CN104857967B - A kind of acidic oxide MoO3/CuO/TiO2Preparation method - Google Patents
A kind of acidic oxide MoO3/CuO/TiO2Preparation method Download PDFInfo
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Abstract
The invention discloses a kind of acidic oxide MoO3/CuO/TiO2And its preparation method and application, the Kocide SD of preparation is mixed with titanium gel, ammonium molybdate, is calcined, acidic oxide MoO is made3/CuO/TiO2。Raw material is cheap and easy to get, and preparation method is simple, and good catalytic activity and stability are shown in the esterification and ester exchange reaction of acid alcohol, reusable, free from environmental pollution.
Description
Technical field
The invention belongs to catalyst field, and in particular to a kind of acidic oxide MoO3/CuO/TiO2And preparation method thereof and
Using.
Background technology
Carboxylic esterification is the important organic chemical reactionses of a class, and esterification products class is various and is widely used.Most commonly seen
It is to be applied to as solvent, spices, surfactant and plasticizer etc. in different chemical industries.Carboxylic acid is prepared by esterification
Ester is most common production technology, and the wherein use of catalyst has played decisive work on the yield of carboxylate and quality control
With.Traditional carboxylate esterification catalyst is generally mineral matter acid, such as H2SO4, the liquid acid such as HCL, HF and HBr.Although liquid acid is honest and clean
Valency is easy to get, but shortcoming is also apparent from.Especially be particularly easy to generation environment pollution, catalyst can not reclaim, complex operation, corruption
Production equipment etc. is lost, solid catalyst can effectively solve the above problems.At present, studying and liquid is substituted using solid catalyst
The method of body acid catalyst, but apply chemical field solid catalyst seldom, reason is that the acid of solid catalyst contains
The shortcomings of amount relatively low, easy in inactivation.Therefore, the key for improving the catalytic efficiency of esterification is the acid strength for improving catalyst.
The content of the invention
It is an object of the invention to provide a kind of acidic oxide MoO3/CuO/TiO2And its preparation method and application, raw material
Cheap and easy to get, preparation method is simple, good catalytic activity is shown in the esterification and ester exchange reaction of acid alcohol and steady
It is qualitative, it is reusable, it is free from environmental pollution.
To achieve the above object, the present invention is adopted the following technical scheme that：
A kind of acidic oxide MoO3/CuO/TiO2Preparation method comprise the following steps：
1）By 5-10 milliliters of dispersant, the 2.0-3.0 grams of mixing of 40-60 milliliters of deionized water and Gerhardite, room temperature
Lower magnetic agitation 12 hours, obtains solution A；
2）0.7-1.3 grams of sodium hydroxide is dissolved in deionized water, solution B is obtained；
3）Solution B is added dropwise in solution A, is stirred at room temperature 12 hours；
4）Centrifugation, precipitation deionized water supersound washing 2 times, then washed 2 times with absolute ethyl alcohol, 80 DEG C of vacuum drying 12 are small
When, grinding obtains Kocide SD powder；
5）By 1 gram of Kocide SD, the 0.2 gram of mixing of 1 gram of titanium gel and ammonium molybdate, grind 3 minutes, 600 DEG C are calcined 2 hours,
Grinding 10 minutes, obtains acidic oxide MoO3/CuO/TiO2。
Described dispersant is one or both of ethylene glycol, glycerine.
Described acidic oxide MoO3/CuO/TiO2Esterification and ester exchange reaction applied to acid alcohol.
The remarkable advantage of the present invention is：Raw material is cheap and easy to get, and preparation method is simple, is handed in the esterification and ester of acid alcohol
Change in reaction and show good catalytic activity and stability, it is reusable, it is free from environmental pollution.
Embodiment
Embodiment 1
A kind of acidic oxide MoO3/CuO/TiO2Preparation method comprise the following steps：
1）2.0 grams of 5 milliliters of dispersant, 40 milliliters of deionized water and Gerhardite are mixed, at room temperature magnetic agitation
12 hours, obtain solution A；
2）0.7 gram of sodium hydroxide is dissolved in deionized water, solution B is obtained；
3）Solution B is added dropwise in solution A, is stirred at room temperature 12 hours；
4）Centrifugation, precipitation deionized water supersound washing 2 times, then washed 2 times with absolute ethyl alcohol, 80 DEG C of vacuum drying 12 are small
When, grinding obtains Kocide SD powder；
5）By 1 gram of Kocide SD, the 0.2 gram of mixing of 1 gram of titanium gel and ammonium molybdate, grind 3 minutes, 600 DEG C are calcined 2 hours,
Grinding 10 minutes, obtains acidic oxide MoO3/CuO/TiO2。
Described dispersant is ethylene glycol.
Embodiment 2
A kind of acidic oxide MoO3/CuO/TiO2Preparation method comprise the following steps：
1）3.0 grams of 10 milliliters of dispersant, 60 milliliters of deionized water and Gerhardite are mixed, at room temperature magnetic agitation
12 hours, obtain solution A；
2）1.3 grams of sodium hydroxides are dissolved in deionized water, solution B is obtained；
3）Solution B is added dropwise in solution A, is stirred at room temperature 12 hours；
4）Centrifugation, precipitation deionized water supersound washing 2 times, then washed 2 times with absolute ethyl alcohol, 80 DEG C of vacuum drying 12 are small
When, grinding obtains Kocide SD powder；
5）By 1 gram of Kocide SD, the 0.2 gram of mixing of 1 gram of titanium gel and ammonium molybdate, grind 3 minutes, 600 DEG C are calcined 2 hours,
Grinding 10 minutes, obtains acidic oxide MoO3/CuO/TiO2。
Described dispersant is glycerine.
Embodiment 3
A kind of acidic oxide MoO3/CuO/TiO2Preparation method comprise the following steps：
1）2.5 grams of 8 milliliters of dispersant, 50 milliliters of deionized water and Gerhardite are mixed, at room temperature magnetic agitation
12 hours, obtain solution A；
2）1.0 grams of sodium hydroxides are dissolved in deionized water, solution B is obtained；
3）Solution B is added dropwise in solution A, is stirred at room temperature 12 hours；
4）Centrifugation, precipitation deionized water supersound washing 2 times, then washed 2 times with absolute ethyl alcohol, 80 DEG C of vacuum drying 12 are small
When, grinding obtains Kocide SD powder；
5）By 1 gram of Kocide SD, the 0.2 gram of mixing of 1 gram of titanium gel and ammonium molybdate, grind 3 minutes, 600 DEG C are calcined 2 hours,
Grinding 10 minutes, obtains acidic oxide MoO3/CuO/TiO2。
Described dispersant is that volume ratio is 1:1 ethylene glycol and the mixed liquor of glycerine.
Application examples 1
By taking the esterification of ethanol and acetic acid as an example, ethanol and acetic acid, its mol ratio are added in 150mL three-neck flask
For 3:1, catalyst（Acidic oxide MoO made from embodiment 13/CuO/TiO2）Consumption is the 1% of reactant gross mass, with band
The electric jacket of magnetic agitation heats flask to 80 DEG C, and magnetic agitation is reacted after 3h, and conversion ratio is reused 5 times up to 60%, catalysis
Effect is without being decreased obviously.
Application examples 2
By taking the esterification of ethanol and acetic acid as an example, ethanol and acetic acid, its mol ratio are added in 150mL three-neck flask
For 3:1, catalyst（Acidic oxide MoO made from embodiment 23/CuO/TiO2）Consumption is the 5% of reactant gross mass, with band
The electric jacket of magnetic agitation heats flask to 95 DEG C, and magnetic agitation is reacted after 6h, and conversion ratio is reused 5 times up to 90%, catalysis
Effect is without being decreased obviously.
Application examples 3
By taking the esterification of ethanol and acetic acid as an example, ethanol and acetic acid, its mol ratio are added in 150mL three-neck flask
For 3:1, catalyst（Acidic oxide MoO made from embodiment 33/CuO/TiO2）Consumption is the 3% of reactant gross mass, with band
The electric jacket of magnetic agitation heats flask to 90 DEG C, and magnetic agitation is reacted after 4h, and conversion ratio is reused 5 times up to 80%, catalysis
Effect is without being decreased obviously.
The foregoing is only presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, should all belong to the covering scope of the present invention.
Claims (2)
1. a kind of acidic oxide MoO3/CuO/TiO2Application, it is characterised in that：Described acidic oxide MoO3/CuO/
TiO2Esterification applied to acid alcohol；The acidic oxide MoO3/CuO/TiO2Preparation method comprise the following steps：
1）2.0-3.0 grams of 5-10 milliliters of dispersant, 40-60 milliliters of deionized water and Gerhardite are mixed, at room temperature magnetic
Power is stirred 12 hours, obtains solution A；
2）0.7-1.3 grams of sodium hydroxide is dissolved in deionized water, solution B is obtained；
3）Solution B is added dropwise in solution A, is stirred at room temperature 12 hours；
4）Centrifugation, precipitation deionized water supersound washing 2 times, then washed 2 times with absolute ethyl alcohol, 80 DEG C are dried in vacuo 12 hours,
Grinding, obtains Kocide SD powder；
5）By 1 gram of Kocide SD, the 0.2 gram of mixing of 1 gram of titanium gel and ammonium molybdate, grind 3 minutes, 600 DEG C are calcined 2 hours, grinding
10 minutes, obtain acidic oxide MoO3/CuO/TiO2。
2. acidic oxide MoO according to claim 13/CuO/TiO2Application, it is characterised in that：In the preparation side
In method, described dispersant is one or both of ethylene glycol, glycerine.
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| CN101703940A (en) * | 2009-11-09 | 2010-05-12 | 中国海洋石油总公司 | Method for preparing solid acid catalyst of esterification |
| CN102580758A (en) * | 2012-03-24 | 2012-07-18 | 中国石油化工股份有限公司 | NiO-MoO3/ TiO2 catalyst and preparation method thereof |
| CN102826617A (en) * | 2012-09-21 | 2012-12-19 | 中国科学院过程工程研究所 | Spherical nickel hydroxide material and preparation method thereof |
| CN103691463A (en) * | 2013-12-17 | 2014-04-02 | 中国科学院长春应用化学研究所 | Solid acid catalyst and preparation method thereof, and preparation method of diolefin compounds |
| CN103990449A (en) * | 2014-05-30 | 2014-08-20 | 贵州大学 | Preparation of mesoporous Ti-Mo solid acid catalyst and application of catalyst |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03115249A (en) * | 1989-09-29 | 1991-05-16 | Ube Ind Ltd | Continuous production of organic acid ester |
| CN101905155A (en) * | 2009-06-08 | 2010-12-08 | 常州化学研究所 | Complex metal oxide catalyst for synthesis of diphenyl carbonate by ester exchange reaction and preparation method thereof |
-
2015
- 2015-04-23 CN CN201510194641.XA patent/CN104857967B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101703940A (en) * | 2009-11-09 | 2010-05-12 | 中国海洋石油总公司 | Method for preparing solid acid catalyst of esterification |
| CN102580758A (en) * | 2012-03-24 | 2012-07-18 | 中国石油化工股份有限公司 | NiO-MoO3/ TiO2 catalyst and preparation method thereof |
| CN102826617A (en) * | 2012-09-21 | 2012-12-19 | 中国科学院过程工程研究所 | Spherical nickel hydroxide material and preparation method thereof |
| CN103691463A (en) * | 2013-12-17 | 2014-04-02 | 中国科学院长春应用化学研究所 | Solid acid catalyst and preparation method thereof, and preparation method of diolefin compounds |
| CN103990449A (en) * | 2014-05-30 | 2014-08-20 | 贵州大学 | Preparation of mesoporous Ti-Mo solid acid catalyst and application of catalyst |
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