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Benzene selection noncrystalline catalyst with hydrogen added and containing ruthenium, boron as well as its preparing method

A technology for selective hydrogenation and catalyst, which is applied in the chemical industry and can solve the problems of unsatisfactory hydrogenation results.

Inactive Publication Date: 2003-10-08
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most catalysts and their corresponding benzene selective hydrogenation results are far from satisfactory

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1: the preparation of ultrafine Ru-B amorphous alloy catalyst

[0021] Will contain 15mL 0.1M RuCl 3 The beaker of the aqueous solution was placed in a constant temperature water bath, and under strong stirring, 10mL of 1M potassium borohydride aqueous solution was added dropwise. First wash the black precipitate fully with distilled water, then wash it several times with absolute ethanol, and finally put the black precipitate Ru-B powder in absolute ethanol for protection. Ru-B powders at different temperatures can be obtained by adjusting the temperature of the water bath. Some characterization results of the catalyst are shown in Table 1.

Embodiment 2

[0022] Embodiment 2: supported amorphous RuB / Zr(OH) 4 ·xH 2 Preparation of O catalyst

[0023] The preparation of the catalyst adopts the preparation methods of chemical reduction and chemical mixing. In a constant temperature water bath at 40°C, under stirring, mix 20mL of 6M ammonia solution and 10mL of 0.2M KBH 4 The aqueous solution was slowly added dropwise to the RuCl 3 (5.3×10 -3 M) and ZrOCl 2 (5.5×10 -2 M) in the mixed solution. After the hydrogen gas was released, the stirring was continued for 40 min. The resulting black precipitate was kept in the mother liquor overnight and then washed with distilled water to be free of Cl - ion.

[0024] The catalyst modified by Zn and Co is prepared by the same method as above, and zinc salt and cobalt salt are respectively pre-dissolved in the mixed solution. The catalyst is recorded as RuB-Zn / Zr(OH) 4 ·xH 2 O and RuB-Co / Zr(OH) 4 ·xH 2 O.

Embodiment 3

[0025] Embodiment 3: Supported RuB / SiO 2 Preparation of Amorphous Catalysts

[0026] Loaded RuB / SiO 2 The amorphous catalyst is prepared by impregnation reduction method. With a certain concentration of RuCl 3 Solution impregnated 1g SiO 2 Carrier, SiO 2Before use, the carrier is boiled and washed with 0.5% by weight of dilute nitric acid for 2 hours, dried under an infrared lamp at 110°C overnight, then roasted in a muffle furnace at 500°C for 2 hours, and then crushed to 40-60 meshes. After the impregnated carrier was dried under an infrared lamp at 110° C. overnight, 0.200 M potassium borohydride solution was slowly added dropwise, with a molar ratio of B / Ru=4 / 1 to ensure that the ruthenium ions were completely reduced. The entire operation was carried out in an ice-water bath and vigorous stirring was avoided to slow down the reduction reaction rate and prevent the reduced ruthenium from being re-oxidized. The catalyst is washed with distilled water to pH = 7.3-7.8, ...

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Abstract

A non-crystal catalyst for preparing cyclodexene by selectively hydrogenating benzene is prepared from Ru, B meta or metal oxide modified M, and the oxide or metal hydroxide carrier L through reducing Ru ions and M in oxide form, and removing ions of impurities. Its advantage is high selectivity and hydrogenating activity.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and relates to a novel amorphous catalyst for preparing cyclohexene through selective hydrogenation of benzene and a preparation method thereof. Background technique [0002] Cyclohexene is an important organic synthesis intermediate, which can be widely used in the production of medicines, pesticides, agrochemicals, feed additives, polyesters and other fine chemicals. In particular, cyclohexanone and adipic acid, the deep-processing products of cyclohexene, are widely used intermediates in the synthesis of polyamide fibers. Due to the traditional methods of producing cyclohexene, such as cyclohexanol dehydration method, halocyclohexane dehydrohalogenation method and Birch reduction method, etc., there are disadvantages such as complex production process and high cost, so cyclohexene is only used in lysine High value-added fine chemical products such as cyclohexene oxide and cyclohexen...

Claims

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Application Information

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IPC IPC(8): B01J23/46B01J37/00C07C5/11C07C13/18
CPCY02P20/52
Inventor 乔明华王建强谢颂海范康年
Owner FUDAN UNIV
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