CN105289607A - Preparation method of copper based catalyst - Google Patents
Preparation method of copper based catalyst Download PDFInfo
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- CN105289607A CN105289607A CN201510779354.5A CN201510779354A CN105289607A CN 105289607 A CN105289607 A CN 105289607A CN 201510779354 A CN201510779354 A CN 201510779354A CN 105289607 A CN105289607 A CN 105289607A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P30/00—Technologies relating to oil refining and petrochemical industry
- Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P30/00—Technologies relating to oil refining and petrochemical industry
- Y02P30/40—Ethylene production
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation method of a copper based catalyst. The copper based catalyst is obtained via reaction of sodium metasilicate with a copper source in an organic phase environment. Compared with the prior art, in the copper based catalyst, copper used for realizing catalytic action are dispersedly immobilized on a silica gel carrier, so that contact area of copper with a reaction base material is enlarged. Compared with the prior art, the copper based catalyst is higher in catalytic efficiency, needed catalytic conditions are milder, and the copper based catalyst is beneficial for industrial production. And at the same time, preparation of the copper based catalyst is completed under pure organic phase conditions, so that catalytic efficiency of the copper based catalyst is higher than that of catalysts obtained at common water conditions.
Description
Technical field
The invention belongs to catalyst field, be specifically related to a kind of preparation method of Cu-series catalyst.
Background technology
The low-carbon alkene such as ethene, propylene is raw material the most basic in petrochemical industry.For ethene, about there are the petrochemicals of 75% by ethylene production, it is mainly used to produce the multiple important Organic chemical products such as polyethylene, polyvinyl chloride, ethylene oxide/ethylene glycol, dichloroethanes, styrene, polystyrene, ethanol, vinyl acetate, in fact, ethylene yield has become the mark of a measurement national oil chemical engineering industry development level.
Statistics display, from nineteen ninety by 2003, China's ethene equivalent consumption figure increases by 12% every year, after this growth rate is more surprising, within 2003, China's ethene equivalent consumption figure is 1,350 ten thousand tons, within 2005, this numeral just reaches 1,876 ten thousand tons, has increased nearly 40% on foot between 2 years, and Chinese Market for Ethylene has become the country that global growth rate is the fastest, the growth duration is the longest.
In the technique of preparing ethylene, propylene and other functionalized olefin, the effect of catalyst has great impact for the productive rate of product and qualification rate.Cu-series catalyst is a kind of conventional catalyst in industrial production, but comparatively active because of it, and reducing power is comparatively strong, and therefore reaction condition is comparatively harsh.Improving Cu-series catalyst catalytic efficiency in the industrial production, is a current large study hotspot.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of Cu-series catalyst, not high to solve the catalytic efficiency of prior art existence, the problems such as catalytic condition is harsh.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
A preparation method for Cu-series catalyst, it comprises the steps:
(1) sodium metasilicate is dissolved in organic solvent, under the condition of nitrogen protection, in organic solvent, passes into hydrogen chloride gas, at 30 ~ 60 DEG C, react 3 ~ 6h;
(2) keep nitrogen protection condition, in the mixed system of step (1) gained, add copper source, at 40 ~ 45 DEG C, react 1 ~ 3h;
(3) in the mixed system of gained in step (2), add precipitating reagent, fully mix, after colloidal sol is complete, get gel;
(4) by after the gel detergent of gained in step (3), drying, roast, Cu-series catalyst is obtained.
Wherein, described sodium metasilicate is anhydrous sodium metasilicate.
Wherein, in above-mentioned preparation method, in step (1) ~ (3), agents useful for same is all through anhydrous process.
Wherein, in above-mentioned preparation method, in step (1) and (2), reaction is all placed on shaking table to be carried out.
In step (1), described organic solvent is pyridine or methyl-sulfoxide.
In step (1), the weight ratio of sodium metasilicate and organic solvent is 1:50 ~ 200.
In step (1), the mol ratio of sodium metasilicate and hydrogen chloride is 1:1.5 ~ 3.5.
In step (2), described copper source is copper chloride or cupric phosphate.
In step (2), in sodium metasilicate and copper source, the mol ratio of copper is 50 ~ 75:1.
In step (3), described precipitating reagent is polyacrylamide or ferric sulfate; Wherein, the mass ratio of precipitating reagent and sodium metasilicate is 1:600 ~ 750.
In step (4), the method for washing is for using deionized water rinsing 2 ~ 3 times, and dry method is for using sodium sulfite dry, and the method for roast is roasting 1 ~ 1.5h at 600 ~ 700 DEG C.
The Cu-series catalyst that above-mentioned preparation method prepares is also within protection scope of the present invention.
Above-mentioned Cu-series catalyst in the application of catalyst field also within protection scope of the present invention.
Beneficial effect: compared with prior art, the present invention has following advantage:
Cu-series catalyst in the present invention, is fixed on silica-gel carrier by the copper dispersion playing catalytic action, expands itself and the contact area of reacting bed material.Compared with prior art, the catalytic efficiency of this Cu-series catalyst is higher, and required catalytic condition milder, is conducive to industrial production.Meanwhile, the inventive method completes under pure organic phase condition, and through contrast, more general aqueous conditions, gained Cu-series catalyst catalytic efficiency is higher.
Detailed description of the invention
According to following embodiment, the present invention may be better understood.But those skilled in the art will readily understand, the content described by embodiment only for illustration of the present invention, and should can not limit the present invention described in detail in claims yet.
The preparation of embodiment 1 catalyst
Preparation method:
(1) anhydrous sodium metasilicate is dissolved in methyl-sulfoxide, under the condition of nitrogen protection, in methyl-sulfoxide, passes into hydrogen chloride gas, on shaking table, react 4h at 45 DEG C;
(2) keep nitrogen protection condition, in the mixed system of step (1) gained, add copper chloride, on shaking table, react 1h at 40 DEG C;
(3) in the mixed system of gained in step (2), add polyacrylamide, fully mix, after colloidal sol is complete, get gel;
(4) by the gel of gained in step (3) with after deionized water rinsing 2 ~ 3 times, dry with sodium sulfite, finally at 700 DEG C, after roasting 1h, obtain Cu-series catalyst.
In step (1) ~ (3), agents useful for same is all through anhydrous process.
In step (1), the weight ratio of anhydrous sodium metasilicate and organic solvent is 1:100.
In step (1), the mol ratio of anhydrous sodium metasilicate and hydrogen chloride is 1:3.
In step (2), in anhydrous sodium metasilicate and copper chloride, the mol ratio of copper is 60:1.
In step (3), the mass ratio of polyacrylamide and anhydrous sodium metasilicate is 1:700.
Comparative example 1
Preparation method is with embodiment 1, and difference is, sodium metasilicate used is metasilicate pentahydrate sodium.
Comparative example 2
Preparation method is with embodiment 1, and difference is, methyl-sulfoxide is replaced with water.
Embodiment 2
The Cu-series catalyst prepared in embodiment 1, comparative example 1 and comparative example 2 is used for the reaction of catalysis ethanol and oxygen.According to the conversion of reaction rate, if the catalytic efficiency of Cu-series catalyst is 1 in embodiment 1, the catalytic efficiency in comparative example 1 is 0.8, and the catalytic efficiency in comparative example 2 is 0.6.
Claims (8)
1. a preparation method for Cu-series catalyst, is characterized in that, comprises the steps:
(1) sodium metasilicate is dissolved in organic solvent, under the condition of nitrogen protection, in organic solvent, passes into hydrogen chloride gas, at 30 ~ 60 DEG C, react 3 ~ 6h;
(2) keep nitrogen protection condition, in the mixed system of step (1) gained, add copper source, at 40 ~ 45 DEG C, react 1 ~ 3h;
(3) in the mixed system of gained in step (2), add precipitating reagent, fully mix, after colloidal sol is complete, get gel;
(4) by after the gel detergent of gained in step (3), drying, roast, Cu-series catalyst is obtained.
2. preparation method according to claim 1, is characterized in that, in step (1), described organic solvent is pyridine or methyl-sulfoxide.
3. preparation method according to claim 1, is characterized in that, in step (1), the weight ratio of sodium metasilicate and organic solvent is 1:50 ~ 200.
4. preparation method according to claim 1, is characterized in that, in step (1), the mol ratio of sodium metasilicate and hydrogen chloride is 1:1.5 ~ 3.5.
5. preparation method according to claim 1, is characterized in that, in step (2), described copper source is copper chloride or cupric phosphate.
6. preparation method according to claim 1, is characterized in that, in step (2), in sodium metasilicate and copper source, the mol ratio of copper is 50 ~ 75:1.
7. preparation method according to claim 1, is characterized in that, in step (3), described precipitating reagent is polyacrylamide or ferric sulfate; Wherein, the mass ratio of precipitating reagent and sodium metasilicate is 1:600 ~ 750.
8. preparation method according to claim 1, is characterized in that, in step (4), the method for washing is for using deionized water rinsing 2 ~ 3 times, and dry method is for using sodium sulfite dry, and the method for roast is roasting 1 ~ 1.5h at 600 ~ 700 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510779354.5A CN105289607A (en) | 2015-11-13 | 2015-11-13 | Preparation method of copper based catalyst |
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| CN201510779354.5A CN105289607A (en) | 2015-11-13 | 2015-11-13 | Preparation method of copper based catalyst |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080183020A1 (en) * | 2007-01-26 | 2008-07-31 | Carter Technologies | Catalytic conversion of alcohols to aldehydes and ketones |
| CN103633268A (en) * | 2012-08-22 | 2014-03-12 | 海洋王照明科技股份有限公司 | Preparation method of silicon dioxide composite separators |
| CN203870880U (en) * | 2014-05-14 | 2014-10-08 | 武守宇 | Simple experiment apparatus for oxidation of ethanol to acetaldehyde |
| CN104190396A (en) * | 2014-08-28 | 2014-12-10 | 无锡普爱德环保科技有限公司 | Preparation method of lithium-loaded silica gel catalyst |
-
2015
- 2015-11-13 CN CN201510779354.5A patent/CN105289607A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080183020A1 (en) * | 2007-01-26 | 2008-07-31 | Carter Technologies | Catalytic conversion of alcohols to aldehydes and ketones |
| CN103633268A (en) * | 2012-08-22 | 2014-03-12 | 海洋王照明科技股份有限公司 | Preparation method of silicon dioxide composite separators |
| CN203870880U (en) * | 2014-05-14 | 2014-10-08 | 武守宇 | Simple experiment apparatus for oxidation of ethanol to acetaldehyde |
| CN104190396A (en) * | 2014-08-28 | 2014-12-10 | 无锡普爱德环保科技有限公司 | Preparation method of lithium-loaded silica gel catalyst |
Non-Patent Citations (2)
| Title |
|---|
| 朱洪法: "《催化剂载体制备及应用技术》", 31 October 2014, 石油工业出版社 * |
| 陆鼎一: "《化学故事新编》", 31 July 2007, 苏州大学出版社 * |
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Application publication date: 20160203 |