CN107308964A - A kind of preparation method of galapectite load indium phosphate catalyst - Google Patents
A kind of preparation method of galapectite load indium phosphate catalyst Download PDFInfo
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- CN107308964A CN107308964A CN201710561912.XA CN201710561912A CN107308964A CN 107308964 A CN107308964 A CN 107308964A CN 201710561912 A CN201710561912 A CN 201710561912A CN 107308964 A CN107308964 A CN 107308964A
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- Prior art keywords
- galapectite
- preparation
- indium phosphate
- load
- phosphate catalyst
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/16—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr
- B01J27/18—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr with metals other than Al or Zr
- B01J27/1802—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates
- B01J27/1811—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates with gallium, indium or thallium
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/16—Clays or other mineral silicates
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
Abstract
The present invention discloses a kind of preparation method of galapectite load indium phosphate catalyst, comprises the following steps：Galapectite is subjected to acidification, galapectite aluminium oxide structure is dissolved, is conducive to load；Galapectite after processing is added in indiumchloride solution, then ammonium phosphate solution is added dropwise thereto, so as to form colloid covering on galapectite surface, finally centrifuges, washing and drying, that is, obtains galapectite load indium phosphate catalyst.The present invention is by using the suction-operated between the rough surface and indium phosphate colloidal solid of galapectite, in galapectite area load phosphoric acid indium nanometer particle, promotes catalyst to fix.
Description
Technical field
It is catalyzed the present invention relates to novel environmental pollution control material technical field, more particularly to a kind of galapectite load indium phosphate
The preparation method of agent.
Background technology
With the development of science and technology, the murder by poisoning organic pollution produced in industrial and agricultural production seriously threatens environment and people
The health of class, seeks a kind of new and effective environmental improvement technology and has great importance.Photocatalysis technology is because of its energy-conservation, height
Effect, contaminant degradation are thorough, non-secondary pollution advantage, turn into a kind of emerging environmental improvement with important application prospect at present
Technology.In recent years, the development of new and effective visible-light photocatalyst turns into an important research content in photocatalysis technology,
Wherein there is the catalysis material of surface plasma resonance effect, because of its unique Surface Physical Chemistry property and efficient visible
One of light photocatalysis performance, focus as research.But nanoparticles are easily reunited, surface area is greatly reduced after reunion, effect
Fruit weakens.
Indium phosphate is also due to have open duct microcellular structure, therefore attracted the notice of people, traditional method is to use
The method of hydro-thermal, solvent heat and ion thermal synthesis, selection is with the organic molecule and metal combination for forming containing Microporous Compounds potential
Thing can have as structure directing agent as the indium (III) in Louis acid catalysis activated centre as metal center to synthesize
The phosphate containing Microporous Compounds of open-framework.But research never finds the photocatalytic activity of indium phosphate in itself.
Galapectite is again by title halloysite.Chemical composition is identical with kaolinite, the SiO with identical 1: 12/Al2O3
Than lamellar structure has been curled into SiO2In outer layer, Al2O3In internal layer, therefore angstrom trachelospermum jasminoide nanotube is with closely similar with SiO2
Surface nature, and Al2O3Similar internal layer property.In general halloysite nanotubes are formed by the curling of multiple kaolin lamellas, are
Natural many wall-shaped nanotubes, pipe external diameter is 20-100nm, and internal diameter is 5-30nm, and length is 150nm-2 μm.Galapectite and kaolinite
The main distinction of the soil on crystal structure, one is tubular structure, and one is sheet structure.Halloysite nanotubes, by kaolinic
Layer is crimped under natural endowment to be formed, in micro-tube shaped structure.
The content of the invention
The purpose of the present invention is that there is provided a kind of system of galapectite load indium phosphate catalyst to overcome the deficiencies in the prior art
Preparation Method.
In order to solve the above technical problems, the present invention uses following technical scheme：
A kind of preparation method of galapectite load indium phosphate catalyst, comprises the following steps：
(1) galapectite that purity is not less than 85wt% is added in 1~5wt% salpeter solution, under normal temperature stir 5~
8h, centrifugal dehydration and drying, obtain the galapectite of acid treatment；Galapectite aluminium oxide structure is dissolved after processing, rough surface,
Beneficial to load；
(2) galapectite after step (1) processing is added in the indiumchloride solution that volume is 25~40mL, then side is stirred
Mix side and ammonium phosphate solution is added dropwise, continue to stir 50~60min after being added dropwise to complete, when galapectite surface forms colloid covering, from
The heart is separated, and with water washing solid is distilled 3~4 times, is dried at 103~105 DEG C, that is, the catalysis of galapectite load indium phosphate is made
Agent.
Preferably, galapectite is 1: 10~20 by weight with salpeter solution in step (1).
Preferably, inidum chloride concentration is 0.1~0.4mol/L in step (2).
Preferably, phosphoric acid ammonium concentration is 0.1~0.4mol/L in step (2).
Preferably, the addition of ammonium phosphate is 25~40mL in step (2).
Preferably, the speed of agitator in step (2) is 300~400r/s.
The invention has the advantages that：(1) by acidizing pretreatment, galapectite surface roughness can be increased, had
Beneficial to load；(2) it is negative on galapectite surface using the suction-operated between the rough surface and indium phosphate colloidal solid of galapectite
Phosphoric acid indium nanometer particle is carried, promotes catalyst to fix.
Embodiment
Embodiment 1
The galapectite that purity is not less than 85wt% is added in 5wt% salpeter solution, the galapectite of reaction system with
Salpeter solution is added by weight for 1: 10, and 8h, centrifugal dehydration and drying are then stirred under normal temperature, angstrom of acid treatment is obtained
Lip river stone；Then the galapectite after processing is added to concentration for 0.4mol/L, in volume 40mL indiumchloride solution, Ran Hou
It is 0.4mol/L that concentration is added dropwise under 400r/s rotating speed thereto while stirring, and volume 40mL ammonium phosphate solution is added dropwise to complete
Continue to stir 60min with 400r/s rotating speed afterwards, when colloid covering is formed on galapectite surface, centrifuge, washed with distillation
Wash solid 4 times, dried at 105 DEG C, that is, galapectite load indium phosphate catalyst is made.
Application test 1
Obtained galapectite load indium phosphate catalyst is used to handle wastewater containing methylene blue：0.5g galapectites are weighed to bear
Carry indium phosphate catalyst and be added to concentration for 40mg/L, in volume 300mL methylene blue waste water, irradiated in 120W LED
Under, after reaction 35min, percent of decolourization is 97.4%；After the catalyst is separated, experiment is reused multiple；6th time,
Also under the same conditions, 35min is reacted, percent of decolourization is 91.4%.The 0.5g indium phosphate particles of phase homogenous quantities are weighed, in identical
Under the conditions of be used to handle wastewater containing methylene blue, after reaction 35min, percent of decolourization is 90.2%, and two kinds of catalyst are contrasted,
It was found that the amount of indium is relatively much greater contained by pure phosphoric acid indium particle, the present embodiment is more economical preferential, and effect is more preferable.
Embodiment 2
The galapectite that purity is not less than 85wt% is added in 1wt% salpeter solution, the galapectite of reaction system with
Salpeter solution is added by weight for 1: 20, and 5h, centrifugal dehydration and drying are then stirred under normal temperature, angstrom of acid treatment is obtained
Lip river stone；Then the galapectite after processing is added to concentration for 0.1mol/L, in volume 25mL indiumchloride solution, Ran Hou
It is 0.1mol/L that concentration is added dropwise under 300r/s rotating speed thereto while stirring, and volume 25mL ammonium phosphate solution is added dropwise to complete
Continue to stir 50min with 300r/s rotating speed afterwards, when colloid covering is formed on galapectite surface, centrifuge, washed with distillation
Wash solid 3 times, dried at 103 DEG C, that is, galapectite load indium phosphate catalyst is made.
Application test 2
Obtained galapectite load indium phosphate catalyst is used to handle waste water containing acid scarlet：0.5g galapectites are weighed to bear
Carry indium phosphate catalyst and be added to concentration for 40mg/L, in volume 300mL acid scarlet waste water, irradiated in 120W LED
Under, 35min is reacted, percent of decolourization is 95.9%；After the catalyst is separated, experiment is reused multiple；6th time, also
Under the same conditions, 35min is reacted, percent of decolourization is 92.0%.The 0.5g indium phosphate particles of phase homogenous quantities are weighed, in identical bar
It is used to handle after waste water containing acid scarlet, reaction 35min under part, percent of decolourization is 90.1%, and two kinds of catalyst are contrasted, hair
The amount of indium is relatively much greater contained by existing pure phosphoric acid indium particle, and the present embodiment is more economical preferential, and effect is more preferable.
Embodiment 3
The galapectite that purity is not less than 85wt% is added in 1wt% salpeter solution, the galapectite of reaction system with
Salpeter solution is added by weight for 1: 15, and 7h, centrifugal dehydration and drying are then stirred under normal temperature, angstrom of acid treatment is obtained
Lip river stone；Then the galapectite after processing is added to concentration for 0.3mol/L, in volume 30mL indiumchloride solution, Ran Hou
It is 0.25mol/L that concentration is added dropwise under 350r/s rotating speed thereto while stirring, and volume 33mL ammonium phosphate solution is added dropwise to complete
Continue to stir 55min with 350r/s rotating speed afterwards, when colloid covering is formed on galapectite surface, centrifuge, washed with distillation
Wash solid 4 times, dried at 104 DEG C, that is, galapectite load indium phosphate catalyst is made.
Application test 3
Obtained galapectite load indium phosphate catalyst is used to handle waste water containing acid scarlet：0.5g galapectites are weighed to bear
Carry indium phosphate catalyst and be added to concentration for 40mg/L, in volume 300mL acid scarlet waste water, irradiated in 120W LED
Under, 30min is reacted, percent of decolourization is 97.3%；After the catalyst is separated, experiment is reused multiple；6th time, also
Under the same conditions, 30min is reacted, percent of decolourization is 95.2%.The 0.5g indium phosphate particles of phase homogenous quantities are weighed, in identical bar
It is used to handle after waste water containing acid scarlet, reaction 30min under part, percent of decolourization is 91.5%, and two kinds of catalyst are contrasted, hair
The amount of indium is relatively much greater contained by existing pure phosphoric acid indium particle, and the present embodiment is more economical preferential, and effect is more preferable.
Claims (6)
1. a kind of preparation method of galapectite load indium phosphate catalyst, it is characterised in that comprise the following steps：
(1) galapectite that purity is not less than 85wt% is added in 1~5wt% salpeter solution, 5~8h is stirred under normal temperature,
Centrifugal dehydration and drying, obtain the galapectite of acid treatment；Galapectite aluminium oxide structure is dissolved after processing, rough surface, profit
In load；
(2) galapectite after step (1) processing is added in the indiumchloride solution that volume is 25~40mL, then while stirring
Ammonium phosphate solution is added dropwise, continues to stir 50~60min after being added dropwise to complete, when galapectite surface forms colloid covering, centrifugation point
From with water washing solid is distilled 3~4 times, the drying at 103~105 DEG C is made galapectite load indium phosphate catalyst.
2. the preparation method of galapectite load indium phosphate catalyst according to claim 1, it is characterised in that the step
(1) galapectite is 1: 10~20 by weight with salpeter solution in.
3. the preparation method of galapectite load indium phosphate catalyst according to claim 1, it is characterised in that the step
(2) inidum chloride concentration is 0.1~0.4mol/L in.
4. the preparation method of galapectite load indium phosphate catalyst according to claim 1, it is characterised in that the step
(2) phosphoric acid ammonium concentration is 0.1~0.4mol/L in.
5. the preparation method of galapectite load indium phosphate catalyst according to claim 1, it is characterised in that the step
(2) addition of ammonium phosphate is 25~40mL in.
6. the preparation method of galapectite load indium phosphate catalyst according to claim 1, it is characterised in that the step
(2) speed of agitator in is 300~400r/s.
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| CN201710561912.XA CN107308964A (en) | 2017-07-11 | 2017-07-11 | A kind of preparation method of galapectite load indium phosphate catalyst |
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| CN201710561912.XA CN107308964A (en) | 2017-07-11 | 2017-07-11 | A kind of preparation method of galapectite load indium phosphate catalyst |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57198681A (en) * | 1981-05-30 | 1982-12-06 | Fujitsu Ltd | Optical semiconductor |
| CN101698474A (en) * | 2009-11-03 | 2010-04-28 | 李伟 | Method for quickly synthesizing indium phosphide semiconductor material |
| CN103301827A (en) * | 2013-06-26 | 2013-09-18 | 常州大学 | Halloysite-based photocatalytic composite material and preparation method of halloysite-based photocatalytic composite material |
| CN103349977A (en) * | 2013-07-19 | 2013-10-16 | 西安建筑科技大学 | Preparation and application of rectorite loading indium oxide photocatalyst |
| CN103934008A (en) * | 2014-04-17 | 2014-07-23 | 常州大学 | Preparation method of halloysite loading phosphoric acid Silverlight catalyst |
| CN106311296A (en) * | 2016-10-19 | 2017-01-11 | 常州大学 | Preparation method of iron phosphate/yttrium phosphate composite catalyst |
-
2017
- 2017-07-11 CN CN201710561912.XA patent/CN107308964A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57198681A (en) * | 1981-05-30 | 1982-12-06 | Fujitsu Ltd | Optical semiconductor |
| CN101698474A (en) * | 2009-11-03 | 2010-04-28 | 李伟 | Method for quickly synthesizing indium phosphide semiconductor material |
| CN103301827A (en) * | 2013-06-26 | 2013-09-18 | 常州大学 | Halloysite-based photocatalytic composite material and preparation method of halloysite-based photocatalytic composite material |
| CN103349977A (en) * | 2013-07-19 | 2013-10-16 | 西安建筑科技大学 | Preparation and application of rectorite loading indium oxide photocatalyst |
| CN103934008A (en) * | 2014-04-17 | 2014-07-23 | 常州大学 | Preparation method of halloysite loading phosphoric acid Silverlight catalyst |
| CN106311296A (en) * | 2016-10-19 | 2017-01-11 | 常州大学 | Preparation method of iron phosphate/yttrium phosphate composite catalyst |
Non-Patent Citations (1)
| Title |
|---|
| 潘红: "用于染料废水处理的InVO4的低温固相合成及InPO4的形貌可控水热合成", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
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Application publication date: 20171103 |
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