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Method for preparing dehydrogenizing nickel-base/kieselguhr catalyst

A catalyst and diatomite technology, which is applied in the field of preparation of dehydrogenation nickel-based/diatomite catalysts, can solve the problems of rising production costs, increased catalyst production costs, and high content of active components nickel, and achieves high selectivity and improved Active and selective, low-dose effect

Inactive Publication Date: 2012-07-25
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the columnar catalyst contains 2wt% Sn, 50wt% Ni, the 1,2-cyclohexanediol conversion rate is 98.1%, and the catechol yield is 86.5%, but the nickel content of the active component is too high, and the catalyst production cost increases, Increased production costs throughout the production process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Weigh 30g of diatomaceous earth, Ni(CH 3 COO) 2 4H 2 O 14.1g, add 500ml of deionized water and stir to dissolve; weigh NaHCO 3 5.7g, dissolved in 150ml deionized water. At ultrasonic frequency 20kHz, ultrasonic sound intensity 100W / m 2 1. Under ultrasonic conditions with an ultrasonic action time of 125min, the nickel precipitate was obtained by ultrasonic precipitation. After the precipitation reaction, the material was filtered, washed with water, dried in an oven at 100°C for 4h, and then roasted in a muffle furnace at 300°C for 3h. Obtain catalyst powder dry matter. Take 10g of the above-mentioned catalyst dry material, add 5g of deionized water and 2g of hydroxymethylcellulose, mix well and knead well, then extrude or press into shape, and then dry at 90°C for 6h to obtain shaped catalyst A.

[0020] Weigh 0.31g of Na2SO4 and dissolve it in 8ml of deionized water, add 5g of the above-mentioned shaped catalyst A, and dissolve it at ultrasonic frequency 10kHz, ...

Embodiment 2

[0022] Get molding catalyst A among the embodiment 1, operate according to the following steps:

[0023] Weigh SnCl 2 2H 2 Dissolve 0.51g of O in 9ml of deionized water, add 5g of catalyst A, and make 2 1. Under the ultrasonic condition with the ultrasonic action time being 50min, the catalyst was modified by ultrasonic impregnation. The supernatant liquid was removed by siphon method, and the sample UPI 2 was obtained after drying at 70° C. for 4 hours. Its catalyst composition was 10 wt % Ni, 6 wt % Sn (based on diatomaceous earth).

Embodiment 3

[0025] Weigh diatomaceous earth 30g, Ni(NO 3 ) 2 ·6H 2 O 37.2g, add deionized water 600ml stirring and dissolving; Weigh (NH 4 ) 2 CO 3 14.7g, dissolved in 345ml deionized water, at ultrasonic frequency 30kHz, ultrasonic sound intensity 600W / m 2 1. Under ultrasonic conditions with an ultrasonic action time of 140min, the nickel precipitate was obtained by ultrasonic precipitation. After the precipitation reaction, the material was filtered, washed with water, dried in an oven at 120°C for 6h, and then roasted in a muffle furnace at 330°C for 4h. Obtain catalyst powder dry matter. Take 10g of the above-mentioned catalyst dry material, add 8g of deionized water, 3g of methyl cellulose, mix evenly and fully knead, extrude or press to form, and then dry at 100°C for 7h to obtain a shaped catalyst.

[0026] Weigh Cr(NO 3 ) 3 9H 2 O 3.3g is dissolved in 10ml of deionized water, add 5g of the above-mentioned molding catalyst, at ultrasonic frequency 30kHz, ultrasonic sound ...

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PUM

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Abstract

The invention relates to a method for preparing a dehydrogenizing nickel-base / kieselguhr catalyst, which comprises the following processes of: performing reaction of suspension obtained by mixing a soluble salt of nickel and kieselguhr and solution of precipitator to generate coprecipitate, and washing, drying, calcining, forming and modifying to prepare a catalyst used for the dehydrogenation of1,2-cyclohexanediol for preparing pyrocatechol. 10 to 30 weight percent of solution of 1,2-cyclohexanediol is used as a raw material, the conversion rate of the 1,2-cyclohexanediol is over 98 percent, and the selectivity of the pyrocatechol serving as a target product is between 90 and 95 percent at the reaction temperature of between 280 and 350 DEG C.

Description

technical field [0001] The invention relates to a preparation method of a dehydrogenation nickel-based / diatomite catalyst, in particular to a catalyst for preparing catechol by dehydrogenating 1,2-cyclohexanediol and a preparation method thereof. Background technique [0002] Catechol is an important chemical raw material, which is widely used in medicine, pesticides, spices, chemical additives, etc. At present, the main production method of catechol is the hydroxylation of phenol with hydrogen peroxide. 3 PO 4 / HClO 4 or H 2 SO 4 Under the action of a catalyst, hydrogen peroxide is hydroxylated to generate catechol and hydroquinone at the same time. This production method produces two kinds of diphenols at the same time, and the separation of the products is difficult, and the purity of catechol is not high; in addition, the above two Catalysts are highly corrosive substances, which not only endanger the environment, but also seriously corrode the equipment, and the op...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/755B01J37/34C07C39/08C07C37/06
Inventor 林陵曾崇余郑稳
Owner NANJING TECH UNIV
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