CN102698705A - Preparation method for nano titanium dioxide coated nano silicon dioxide - Google Patents
Preparation method for nano titanium dioxide coated nano silicon dioxide Download PDFInfo
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- CN102698705A CN102698705A CN2012101807625A CN201210180762A CN102698705A CN 102698705 A CN102698705 A CN 102698705A CN 2012101807625 A CN2012101807625 A CN 2012101807625A CN 201210180762 A CN201210180762 A CN 201210180762A CN 102698705 A CN102698705 A CN 102698705A
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Abstract
The invention relates to a preparation method for a coating material, in particular to a preparation method for nano titanium dioxide coated nano silicon dioxide, and aims to solve the problem that the present nano titanium dioxide coated nano silicon dioxide is complicated in preparation technology and is non-uniform in coating. The preparation method comprises the steps as follows: uniformly dispersing nano silicon dioxide in a mixed solution of deionized water and alcohol through a high-speed dispersion machine; adding tetrabutyl titanate; placing in a reaction still; inflating carbon dioxide gas to a certain pressure and then sealing; placing the reaction still in a high-temperature salt bath and keeping the temperature and the pressure constant; and after a period of time, slowly deflating to a normal pressure and cooling to an ordinary temperature, so as to obtain the nano titanium dioxide coated nano silicon dioxide. The prepared nano titanium dioxide coated nano silicon dioxide is mainly applicable to ink absorbing layer material for inkjet printing as well as to sewage disposal.
Description
Technical field
The present invention relates to a kind of preparation method of clad material.
Background technology
Along with the continuous development of nanometer technology, high-quality, high performance nano material are required increasingly high, wherein nano silicon has advantages such as particle size is little, micropore is many, specific area is big and is widely used in fields such as building, printing.Nano titanium oxide uses also very extensive owing to have unique anti-uv-ray.But because the cost of titanium dioxide is higher and utilization rate is lower, therefore utilize big specific area of nano silicon and aperture, degraded of nano titanium oxide ultraviolet light and absorption property with two kinds of material preparation clad materials, have great importance.The nano silicon dioxide coated by nano titanium dioxide material of preparation possesses the performance of two kinds of materials, and the clad material of preparation is mainly used in fields such as absorption and light degradation, like sewage disposal and environmental protection etc.Application number is 200910063398.2 Chinese patent, discloses a kind of preparation method of nano silicon dioxide coated by nano titanium dioxide, and this method is at first under stirring and hyperacoustic condition; Dropping inorganic acid in silicate solutions, obtains white silica sol at pH, reaction temperature, the time of control reaction system; Drying obtains silicic acid gel, again with silicic acid gel mix with water, ball milling, washing, filtration obtain gel; With the silicic acid gel thermal decomposition, obtain the nano-silica powder end; Secondly under ultrasonic wave effect and stirring condition, the nano-silica powder end is mixed with the mixed solution of glacial acetic acid with water, absolute ethyl alcohol; The 3rd under ultrasonic wave effect and stirring, uniform temperature, and butyl titanate and absolute ethyl alcohol mixed liquor are joined in the mixture, leaves standstill, dry, ball milling, obtains the metatitanic acid gel and coats SiO 2 powder, and heating and decomposition obtains composite powder.This method prepares and adds multiple auxiliary agent in the process, complex operation, and covered effect is poor.
Summary of the invention
The present invention be add for solving existing nano silicon dioxide coated by nano titanium dioxide preparation method that auxiliary agent is many, the technical problem of complex operation, covered effect difference, and a kind of preparation method of nano silicon dioxide coated by nano titanium dioxide is provided.
The preparation method of a kind of nano silicon dioxide coated by nano titanium dioxide of the present invention, carry out according to the following steps:
One, be 1: 0.5～1 to take by weighing nano silicon and butyl titanate by the mass ratio of nano silicon and butyl titanate;
Two, be that nano silicon that 1g: 8mL～15mL takes by weighing step 1 joins and obtains mixed liquor in the mixed solvent by the ratio of nano silicon quality and mixed solvent volume; Again mixed liquor is utilized high speed dispersor; At rotating speed is under the condition of 3000r/min～5000r/min; Disperse 10min～40min, obtain dispersion liquid;
Three, the butyl titanate that step 1 is taken by weighing joins in the dispersion liquid of step 2 preparation, transfers in the agitated reactor after mixing, and in agitated reactor, fills CO
2Gas to still internal pressure seals during for 5MPa-7MPa, and then agitated reactor being placed temperature is 350 ℃～450 ℃ salt bath, in the still internal pressure is to keep 40min～60min under the condition of 7MPa～10MPa; Then the still internal pressure is depressurized to normal pressure, whole step-down process continues 10min, takes out agitated reactor then, is cooled to room temperature;
Four, with the product in the agitated reactor after filtration, washing and drying, obtain nano silicon dioxide coated by nano titanium dioxide.
Effect of the present invention:
Compared with prior art, the present invention has only used ethanol and deionized water when the preparation clad material, do not use other chemical reagent, and the preparation process uses chemical reagent few, preparation method's environmental protection.The nano silicon dioxide coated by nano titanium dioxide of the present invention's preparation; Particle diameter is that the silica of nanometer is reunited in processing procedure in the preparation process; And the titanium dioxide of nanometer is coated on the silica particles of reunion equably, coats evenly, and covered effect is good.The preparation process does not need the pH value of regulation system, does not need ultrasonicly, and technology is simple, is convenient to operation.
The nano silicon dioxide coated by nano titanium dioxide of the present invention's preparation is mainly used in sewage disposal and inkjet printing is used ink-absorption layer material.
Description of drawings
Fig. 1 amplifies 100000 times electron scanning electromicroscopic photograph for the nano silicon dioxide coated by nano titanium dioxide of test one preparation; Fig. 2 amplifies 100000 times electron scanning electromicroscopic photograph for the nano silicon dioxide coated by nano titanium dioxide of experiment two preparations.
The specific embodiment
The specific embodiment one: the preparation method of a kind of nano silicon dioxide coated by nano titanium dioxide of this embodiment, carry out according to the following steps:
One, be 1: 0.5～1 to take by weighing nano silicon and butyl titanate by the mass ratio of nano silicon and butyl titanate;
Two, be that nano silicon that 1g: 8mL～15mL takes by weighing step 1 joins and obtains mixed liquor in the mixed solvent by the ratio of nano silicon quality and mixed solvent volume; Again mixed liquor is utilized high speed dispersor; At rotating speed is under the condition of 3000r/min～5000r/min; Disperse 10min～40min, obtain dispersion liquid;
Three, the butyl titanate that step 1 is taken by weighing joins in the dispersion liquid of step 2 preparation; Transfer in the agitated reactor after mixing; Seal when in agitated reactor, filling CO2 gas to still internal pressure and be 5MPa～7MPa; Then agitated reactor being placed temperature is 350 ℃～450 ℃ salt bath, in the still internal pressure is to keep 40min～60min under the condition of 7MPa～10MPa; Then the still internal pressure is depressurized to normal pressure, whole step-down process continues 10min, takes out agitated reactor then, is cooled to room temperature;
Four, with the product in the agitated reactor after filtration, washing and drying, obtain nano silicon dioxide coated by nano titanium dioxide.
Compared with prior art, this embodiment has only used ethanol and deionized water when the preparation clad material, do not use other chemical reagent, preparation method's environmental protection.The nano silicon dioxide coated by nano titanium dioxide of preparation coats evenly, and covered effect is good.Preparation technology of the present invention is simple, is convenient to operation.
The specific embodiment two: this embodiment and the specific embodiment one are different is that the mass ratio of nano silicon and butyl titanate is 1 in the step 1: (0.6～0.8), other is identical with the specific embodiment one.
The specific embodiment three: this embodiment is different with the specific embodiment one or two is that mixed solvent in the step 2 is the mixture of deionized water and ethanol; Wherein the volume ratio of deionized water and ethanol is 2～5: 1, and other is identical with the specific embodiment one or two.
The specific embodiment four: this embodiment is different with one of specific embodiment one to three is that the ratio of nano silicon quality and mixed solvent volume in the step 2 is 1g: 9mL～12mL, and other is identical with one of specific embodiment one to three.
The specific embodiment five: this embodiment is different with one of specific embodiment one to four is that the rotating speed of step 2 high speed dispersion machine is 3500r/min～4500r/min.Other is identical with one of specific embodiment one to four.
The specific embodiment six: what this embodiment was different with one of specific embodiment one to five is that the time that step 2 high speed dispersion machine disperses is 20min～30min.Other is identical with one of specific embodiment one to five.
The specific embodiment seven: this embodiment is different with one of specific embodiment one to six is that to fill CO2 pressure to the agitated reactor in the step 3 be 5MPa～6MPa, and other is identical with one of specific embodiment one to six.
The specific embodiment eight: this embodiment is different with one of specific embodiment one to seven is that the temperature of salt bath in the step 3 is 370 ℃～420 ℃, and other is identical with one of specific embodiment one to seven.
The specific embodiment nine: this embodiment is different with one of specific embodiment one to eight be in the step 3 during pressurize pressure in the agitated reactor be 7MPa～9MPa, other is identical with the specific embodiment one to eight.
The specific embodiment ten: this embodiment is different with one of specific embodiment one to nine be in the step 3 dwell time be 40min～50min, other is identical with the specific embodiment one to nine.
Adopt following verification experimental verification beneficial effect of the present invention:
Test one: the preparation method of a kind of nano silicon dioxide coated by nano titanium dioxide of this test, specifically accomplish according to the following steps:
One, takes by weighing 3g nano silicon and 3g butyl titanate;
Two, the nano silicon that step 1 is taken by weighing joins in the mixed solvent that is mixed by 10mL deionized water and 30mL ethanol and obtains mixed liquor; Again mixed liquor is utilized high speed dispersor; At rotating speed is under the condition of 4000r/min, disperses 30min, obtains dispersion liquid;
Three, the butyl titanate that step 1 is taken by weighing joins in the dispersion liquid of step 2 preparation; Transfer in the agitated reactor after mixing; Seal when in agitated reactor, filling CO2 gas to still internal pressure for 6MPa; Then agitated reactor being placed temperature is 350 ℃ salt bath, in the still internal pressure is to keep 60min under the condition of 7MPa; Then the still internal pressure is depressurized to normal pressure, whole step-down process continues 10min, takes out agitated reactor then, is cooled to room temperature;
Four, with the product in the agitated reactor after filtration, washing and drying, obtain nano silicon dioxide coated by nano titanium dioxide.
The ESEM picture of the nano silicon dioxide coated by nano titanium dioxide of test one preparation is as shown in Figure 1.
Test two: test two is contrast tests of experiment one, and this test is a prior art for preparing nano silicon dioxide coated by nano titanium dioxide method, specifically accomplishes according to the following steps:
One, take by weighing 3g butyl titanate and 30g absolute ethyl alcohol mix the back subsequent use with the dropping funel splendid attire, be labeled as solution 1.
Two, take by weighing 3g nano silicon and 10ml deionized water, use high speed dispersor under the condition of rotating speed as 4500r/min, to disperse 30min, using the pH of the acetate hierarchy of control simultaneously is 2～3, is labeled as solution 2.
Three, solution 1 slowly is added drop-wise in the solution 2, the control dropping time is 30min, promptly makes colloidal sol.
Four, the colloidal sol that makes in the step 3 is transferred in the agitated reactor, sealed when in agitated reactor, filling CO2 gas to still internal pressure for 7MPa, then agitated reactor being placed temperature is 350 ℃ salt bath, in the still internal pressure is to keep 50min under the condition of 8MPa; Then the still internal pressure is depressurized to normal pressure, whole step-down process continues 10min, takes out agitated reactor then, is cooled to room temperature;
Five, with the product in the agitated reactor after filtration, washing and drying, obtain nano silicon dioxide coated by nano titanium dioxide.
The ESEM picture of the nano silicon dioxide coated by nano titanium dioxide of test two preparations is as shown in Figure 2.
Test one can draw with test two contrasts:
One, only used deionized water and ethanol in the test one preparation process, used acetate in the test two, got ionized water and ethanol, the chemical reagent that uses in the experiment one is few.
Two, need the pH with the acetate regulation system in test two the preparation process, and complicated steps, it is simple to test one preparation method by contrast.
Three, can find out clearly among Fig. 1; Coating at nano-silica surface villous shape is evenly distributed, and the nano silicon dioxide coated by nano titanium dioxide of preparation in the test one is described; Nano titanium oxide is coated on nano-silica surface uniformly, and covered effect is good; Can see the random dough of nano titanium oxide and nano silicon among Fig. 2, the nano silicon dioxide coated by nano titanium dioxide of preparation in the test two is described, agglomeration has taken place in titanium dioxide and nano silicon, and covered effect is bad.
Claims (9)
1. the preparation method of a nano silicon dioxide coated by nano titanium dioxide is characterized in that the preparation method of nano silicon dioxide coated by nano titanium dioxide carries out according to the following steps:
One, be 1: 0.5～1 to take by weighing nano silicon and butyl titanate by the mass ratio of nano silicon and butyl titanate;
Two, be that nano silicon that 1g: 8～15mL takes by weighing step 1 joins and obtains mixed liquor in the mixed solvent by the ratio of nano silicon quality and mixed solvent volume; Again mixed liquor is utilized high speed dispersor; At rotating speed is under the condition of 3000r/min～5000r/min; Disperse 10min～40min, obtain dispersion liquid;
Three, the butyl titanate that step 1 is taken by weighing joins in the dispersion liquid of step 2 preparation; Transfer in the agitated reactor after mixing; Seal when in agitated reactor, filling CO2 gas to still internal pressure for 5MPa-7MPa; Then agitated reactor being placed temperature is 350 ℃～450 ℃ salt bath, in the still internal pressure is to keep 40min～60min under the condition of 7MPa～10MPa; Then the still internal pressure is depressurized to normal pressure, whole step-down process continues 10min, takes out agitated reactor then, is cooled to room temperature;
Four, with the product in the agitated reactor after filtration, washing and drying, obtain nano silicon dioxide coated by nano titanium dioxide.
2. the preparation method of a kind of nano silicon dioxide coated by nano titanium dioxide according to claim 1 is characterized in that the mass ratio of nano silicon and butyl titanate is 1: 0.6～0.8 in the step 1.
3. the preparation method of a kind of nano silicon dioxide coated by nano titanium dioxide according to claim 1 and 2 is characterized in that mixed solvent is the mixed liquor of deionized water and ethanol in the step 2, and wherein the volume ratio of deionized water and ethanol is 2～5: 1.
4. the preparation method of a kind of nano silicon dioxide coated by nano titanium dioxide according to claim 3 is characterized in that the ratio of nano silicon quality and mixed solvent volume is 1g: 9mL～12mL in the step 2.
5. the preparation method of a kind of nano silicon dioxide coated by nano titanium dioxide according to claim 4, the rotating speed that it is characterized in that step 2 high speed dispersion machine is 3500r/min～4500r/min.
6. the preparation method of a kind of nano silicon dioxide coated by nano titanium dioxide according to claim 5 is characterized in that the time that step 2 high speed dispersion machine disperses is 20min～30min.
7. the preparation method of a kind of nano silicon dioxide coated by nano titanium dioxide according to claim 6, it is characterized in that filling in the step 3 CO2 pressure to the agitated reactor is 5MPa～6MPa.
8. the preparation method of a kind of nano silicon dioxide coated by nano titanium dioxide according to claim 7, the temperature that it is characterized in that salt bath in the step 3 is 370 ℃～420 ℃.
9. the preparation method of a kind of nano silicon dioxide coated by nano titanium dioxide according to claim 8, the pressure when it is characterized in that pressurize in the step 3 in the agitated reactor is 7MPa～9MPa.
The preparation method of 10 a kind of nano silicon dioxide coated by nano titanium dioxide according to claim 9 is characterized in that the dwell time is 40min～50min in the step 3.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104057082A (en) * | 2014-06-18 | 2014-09-24 | 南京理工大学 | Preparing method of TiO2 (titanium dioxide) coated nanometer nickel powder |
| CN105860945A (en) * | 2016-05-04 | 2016-08-17 | 无锡市嘉邦电力管道厂 | Thixotropic chemical channeling sealing agent |
| CN107572537A (en) * | 2017-09-27 | 2018-01-12 | 东莞市联洲知识产权运营管理有限公司 | A kind of nano-titanium oxide coats the preparation method of nano oxidized silicon carrier |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101613537A (en) * | 2009-07-31 | 2009-12-30 | 孝感学院 | A kind of preparation method of nano silicon dioxide coated by nano titanium dioxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101613537A (en) * | 2009-07-31 | 2009-12-30 | 孝感学院 | A kind of preparation method of nano silicon dioxide coated by nano titanium dioxide |
Non-Patent Citations (1)
| Title |
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| 殷婷婷等: "水热法制备纳米二氧化钛的研究进展", 《广州化工》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104057082A (en) * | 2014-06-18 | 2014-09-24 | 南京理工大学 | Preparing method of TiO2 (titanium dioxide) coated nanometer nickel powder |
| CN105860945A (en) * | 2016-05-04 | 2016-08-17 | 无锡市嘉邦电力管道厂 | Thixotropic chemical channeling sealing agent |
| CN105860945B (en) * | 2016-05-04 | 2019-03-08 | 无锡市嘉邦电力管道厂 | Thixotropic chemical sealing channeling agent |
| CN107572537A (en) * | 2017-09-27 | 2018-01-12 | 东莞市联洲知识产权运营管理有限公司 | A kind of nano-titanium oxide coats the preparation method of nano oxidized silicon carrier |
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Application publication date: 20121003 |