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Modified nickel silicon catalyst and application thereof in preparation of gamma-butyrolactone (GBL) by means of catalytic hydrogenation of maleic anhydride

A catalyst and modification technology, which is applied in the field of modified nickel-silicon catalyst and its catalytic hydrogenation of maleic anhydride to prepare γ-butyrolactone, which can solve the problem of accelerating the aggregation and growth of catalyst active centers and the rate of carbon deposition, limiting large-scale In order to improve the activity and selectivity of the target product, promote adsorption and activation, and achieve good stability due to the application and harsh reaction conditions

Active Publication Date: 2019-03-29
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In summary, the reaction conditions for preparing GBL by hydrogenation of maleic anhydride are harsh (reaction temperature 200 o C), not only increases the energy consumption of the reaction, but also accelerates the rate of catalyst active center aggregation and carbon deposition, resulting in catalyst deactivation and poor stability. In addition, some catalysts contain metal Cr, which is seriously polluted and limits its large-scale application. application

Method used

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  • Modified nickel silicon catalyst and application thereof in preparation of gamma-butyrolactone (GBL) by means of catalytic hydrogenation of maleic anhydride

Examples

Experimental program
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Effect test

Embodiment 1

[0028] 1) At room temperature, 15.36 g Ni(NO 3 ) 2 ·6H 2 O and 0.3102g Ce(NO 3 )2 ·6H 2 Dissolve O in 300 ml distilled water, add 25% concentrated ammonia water (wt) dropwise to pH=11~12, stir to form a blue metal-ammonia complex solution;

[0029] 2) Add 17g of alkaline silica sol dropwise to the ammonium complex solution obtained in step 1) while stirring, continue to stir for 6 hours after the dropwise addition, and raise the temperature to 90 °C for uniform precipitation until the pH of the solution is 7. The precipitate was centrifuged, washed with distilled water three times, then dried overnight at 100 °C, and then roasted at 5 °C / min to 500 °C for 4 h to obtain the desired catalyst Ni-Ce-PS, active metal nickel: additive CeO 2 : Carrier SiO 2 The mass ratio is: 1:0.04:2.19.

[0030] 3) Catalyst at 25V%H with a hydrogen flow rate of 40 ml / min 2 -75V%N 2 In a mixed atmosphere, the temperature was raised to 400 °C at 5 °C / min for reduction for 2 h to obtain cataly...

Embodiment 2

[0032] 1) At room temperature, 15.36gNi(NO 3 ) 2 ·6H 2 O and 0.4577g Zn(NO 3 ) 2 ·6H 2 Dissolve O in a mixed solution of 250 ml of water and ethanol, add 25% concentrated ammonia water (wt) dropwise to pH=11~12, and stir to make a metal salt-ammonia complex solution;

[0033] 2) Add 17g of alkaline silica sol dropwise to the ammonium complex solution obtained in step 1) while stirring, continue to stir for 6 hours after the dropwise addition, and raise the temperature to 80 °C for uniform precipitation until the pH of the solution is 7. The precipitate was centrifuged, washed 3 times with distilled water, then dried overnight at 80 °C, and then roasted at 5 °C / min to 550 °C for 5 h to make catalyst Ni-Zn-PS, active metal nickel: additive ZnO: carrier SiO 2 The mass ratio is: 1:0.04:2.19.

[0034] 3) Catalyst at 25V%H with a hydrogen flow rate of 40 ml / min 2 -75V%N 2 In a mixed atmosphere, the temperature was raised to 500 °C at 5 °C / min for 2 h, and the catalyst 2# for...

Embodiment 3

[0036] 1) At room temperature, 15.36g Ni(NO 3 ) 2 ·6H 2 O and 0.1839g (NH 4 ) 6 Mo 7 o 24 4H 2 Dissolve O in 300 ml of water, add 25% concentrated ammonia water (wt) dropwise to pH=11~12, and stir to make a blue metal salt-ammonia complex solution;

[0037] 2) Add 17 g of alkaline silica sol dropwise to the ammonium complex solution obtained in step 1) while stirring, continue stirring for 10 h after the dropwise addition, and raise the temperature to 80 °C for uniform precipitation until the pH of the solution is 7. The precipitate was centrifuged, washed with distilled water three times, then dried overnight at 80 °C, and then calcined at 5 °C / min to 600 °C for 4 h to make the catalyst Ni-Mo-PS, active metal nickel: additive MoO 3 : Carrier SiO 2 The mass ratio is: 1:0.05:2.19.

[0038] 3) Catalyst at 25V%H with a hydrogen flow rate of 40 ml / min 2 -75V%N 2 In a mixed atmosphere, the temperature was raised to 550 °C at 5 °C / min for 2 h to reduce, and catalyst 3# fo...

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Abstract

The invention discloses a modified nickel silicon catalyst and application thereof in preparation of gamma-butyrolactone (GBL) by means of catalytic hydrogenation of maleic anhydride. The active component of the catalyst is metal Ni, one or two of reducible metal oxides CeO2 ZnO and MoO3 is / are used as additive(s), and SiO2 is taken as a carrier, wherein the mass ratio of the metal Ni to the additive(s) to the SiO2 is equal to 1 to (0.04-0.7) to (2-3.2). A preparation method of the catalyst comprises the following steps: mixing a nickel salt with an additive precursor metal salt solution in proportion, and then adding ammonia water into the metal mixture to form a metal ammonia complex; then, dropwise adding alkaline silica sol into the complex mixed solution, and precipitating by using aheating ammonia distillation method; filtering the obtained precipitate, washing, drying and calcining to obtain the oxidized state modified nickel silicon catalyst which is abbreviated as a Ni-M-PS catalyst. The catalyst can be used for preparation of the GBL by means of the catalytic hydrogenation of the maleic anhydride, has higher catalytic activity and stability, and has a potential industrial application value.

Description

technical field [0001] The invention relates to a modified nickel-silicon catalyst and its application in catalyzing the hydrogenation of maleic anhydride to prepare gamma-butyrolactone, belonging to the technical field of chemical catalysts. Background technique [0002] γ-butyrolactone (GBL), also known as γ-hydroxybutyrolactone, has the characteristics of good thermal stability, high boiling point, and strong conductivity. It is an important fine chemical and a strategic chemical intermediate with a wide range of uses . GBL is a green solvent widely used in the fields of fiber, polyester, agriculture and medicine. It is often used as a dyeing agent and antistatic agent in the fiber industry; it is often used as a dispersant, dyeing improver, plasticizer, etc. in the polyester industry. In the field of agriculture, it is a key intermediate for the synthesis of pesticides and herbicides. In the field of medicine, it is an intermediate for the synthesis of antibiotics suc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/83B01J23/80B01J23/883C07D305/10
CPCB01J23/80B01J23/83B01J23/883C07D305/10
Inventor 谭静静赵永祥赵丽丽崔静磊夏晓丽
Owner SHANXI UNIV
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