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Pd-based catalyst prepared through colloid deposition, preparation method and application

A catalyst and deposition technology, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of high equipment and material requirements, high catalyst costs, and high product costs, and achieve high colloidal stability. The effect of good restoration effect and reduction of production cost

Active Publication Date: 2013-04-03
SHANGHAI HUAYI GRP CO +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Patent CN101735182A discloses a process for continuously producing succinic anhydride by hydrogenation of maleic anhydride, but due to the high reaction pressure of this process, there are special requirements for reactor equipment, and the reaction process is many and complicated, resulting in high product cost and energy consumes a lot
[0005] Patent US5616730 and EP0691335 disclose a kind of use noble metal as catalyst to catalyze the hydrogenation of maleic anhydride to prepare succinic anhydride under solvent condition, wherein the content of noble metal catalyst Pd is 2-10%wt, thus cause catalyst cost to be too high, and reaction pressure is 4-6MPa, so the requirements for reactor equipment and materials are high

Method used

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  • Pd-based catalyst prepared through colloid deposition, preparation method and application

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Weigh 0.3366g PdCl 2 And 0.5547g NaCl solid is dissolved in the ethylene glycol solution of 1155.17ml, prepares Pd salt solution. Add 2.8485g PVP to the Pd salt solution to obtain a mixed solution, which is stirred for 2h.

[0035] Prepare fresh 0.5M NaOH / ethylene glycol solution, pipette an accurate amount of 7.6ml into the above mixture, and immediately obtain a black colloidal solution, stir for 3 hours.

[0036]Add 20g Al to the above black colloidal solution 2 o 3 Carrier and 1780ml distilled water, stirred for 3h. Then put it in a water bath for 12 hours. After the water bath, the mixture was suction filtered and washed with distilled water until no Cl was detected. - until. The washed catalysts were dried at 100°C for 2h and then dried at 300°C 2 / Ar roasting 2h, 300℃H 2 / Ar mixed gas reduction for 2h, down to room temperature, that is, Pd-based catalyst A.

Embodiment 2

[0038] Weigh 0.3366g PdCl 2 And 0.5547g NaCl solid is dissolved in the ethylene glycol solution of 1155.17ml, prepares Pd salt solution. Weigh 0.1355g of copper chloride and 0.2045g of nickel chloride and dissolve them in the Pd salt solution, then add 2.8485g of PVP to obtain a mixed solution, and stir for 2h.

[0039] Prepare fresh 0.5M NaOH / ethylene glycol solution, pipette an accurate 7.6ml of fresh 0.5M NaOH / ethylene glycol solution dropwise into the above mixture, and immediately obtain a black colloidal solution, stir for 3 hours.

[0040] Add 9.7983g Al to the above black colloidal solution 2 o 3 Carrier and 1780ml distilled water, stirred for 3h. Then put it in a water bath for 12 hours. After the water bath, the mixture was suction filtered and washed with distilled water until no Cl was detected. - until. The washed catalysts were dried at 100°C for 2h and then dried at 300°C 2 / Ar roasting 2h, 300℃H 2 / Ar mixed gas reduction for 2h, down to room temperature...

Embodiment 3

[0042] Weigh 0.3366g PdCl 2 And 0.5547g NaCl solid is dissolved in the ethylene glycol solution of 1155.17ml, prepares Pd salt solution. Weigh 0.1056g of chloroauric acid and dissolve it in the Pd salt solution. Then 2.8485g of PVP was added to obtain a mixed liquid, which was stirred for 2h.

[0043] Prepare fresh 0.5M NaOH / ethylene glycol solution, pipette an accurate amount of 7.6ml into the above mixture, and immediately obtain a black colloidal solution, stir for 3 hours.

[0044] Add 9.8488g apricot kernel charcoal carrier and 1780ml distilled water to the above black colloidal solution, and stir for 3h. Then put it in a water bath for 12 hours. After the water bath, the mixture was suction filtered and washed with distilled water until no Cl was detected. - until. The washed catalysts were dried at 100°C for 2h and then dried at 300°C 2 / Ar roasting 2h, 300℃H 2 / Ar mixed gas for 2h, then lowered to room temperature to obtain Pd-based catalyst C.

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Abstract

The invention discloses a Pd-based catalyst prepared through colloid deposition, a preparation method and application and specifically to a Pd-based catalyst prepared through addition of a protective agent PVP or PVA by using a colloid deposition process, a preparation method for the catalyst and application of the catalyst in preparation of succinic anhydride through hydrogenation of maleic anhydride. Under a mild condition, the Pd-based catalyst can realize continuous and high-activity catalysis of production of succinic anhydride through hydrogenation of maleic anhydride both in an intermittent high-pressure reaction vessel and on a fixed bed reactor, and high selectivity of succinic anhydride and good stability of the catalyst are achieved; the conversion rate of maleic anhydride is no less than 99.99%, and selectivity of succinic acid is no less than 99.99%. The Pd-based catalyst prepared in the invention has the advantages of small usage amount of the precious metal Pd, high activity and a long service life; and the catalyst can be repeatedly and indiscriminately used, so production cost is reduced, and the catalyst is suitable for industrial production.

Description

technical field [0001] The invention relates to a Pd-based catalyst, a preparation method and its application in catalyzing the hydrogenation of maleic anhydride to prepare succinic anhydride, in particular to a Pd-based catalyst prepared by adding a protective agent PVP or PVA colloidal deposition method, and its preparation Method and its application in the hydrogenation of maleic anhydride to prepare succinic anhydride. Background technique [0002] Succinic anhydride, also known as succinic anhydride, molecular formula C 4 h 4 o 3 , Colorless orthorhombic prismatic crystals. Soluble in carbon tetrachloride, alcohol, and chloroform, slightly soluble in water and ether. Succinic anhydride is an important fine chemical raw material, which is widely used in medicine, food industry, agriculture, petrochemical industry and other industries. In recent years, with the rapid development of these industries, the demand for succinic anhydride is also increasing year by year. ...

Claims

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Application Information

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IPC IPC(8): B01J23/44B01J23/89B01J23/52B01J29/00C07D307/60
Inventor 王振旅张春雷张文祥宁春利贾明君唐勇
Owner SHANGHAI HUAYI GRP CO
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