effects 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000010718 Oxidation Activity Effects 0.000 description 1
- UGACIEPFGXRWCH-UHFFFAOYSA-N [Si].[Ti] Chemical compound [Si].[Ti] UGACIEPFGXRWCH-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000009510 drug design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000010525 oxidative degradation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis 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
- B01J29/00—Catalysts comprising molecular sieves
-
- 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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- 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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
-
- 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
- B01J20/28002—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 physical properties
- B01J20/28004—Sorbent size or size distribution, e.g. particle size
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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
- B01J20/28—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
- B01J20/28016—Particle form
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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- Inorganic Compounds Of Heavy Metals (AREA)
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Abstract
A method of Sr Ti In ternary oxide molecular sieves are prepared, surrounding purifying material field, including following processing steps are belonged to：Strontium indium mixed solution is prepared with aqueous ammonium chloride solution, strontium carbonate and indium nitrate aqueous solution, template titanium alcoholic solution is prepared with ethyl alcohol, ammonium acetate, tetrabutyl titanate, octadecylamine and strontium indium mixed solution, template titanium alcoholic solution rotary evaporation to volume is basically unchanged, hydro-thermal pore-creating is carried out in stainless steel cauldron, and aging molding is carried out by freeze-day with constant temperature and high-temperature calcination.The material can be used for the absorption of organic pollution and photocatalytic degradation in environment.
Description
Technical field：
The invention belongs to surrounding purifying material fields, and in particular to a kind of side preparing Sr-Ti-In ternary oxide molecular sieves
Method.
Background technology：
Molecular sieve refers to having uniform pore structure, can accommodate a substance of organic molecule.Molecular sieve is typically to tie
The alumino-silicate of crystal form, it is also possible to which other element portions substitution framework silicons or aluminium form heteroatom type molecular sieve.Framework of molecular sieve
It is a kind of high-efficiency adsorbent that there are ducts and cavity to have prodigious specific surface area in structure.Energy spectrum sieve usually with
Silicon is the basic element for forming skeleton, also there is the trial that molecular sieve is prepared using titanium silicon recently.Although such molecular sieve has one
Fixed adsorption capacity cannot but make organic pollution oxygenolysis, i.e., not have Photocatalytic oxidation activity under light illumination.Photocatalysis
Oxidation, purification technology is a kind of efficient advanced oxidation technology, and the organic pollution point in air and water can be made under the action of light
Solution, to achieve the purpose that pollution administration.The technology has played great function in various pollution control fields.New and effective
Catalysis material is the key factor of this technology and the target of numerous researchers effort for many years.Organic pollution is present in
In a variety of media of big gas and water and solid waste etc..Organic pollution is of different sizes because of molecular composition and structure difference,
Pore structure and size to catalysis material have different requirements.Although Photocatalytic Oxidation betides the table of material
Face, and must have the excitation process of specific light source, the adsorption capacity of porous material is still to its photocatalytic activity with important
Influence.Molecular sieve type photochemical catalyst not only has stronger adsorption capacity, and also having has in illumination condition declines solution environment
The activity of machine pollutant.Titanium has the reactivity being remarkably reinforced, Sr-Ti- with catalysis material prepared by other elements compoundings
In ternary oxide molecular sieves are a kind of new materials.
Invention content：
In view of the problems of the existing technology, the present invention is intended to provide a kind of side preparing Sr-Ti-In ternary oxide molecular sieves
Method.For such molecular sieve with Sr-Ti-In ternary oxide ingredient sieve skeleton framves, molecular sieve bore diameter is nano-scale, can be used for ring
The absorption of organic pollution and photocatalytic degradation in border.
The technical solution adopted by the present invention is：
A method of preparing Sr-Ti-In ternary oxide molecular sieves, including following processing steps：
Step 1：Prepare strontium-indium mixed solution
1.1 are added 5 ~ 10g strontium carbonates in 200 mL 0.1mol/L aqueous ammonium chloride solutions, and stirring is allowed to be completely dissolved；
1.2 60 ~ 150 mL 0.3mol/L indium nitrate aqueous solutions are added into above-mentioned solution, are uniformly mixed, and strontium-indium mixing is made
Solution, it is spare.
Step 2：Prepare template-titanium alcoholic solution
2.1 take two mouthfuls of 1L round-bottomed flasks 1, install temperature thermocouple and spherical condensation tube, it is cold that condenser pipe is passed through tap water progress
But；
2.2 are added 260 ~ 320 mL ethyl alcohol, 8 ~ 11g ammonium acetates, 22 ~ 25 mL tetrabutyl titanates, 3 ~ 5g octadecylamines in flask,
Above-mentioned material is pure material；Flask is placed in 72 DEG C of waters bath with thermostatic control, flow back 50 min；
2.3 pour into the strontium in step 1.2-indium mixed solution in flask, continue 70 min that flow back in 72 DEG C of waters bath with thermostatic control,
Template-titanium alcoholic solution is made.
Step 3：Rotary evaporation hydrolyzes
3.1 install flask on the rotary evaporator, keep 85 DEG C of bath temperature, speed of rotation 150rpm, system is decompressed to
500 mmHg, by template in flask-titanium alcoholic solution rotary evaporation until volume is basically unchanged.
Step 4：Hydro-thermal pore-creating
4.1 move into remaining liq in flask in stainless steel cauldron, 195 ~ 215 DEG C of controlling reaction temperature, reaction system pressure
2.5 ~ 3 MPa, 55 ~ 75 h of reaction time；
4.2 after reaction, and solid-liquid mix products are filtered, and filter cake is cleaned with deionized water；
Step 5：Aging is molded
Filter cake is placed 48 h by 5.1 in 220 DEG C of constant temperature electric heating drying boxes；
Solid product after drying is calcined 3 ~ 6 h at 530 ~ 660 DEG C by 5.2, and being ground into grain size in porcelain mortar after cooling is less than
5 μm of powder obtains Sr-Ti-In ternary oxide molecular sieves.
Compared with the prior art, the advantages of the present invention are as follows：
For the present invention by the rational design to raw material composition and synthesis technology, optimization generates the oxidation of molecular sieve type Sr-Ti-In ternarys
The preparation condition of object.The prepared new material not only ability with molecular sieve adsorbing and removing pollutant, while can also be
Oxidative degradation organic pollution under illumination has very extensive purposes.Preparation process controllability provided by the invention is good, generates
Sr-Ti-In ternary oxides sieve particle and pore-size it is uniform, performance stablize.
Specific implementation mode：
Embodiment 1
A method of preparing Sr-Ti-In ternary oxide molecular sieves, including following processing steps：
Step 1：Prepare strontium-indium mixed solution
1.1 are added 5g strontium carbonates in 200 mL 0.1mol/L aqueous ammonium chloride solutions, and stirring is allowed to be completely dissolved；
1.2 60 mL 0.3mol/L indium nitrate aqueous solutions are added into above-mentioned solution, are uniformly mixed, and it is molten that strontium-indium mixing is made
Liquid, it is spare.
Step 2：Prepare template-titanium alcoholic solution
2.1 take two mouthfuls of 1L round-bottomed flasks 1, install temperature thermocouple and spherical condensation tube, it is cold that condenser pipe is passed through tap water progress
But；
2.2 are added 260 mL ethyl alcohol, 8g ammonium acetates, 22 mL tetrabutyl titanates, 3g octadecylamines in flask, and above-mentioned material is pure
Material；Flask is placed in 72 DEG C of waters bath with thermostatic control, flow back 50 min；
2.3 pour into the strontium in step 1.2-indium mixed solution in flask, continue 70 min that flow back in 72 DEG C of waters bath with thermostatic control,
Template-titanium alcoholic solution is made.
Step 3：Rotary evaporation hydrolyzes
3.1 install flask on the rotary evaporator, keep 85 DEG C of bath temperature, speed of rotation 150rpm, system is decompressed to
500 mmHg, by template in flask-titanium alcoholic solution rotary evaporation until volume is basically unchanged.
Step 4：Hydro-thermal pore-creating
4.1 move into remaining liq in flask in stainless steel cauldron, 195 DEG C of controlling reaction temperature, reaction system pressure 2.5
MPa, 55 h of reaction time；
4.2 after reaction, and solid-liquid mix products are filtered, and filter cake is cleaned with deionized water；
Step 5：Aging is molded
Filter cake is placed 48 h by 5.1 in 220 DEG C of constant temperature electric heating drying boxes；
Solid product after drying is calcined 6 h at 530 DEG C by 5.2, is ground into grain size after cooling in porcelain mortar and is less than 5 μm
Powder obtains Sr-Ti-In ternary oxide molecular sieves.
Embodiment 2
A method of preparing Sr-Ti-In ternary oxide molecular sieves, including following processing steps：
Step 1：Prepare strontium-indium mixed solution
1.1 are added 7g strontium carbonates in 200 mL 0.1mol/L aqueous ammonium chloride solutions, and stirring is allowed to be completely dissolved；
1.2 90 mL 0.3mol/L indium nitrate aqueous solutions are added into above-mentioned solution, are uniformly mixed, and it is molten that strontium-indium mixing is made
Liquid, it is spare.
Step 2：Prepare template-titanium alcoholic solution
2.1 take two mouthfuls of 1L round-bottomed flasks 1, install temperature thermocouple and spherical condensation tube, it is cold that condenser pipe is passed through tap water progress
But；
2.2 are added 290 mL ethyl alcohol, 9g ammonium acetates, 23 mL tetrabutyl titanates, 4g octadecylamines in flask, and above-mentioned material is pure
Material；Flask is placed in 72 DEG C of waters bath with thermostatic control, flow back 50 min；
2.3 pour into the strontium in step 1.2-indium mixed solution in flask, continue 70 min that flow back in 72 DEG C of waters bath with thermostatic control,
Template-titanium alcoholic solution is made.
Step 3：Rotary evaporation hydrolyzes
3.1 install flask on the rotary evaporator, keep 85 DEG C of bath temperature, speed of rotation 150rpm, system is decompressed to
500 mmHg, by template in flask-titanium alcoholic solution rotary evaporation until volume is basically unchanged.
Step 4：Hydro-thermal pore-creating
4.1 move into remaining liq in flask in stainless steel cauldron, 205 DEG C of controlling reaction temperature, reaction system pressure 2.7
MPa, 63 h of reaction time；
4.2 after reaction, and solid-liquid mix products are filtered, and filter cake is cleaned with deionized water；
Step 5：Aging is molded
Filter cake is placed 48 h by 5.1 in 220 DEG C of constant temperature electric heating drying boxes；
Solid product after drying is calcined 4 h at 580 DEG C by 5.2, is ground into grain size after cooling in porcelain mortar and is less than 5 μm
Powder obtains Sr-Ti-In ternary oxide molecular sieves.
Embodiment 3
A method of preparing Sr-Ti-In ternary oxide molecular sieves, including following processing steps：
Step 1：Prepare strontium-indium mixed solution
1.1 are added 10g strontium carbonates in 200 mL 0.1mol/L aqueous ammonium chloride solutions, and stirring is allowed to be completely dissolved；
1.2 150 mL 0.3mol/L indium nitrate aqueous solutions are added into above-mentioned solution, are uniformly mixed, and it is molten that strontium-indium mixing is made
Liquid, it is spare.
Step 2：Prepare template-titanium alcoholic solution
2.1 take two mouthfuls of 1L round-bottomed flasks 1, install temperature thermocouple and spherical condensation tube, it is cold that condenser pipe is passed through tap water progress
But；
2.2 are added 320 mL ethyl alcohol, 11g ammonium acetates, 25 mL tetrabutyl titanates, 5g octadecylamines in flask, and above-mentioned material is
Pure material；Flask is placed in 72 DEG C of waters bath with thermostatic control, flow back 50 min；
2.3 pour into the strontium in step 1.2-indium mixed solution in flask, continue 70 min that flow back in 72 DEG C of waters bath with thermostatic control,
Template-titanium alcoholic solution is made.
Step 3：Rotary evaporation hydrolyzes
3.1 install flask on the rotary evaporator, keep 85 DEG C of bath temperature, speed of rotation 150rpm, system is decompressed to
500 mmHg, by template in flask-titanium alcoholic solution rotary evaporation until volume is basically unchanged.
Step 4：Hydro-thermal pore-creating
4.1 move into remaining liq in flask in stainless steel cauldron, 215 DEG C of controlling reaction temperature, reaction system pressure 3
MPa, 75 h of reaction time；
4.2 after reaction, and solid-liquid mix products are filtered, and filter cake is cleaned with deionized water；
Step 5：Aging is molded
Filter cake is placed 48 h by 5.1 in 220 DEG C of constant temperature electric heating drying boxes；
Solid product after drying is calcined 3 h at 660 DEG C by 5.2, is ground into grain size after cooling in porcelain mortar and is less than 5 μm
Powder obtains Sr-Ti-In ternary oxide molecular sieves.
Claims (1)
1. a kind of method preparing Sr-Ti-In ternary oxide molecular sieves, which is characterized in that including following processing steps：
Step 1：Prepare strontium-indium mixed solution
1.1 are added 5 ~ 10g strontium carbonates in 200 mL 0.1mol/L aqueous ammonium chloride solutions, and stirring is allowed to be completely dissolved；
1.2 60 ~ 150 mL 0.3mol/L indium nitrate aqueous solutions are added into above-mentioned solution, are uniformly mixed, and strontium-indium mixing is made
Solution, it is spare；
Step 2：Prepare template-titanium alcoholic solution
2.1 take two mouthfuls of 1L round-bottomed flasks 1, install temperature thermocouple and spherical condensation tube, it is cold that condenser pipe is passed through tap water progress
But；
2.2 are added 260 ~ 320 mL ethyl alcohol, 8 ~ 11g ammonium acetates, 22 ~ 25 mL tetrabutyl titanates, 3 ~ 5g octadecylamines in flask,
Above-mentioned material is pure material；Flask is placed in 72 DEG C of waters bath with thermostatic control, flow back 50 min；
2.3 pour into the strontium in step 1.2-indium mixed solution in flask, continue 70 min that flow back in 72 DEG C of waters bath with thermostatic control,
Template-titanium alcoholic solution is made；
Step 3：Rotary evaporation hydrolyzes
3.1 install flask on the rotary evaporator, keep 85 DEG C of bath temperature, speed of rotation 150rpm, system is decompressed to
500 mmHg, by template in flask-titanium alcoholic solution rotary evaporation until volume is basically unchanged；
Step 4：Hydro-thermal pore-creating
4.1 move into remaining liq in flask in stainless steel cauldron, 195 ~ 215 DEG C of controlling reaction temperature, reaction system pressure
2.5 ~ 3 MPa, 55 ~ 75 h of reaction time；
4.2 after reaction, and solid-liquid mix products are filtered, and filter cake is cleaned with deionized water；
Step 5：Aging is molded
Filter cake is placed 48 h by 5.1 in 220 DEG C of constant temperature electric heating drying boxes；
Solid product after drying is calcined 3 ~ 6 h at 530 ~ 660 DEG C by 5.2, and being ground into grain size in porcelain mortar after cooling is less than
5 μm of powder obtains Sr-Ti-In ternary oxide molecular sieves.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810218888.4A CN108435129B (en) | 2018-03-16 | 2018-03-16 | Method for preparing Sr-Ti-In ternary oxide molecular sieve |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810218888.4A CN108435129B (en) | 2018-03-16 | 2018-03-16 | Method for preparing Sr-Ti-In ternary oxide molecular sieve |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108435129A true CN108435129A (en) | 2018-08-24 |
| CN108435129B CN108435129B (en) | 2020-09-04 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109158101A (en) * | 2018-10-11 | 2019-01-08 | 南通纺织丝绸产业技术研究院 | A kind of doping niobium, the tantalic acid titanium-based photochemical catalyst of vanadium, preparation method and application |
| CN109399726A (en) * | 2018-11-15 | 2019-03-01 | 沈阳理工大学 | A kind of preparation method of iron lanthanum-oxides molecular sieve type scavenging material |
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| CN103100414A (en) * | 2013-01-31 | 2013-05-15 | 沈阳理工大学 | Molecular sieve with photocatalysis function, and preparation method thereof |
| CN106006660A (en) * | 2016-05-25 | 2016-10-12 | 沈阳理工大学 | Method for preparing samarium titanate molecular sieve |
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| CN103100414A (en) * | 2013-01-31 | 2013-05-15 | 沈阳理工大学 | Molecular sieve with photocatalysis function, and preparation method thereof |
| JP6211499B2 (en) * | 2014-09-29 | 2017-10-11 | 富士フイルム株式会社 | Strontium titanate fine particles, photocatalyst and hydrogen / oxygen generation photocatalyst system |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109158101A (en) * | 2018-10-11 | 2019-01-08 | 南通纺织丝绸产业技术研究院 | A kind of doping niobium, the tantalic acid titanium-based photochemical catalyst of vanadium, preparation method and application |
| CN109158101B (en) * | 2018-10-11 | 2021-09-17 | 南通纺织丝绸产业技术研究院 | Niobium and vanadium doped titanium-based tantalate photocatalyst, preparation method and application |
| CN109399726A (en) * | 2018-11-15 | 2019-03-01 | 沈阳理工大学 | A kind of preparation method of iron lanthanum-oxides molecular sieve type scavenging material |
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