CN102335611A - Novel catalyst used in maleic anhydride liquid phase hydrogenation for preparing gamma-butyrolactone, and preparation method thereof - Google Patents
Novel catalyst used in maleic anhydride liquid phase hydrogenation for preparing gamma-butyrolactone, and preparation method thereof Download PDFInfo
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- CN102335611A CN102335611A CN2010102347850A CN201010234785A CN102335611A CN 102335611 A CN102335611 A CN 102335611A CN 2010102347850 A CN2010102347850 A CN 2010102347850A CN 201010234785 A CN201010234785 A CN 201010234785A CN 102335611 A CN102335611 A CN 102335611A
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Abstract
The invention discloses a novel catalyst used in maleic anhydride liquid phase hydrogenation for preparing gamma-butyrolactone. The catalyst is characterized in that: the catalyst is composed of a carrier, a main active component, and an auxiliary agent. The main active component is metal nickel, the auxiliary agent is molybdenum, and the carrier is active carbon. The product provided by the invention is advantaged in that: according to the invention, when the 20% Ni-Mo/AC catalyst prepared by using a co-impregnation method is used in a maleic anhydride hydrogenation, a result shows that the activity of the novel catalyst prepared with the co-impregnation method is high, and a gamma-butyrolactone yield reaches 97.6%. The invention also provides a preparation method for the novel catalyst used in the maleic anhydride hydrogenation for preparing gamma-butyrolactone, such that the product can be obtained.
Description
Technical field
The present invention relates to a kind ofly be used for cis-butenedioic anhydride liquid-phase hydrogenatin and prepare new catalyst of gamma-butyrolacton and preparation method thereof.This catalyst is that main active component, molybdenum are that auxiliary agent, active carbon are carrier with metallic nickel, and its preparation method comprises step impregnation method and co-impregnation.
Background technology
Cis-butenedioic anhydride liquid-phase hydrogenatin is divided into homogeneous phase liquid phase catalytic hydrogenation and heterogeneous liquid phase catalytic hydrogenation.The metal ion that is used for the homogeneous catalyst of cis-butenedioic anhydride liquid-phase hydrogenatin mainly is noble metal such as Ru, Rh, the Pd etc. in the transition metal, also has base metals such as Ni, Co in addition, and its part is organic phosphine mostly.Though homogeneous catalytic hydrogenation has higher gamma-butyrolacton selectivity, sees from the angle of technology, still exists catalyst activity lower, and a lot of Ru complex compound catalysts also contain the shortcomings such as halogen atom of meeting corrosion reaction equipment.The active component that is used for heterogeneous liquid phase catalytic hydrogenation reaction system mainly contains precious metals pt, Pd, Ru etc. and base metal Cu, Ni etc., and suitably adds other auxiliary agents to improve activity of such catalysts and selectivity.But because noble metal catalyst costs an arm and a leg, therefore cheap nickel obtains going deep into extensive studies as a kind of effective liquid phase hydrogenating catalyst.
Summary of the invention
In order to improve the yield of gamma-butyrolacton in the maleic anhydride hydrogenation reaction, the present invention provides a kind of preparation method who is used for the new catalyst of maleic anhydride hydrogenation reaction.This method is to be carrier with the active carbon, and metallic nickel is a major catalyst, and molybdenum is the aided metal catalyst.Use this bimetallic catalyst to make the yield of butyrolactone up to 97.6%.
Technical scheme of the present invention is following: a kind of maleic anhydride hydrogenation prepares the new catalyst of gamma-butyrolacton, it is characterized in that: this catalyst is made up of carrier, main active component and auxiliary agent three parts; Said main active component is a metallic nickel; Said auxiliary agent is a molybdenum; Said carrier is an active carbon.
Further, the content of said metallic nickel is at 10%-50%.
Further, in the said catalyst atomic ratio of auxiliary agent molybdenum and metallic nickel between 0.1-0.5.
The present invention also provides with a kind of and prepares the method that maleic anhydride hydrogenation prepares the new catalyst of gamma-butyrolacton, it is characterized in that step is following: the active carbon that carrier is selected for use is washed till neutral subsequent use through 120 ℃ of reflux of red fuming nitric acid (RFNA) 4 hours then; Choose metallic nickel and auxiliary agent molybdenum in proportion, adopt the method that is total to dipping and step impregnation to prepare 20%Ni-Mo/AC (n (Mo)/n (Ni)=0.1) catalyst; The aqueous solution Immesion active carbon of nickel nitrate that is prepared into then and ammonium molybdate, drying, hydrogen reducing gets finished product.
Advantage of the present invention: adopt that the prepared 20%Ni-Mo/AC catalyst of co-impregnation is used for the maleic anhydride hydrogenation reaction among the present invention, the result shows that the prepared new catalyst activity of co-impregnation is higher, makes the yield of gamma-butyrolacton up to 97.6%.
The practical implementation method
Embodiment 1
The 0.9910g nickel nitrate is dissolved in the 1.132g deionized water, and wiring solution-forming is added drop-wise in the 0.8g absorbent charcoal carrier then.With leaving standstill 12 hours under the sample room temperature that obtains,, and then be added to that (0.0602g ammonium molybdate, 1.5g deionized water) left standstill 12 hours in the ammonium molybdate aqueous solution for preparing under room temperature again 120 ℃ of oven dry; In 120 ℃ of dryings 12 hours, temperature programming to 400 ℃ was through hydrogen reducing 4 hours; Naturally cooling adds the 40mL solvent, the 4g cis-butenedioic anhydride then; 180 ℃, be used for the maleic anhydride hydrogenation reaction under the 6MPa condition, the yield of gamma-butyrolacton is 91.1%.
Embodiment 2
0.9910g nickel nitrate and 0.0602g ammonium molybdate are dissolved in the 1.132g deionized water, and wiring solution-forming was added drop-wise in the 0.8g absorbent charcoal carrier under the room temperature incipient impregnation 12 hours then; In 120 ℃ of dryings 12 hours, temperature programming to 400 ℃ was through hydrogen reducing 4 hours; Naturally cooling adds the 40mL solvent, the 4g cis-butenedioic anhydride then; 180 ℃, be used for the maleic anhydride hydrogenation reaction under the 6MPa condition, the yield of gamma-butyrolacton is 97.6%.
Claims (4)
1. a cis-butenedioic anhydride liquid-phase hydrogenatin prepares the new catalyst of gamma-butyrolacton, and it is characterized in that: this catalyst is made up of carrier, main active component and auxiliary agent three parts; Said main active component is a metallic nickel; Said auxiliary agent is a molybdenum; Said carrier is an active carbon.
2. a kind of cis-butenedioic anhydride liquid-phase hydrogenatin according to claim 1 prepares the new catalyst of gamma-butyrolacton, it is characterized in that: the content of said metallic nickel is at 10%-50%.
3. a kind of cis-butenedioic anhydride liquid-phase hydrogenatin according to claim 1 prepares the new catalyst of gamma-butyrolacton, it is characterized in that: the atomic ratio of auxiliary agent molybdenum and metallic nickel is between 0.1-0.5 in the said catalyst.
4. one kind prepares the method that the described cis-butenedioic anhydride liquid-phase hydrogenatin of claim 1 prepares the new catalyst of gamma-butyrolacton, it is characterized in that step is following: the active carbon that carrier is selected for use is washed till neutral subsequent use through 120 ℃ of reflux of red fuming nitric acid (RFNA) 4 hours then; Choose metallic nickel and auxiliary agent molybdenum in proportion, adopting altogether, the method for dipping prepares 20%Ni-Mo/AC (n (Mo)/n (Ni)=0.1) catalyst; The aqueous solution Immesion active carbon of nickel nitrate that is prepared into then and ammonium molybdate, drying, hydrogen reducing gets finished product.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010102347850A CN102335611A (en) | 2010-07-23 | 2010-07-23 | Novel catalyst used in maleic anhydride liquid phase hydrogenation for preparing gamma-butyrolactone, and preparation method thereof |
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| CN2010102347850A CN102335611A (en) | 2010-07-23 | 2010-07-23 | Novel catalyst used in maleic anhydride liquid phase hydrogenation for preparing gamma-butyrolactone, and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103055883A (en) * | 2012-12-28 | 2013-04-24 | 浙江大学 | Supported nickel-based catalyst and its preparation method and use |
| CN103769105A (en) * | 2012-10-24 | 2014-05-07 | 中国石油化工股份有限公司 | Catalyst for hydrogenating cis-butenedioic anhydride to prepare butanedioic anhydride and its preparation method and application |
| CN103769117A (en) * | 2012-10-24 | 2014-05-07 | 中国石油化工股份有限公司 | Catalyst for hydrogenating cis-butenedioic anhydride to prepare butanedioic anhydride and its preparation method and application |
| CN105642292A (en) * | 2016-01-30 | 2016-06-08 | 山西大学 | Preparation method for C(Ni) nano-catalyst for synthesizing gamma-butyrolactone through maleic anhydride hydrogenation |
| CN106861706A (en) * | 2017-02-28 | 2017-06-20 | 山西大学 | Synthesize nickel-base catalyst and preparation method and the application of gamma butyrolactone |
| CN106861703A (en) * | 2017-02-28 | 2017-06-20 | 山西大学 | A kind of catalyst and its preparation method and application for cis-butenedioic anhydride liquid-phase hydrogenatin synthesis gamma butyrolactone |
| CN106914246A (en) * | 2017-02-28 | 2017-07-04 | 山西大学 | The supported nickel catalyst and preparation method and application of cis-butenedioic anhydride liquid-phase hydrogenatin synthesis gamma butyrolactone |
| CN107698542A (en) * | 2017-10-19 | 2018-02-16 | 山东德普化工科技有限公司 | Prepare the device and method of gamma butyrolactone |
| RU2722837C1 (en) * | 2019-12-27 | 2020-06-04 | Федеральное государственное автономное образовательное учреждение высшего образования "Новосибирский национальный исследовательский государственный университет" (Новосибирский государственный университет, НГУ) | Method of preparing a hydrogenation catalyst for furfurol and furfuryl alcohol to 2-methylfuran |
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2010
- 2010-07-23 CN CN2010102347850A patent/CN102335611A/en active Pending
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103769105A (en) * | 2012-10-24 | 2014-05-07 | 中国石油化工股份有限公司 | Catalyst for hydrogenating cis-butenedioic anhydride to prepare butanedioic anhydride and its preparation method and application |
| CN103769117A (en) * | 2012-10-24 | 2014-05-07 | 中国石油化工股份有限公司 | Catalyst for hydrogenating cis-butenedioic anhydride to prepare butanedioic anhydride and its preparation method and application |
| CN103769117B (en) * | 2012-10-24 | 2015-11-18 | 中国石油化工股份有限公司 | A kind of maleic anhydride hydrogenation prepares succinic anhydride Catalysts and its preparation method and application |
| CN103769105B (en) * | 2012-10-24 | 2016-01-06 | 中国石油化工股份有限公司 | A kind of maleic anhydride hydrogenation prepares Catalysts and its preparation method and the application of succinic anhydride |
| CN103055883A (en) * | 2012-12-28 | 2013-04-24 | 浙江大学 | Supported nickel-based catalyst and its preparation method and use |
| CN105642292B (en) * | 2016-01-30 | 2018-04-03 | 山西大学 | Preparation method for C (Ni) nanocatalyst of maleic anhydride hydrogenation synthesis gamma butyrolactone |
| CN105642292A (en) * | 2016-01-30 | 2016-06-08 | 山西大学 | Preparation method for C(Ni) nano-catalyst for synthesizing gamma-butyrolactone through maleic anhydride hydrogenation |
| CN106861706A (en) * | 2017-02-28 | 2017-06-20 | 山西大学 | Synthesize nickel-base catalyst and preparation method and the application of gamma butyrolactone |
| CN106914246A (en) * | 2017-02-28 | 2017-07-04 | 山西大学 | The supported nickel catalyst and preparation method and application of cis-butenedioic anhydride liquid-phase hydrogenatin synthesis gamma butyrolactone |
| CN106861703A (en) * | 2017-02-28 | 2017-06-20 | 山西大学 | A kind of catalyst and its preparation method and application for cis-butenedioic anhydride liquid-phase hydrogenatin synthesis gamma butyrolactone |
| CN106861706B (en) * | 2017-02-28 | 2019-09-10 | 山西大学 | The preparation method and application of the nickel-base catalyst of synthetic gamma butyrolactone |
| CN106861703B (en) * | 2017-02-28 | 2019-09-10 | 山西大学 | A kind of preparation method of the catalyst for cis-butenedioic anhydride liquid-phase hydrogenatin synthetic gamma butyrolactone |
| CN106914246B (en) * | 2017-02-28 | 2019-11-19 | 山西大学 | The preparation method of the supported nickel catalyst of cis-butenedioic anhydride liquid-phase hydrogenatin synthetic gamma butyrolactone |
| CN107698542A (en) * | 2017-10-19 | 2018-02-16 | 山东德普化工科技有限公司 | Prepare the device and method of gamma butyrolactone |
| RU2722837C1 (en) * | 2019-12-27 | 2020-06-04 | Федеральное государственное автономное образовательное учреждение высшего образования "Новосибирский национальный исследовательский государственный университет" (Новосибирский государственный университет, НГУ) | Method of preparing a hydrogenation catalyst for furfurol and furfuryl alcohol to 2-methylfuran |
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Application publication date: 20120201 |