CN109876812A - A kind of preparation method of nickel-base hydrogenation catalyst - Google Patents
A kind of preparation method of nickel-base hydrogenation catalyst Download PDFInfo
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- CN109876812A CN109876812A CN201910074351.XA CN201910074351A CN109876812A CN 109876812 A CN109876812 A CN 109876812A CN 201910074351 A CN201910074351 A CN 201910074351A CN 109876812 A CN109876812 A CN 109876812A
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Abstract
The present invention discloses a kind of preparation method of nickel-base hydrogenation catalyst, which comprises the following steps: step 1: taking soluble nickel salt that deionized water is added to be made into the first solution；Take precipitating reagent that deionized water is added to be made into the second solution；Silica solution is taken, is configured to silicon sol solution to silica solution plus deionized water dilution；Step 2: silicon sol solution made from whipping step one, while the first solution made from step 1 and the second solution being taken to be added in silicon sol solution；Step 3: taking silicon sol solution made from step 2 to be warming up to 90~110 DEG C of evaporation waters, and be stirred simultaneously to it, and the silica solution for being loaded with nickel is precipitated；Step 4: will carry nisiloy sol precipitation and be washed with deionized to radical anion less than 0.03% (w/w), is then successively drying, is roasting, is obtaining catalyst precursor；Step 5: it takes catalyst precursor made from step 4 to restore and hydrogenation catalyst is made；The catalyst is used for aldehyde hydrogenation to alcohol.
Description
Technical field
The present invention relates to a kind of catalyst, and in particular to a kind of preparation method of nickel-base hydrogenation catalyst.
Background technique
Preparing alcohol by aldehyde plus hydrogen is a kind of important method for producing alcohol, uses Raney's nickel as hydrogenation catalyst at present more,
Although Raney's nickel activity is good, its is at high cost；Also useful Cu-series catalyst, but catalyst activity is bad, and reaction temperature is high.
Summary of the invention
It is an object of the invention to overcome above-mentioned technical deficiency, a kind of preparation method of nickel-base hydrogenation catalyst is provided, is had
Active height, feature at low cost are suitable for aldehyde and hydrogen are added to prepare alcohol.
To reach above-mentioned technical purpose, technical solution of the present invention provides a kind of preparation method of nickel-base hydrogenation catalyst,
Characterized by comprising the following steps:
Step 1: take soluble nickel salt that deionized water is added to be made into the first solution；Take precipitating reagent that deionized water is added to be made into second
Solution；Silica solution is taken, is configured to silicon sol solution to silica solution plus deionized water dilution；
Step 2: silicon sol solution made from whipping step one, while taking the first solution made from step 1 and second molten
Liquid is added in silicon sol solution, keeps the pH value of silicon sol solution between 8~10；
Step 3: it takes silicon sol solution made from step 2 to be warming up to 90~110 DEG C of evaporation waters, and it is carried out simultaneously
The silica solution for being loaded with nickel is precipitated in stirring；
Step 4: nisiloy sol precipitation will be carried and be washed with deionized to radical anion less than 0.03% (w/w), so
It is roasted under conditions of successively drying, 250~450 DEG C under conditions of 100~150 DEG C afterwards, obtains catalyst precursor.
Step 5: taking catalyst precursor made from step 4, is granulated, compression molding, forms rear catalyst in temperature
Degree restores for 200~450 DEG C of condition 1~10%H2-N2 gas, and hydrogenation catalyst is made.
Compared with prior art, the beneficial effect comprise that the catalyst is used for aldehyde hydrogenation to alcohol, 60~180
DEG C, under the conditions of 0.1~20Mpa of pressure, aldehyde can be saturated to methyl ester hydrogenation alcohol, selectivity is greater than 99%, and the catalyst system
This is caused to be lower than the manufacturing cost of Raney's nickel.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The present invention provides a kind of preparation methods of nickel-base hydrogenation catalyst, which comprises the following steps:
Step 1: take soluble nickel salt that deionized water is added to be made into the first solution；Take precipitating reagent that deionized water is added to be made into second
Solution；Silica solution is taken, is configured to silicon sol solution to silica solution plus deionized water dilution；
Step 2: silicon sol solution made from whipping step one, while taking the first solution made from step 1 and second molten
Liquid is added in silicon sol solution, keeps the pH value of silicon sol solution between 8~10；
Step 3: it takes silicon sol solution made from step 2 to be warming up to 90~110 DEG C of evaporation waters, and it is carried out simultaneously
The silica solution for being loaded with nickel is precipitated in stirring；
Step 4: nisiloy sol precipitation will be carried and be washed with deionized to radical anion less than 0.03% (w/w), so
It is roasted under conditions of successively drying, 250~450 DEG C under conditions of 100~150 DEG C afterwards, obtains catalyst precursor.
Step 5: taking catalyst precursor made from step 4, is granulated, compression molding, forms rear catalyst in temperature
Degree restores for 200~450 DEG C of condition 1~10%H2-N2 gas, and hydrogenation catalyst is made.
Specifically, the precipitating reagent is one of Na2CO3, NaOH, ammonium hydroxide or a variety of mixtures.
Specifically, the mass concentration of first solution is 1.0~30.0%；The mass concentration of second solution is
1.0~30.0%；The mass concentration of the silicon sol solution made from step 1 is 1.0~30.0%.
Aldehyde can be saturated first under the conditions of 60~180 DEG C, 0.1~20Mpa of pressure for aldehyde hydrogenation to alcohol by the catalyst
Ester through hydrogenation alcohol, selectivity is greater than 99%, and the catalyst manufacturing cost is lower than the manufacturing cost of Raney's nickel.
The above described specific embodiments of the present invention are not intended to limit the scope of the present invention..Any basis
Any other various changes and modifications that technical concept of the invention is made should be included in the guarantor of the claims in the present invention
It protects in range.
Claims (5)
1. a kind of preparation method of nickel-base hydrogenation catalyst, which comprises the following steps:
Step 1: take soluble nickel salt that deionized water is added to be made into the first solution；Take precipitating reagent that deionized water is added to be made into the second solution；
Silica solution is taken, is configured to silicon sol solution to silica solution plus deionized water dilution；
Step 2: silicon sol solution made from whipping step one, while the first solution made from step 1 being taken to add with the second solution
Enter in silicon sol solution, keeps the pH value of silicon sol solution between 8~10；
Step 3: it takes silicon sol solution made from step 2 to be warming up to 90~110 DEG C of evaporation waters, and it is stirred simultaneously
It mixes, the silica solution for being loaded with nickel is precipitated；
Step 4: by carry nisiloy sol precipitation be washed with deionized to radical anion less than 0.03% (w/w), then according to
Secondary drying under conditions of 100~150 DEG C roasts under conditions of 250~450 DEG C, obtains catalyst precursor；
Step 5: taking catalyst precursor made from step 4, is granulated, compression molding, forms rear catalyst in temperature and is
200~450 DEG C of condition is restored with 1~10%H2-N2 gas, and hydrogenation catalyst is made.
2. the preparation method of nickel-base hydrogenation catalyst according to claim 1, which is characterized in that the precipitating reagent is
One of Na2CO3, NaOH, ammonium hydroxide or a variety of mixtures.
3. the preparation method of nickel-base hydrogenation catalyst according to claim 1, which is characterized in that the matter of first solution
Measuring concentration is 1.0~30.0%.
4. the preparation method of nickel-base hydrogenation catalyst according to claim 1, which is characterized in that the matter of second solution
Measuring concentration is 1.0~30.0%.
5. the preparation method of nickel-base hydrogenation catalyst according to claim 1, which is characterized in that described made from step 1
The mass concentration of silicon sol solution is 1.0~30.0%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201910074351.XA CN109876812A (en) | 2019-01-25 | 2019-01-25 | A kind of preparation method of nickel-base hydrogenation catalyst |
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| CN201910074351.XA CN109876812A (en) | 2019-01-25 | 2019-01-25 | A kind of preparation method of nickel-base hydrogenation catalyst |
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5258346A (en) * | 1992-07-13 | 1993-11-02 | United Catalysts Inc. | Nickel hydrogenation catalyst |
| CN1478596A (en) * | 2002-08-26 | 2004-03-03 | 中国石化集团齐鲁石油化工公司 | technology of hydrogenatioin to produce iso octanol using iso octaldehyde mixture and its catalyst |
| CN103506123A (en) * | 2012-06-29 | 2014-01-15 | 中国石油化工股份有限公司 | Preparation method of aldehyde liquid-phase hydrogenation catalyst |
| CN103553876A (en) * | 2013-10-23 | 2014-02-05 | 中国海洋石油总公司 | Liquid phase hydrogenation method for residual liquids of butanol and octanol |
| CN105080548A (en) * | 2014-05-08 | 2015-11-25 | 中国石油化工股份有限公司 | Method for improving selectivity and stability of nickel liquid phase hydrogenation catalyst |
| WO2016025383A1 (en) * | 2014-08-11 | 2016-02-18 | Basf Corporation | Hydrogenation catalysts |
| CN105561997A (en) * | 2014-10-11 | 2016-05-11 | 中国石油化工股份有限公司 | Preparation method of nickel liquid phase hydrogenation catalyst |
| CN107486207A (en) * | 2017-08-28 | 2017-12-19 | 如皋市玉辉助剂厂 | A kind of aldehyde liquid phase hydrogenating catalyst |
| CN107970938A (en) * | 2016-10-25 | 2018-05-01 | 中国石油化工股份有限公司 | A kind of hydrogenation catalyst and its preparation method and application |
-
2019
- 2019-01-25 CN CN201910074351.XA patent/CN109876812A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5258346A (en) * | 1992-07-13 | 1993-11-02 | United Catalysts Inc. | Nickel hydrogenation catalyst |
| CN1478596A (en) * | 2002-08-26 | 2004-03-03 | 中国石化集团齐鲁石油化工公司 | technology of hydrogenatioin to produce iso octanol using iso octaldehyde mixture and its catalyst |
| CN103506123A (en) * | 2012-06-29 | 2014-01-15 | 中国石油化工股份有限公司 | Preparation method of aldehyde liquid-phase hydrogenation catalyst |
| CN103553876A (en) * | 2013-10-23 | 2014-02-05 | 中国海洋石油总公司 | Liquid phase hydrogenation method for residual liquids of butanol and octanol |
| CN105080548A (en) * | 2014-05-08 | 2015-11-25 | 中国石油化工股份有限公司 | Method for improving selectivity and stability of nickel liquid phase hydrogenation catalyst |
| WO2016025383A1 (en) * | 2014-08-11 | 2016-02-18 | Basf Corporation | Hydrogenation catalysts |
| CN105561997A (en) * | 2014-10-11 | 2016-05-11 | 中国石油化工股份有限公司 | Preparation method of nickel liquid phase hydrogenation catalyst |
| CN107970938A (en) * | 2016-10-25 | 2018-05-01 | 中国石油化工股份有限公司 | A kind of hydrogenation catalyst and its preparation method and application |
| CN107486207A (en) * | 2017-08-28 | 2017-12-19 | 如皋市玉辉助剂厂 | A kind of aldehyde liquid phase hydrogenating catalyst |
Non-Patent Citations (1)
| Title |
|---|
| 李建中等: "以单分散硅溶胶为前体制备的Ni/SiO_2催化剂上甲烷部分氧化制合成气 ", 《石油化工》 * |
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Application publication date: 20190614 |
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