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Amorphous alloy catalyst for hydrogenating cyclobufene sultone and its prepn. and application

An amorphous alloy, sulfolane technology, applied in the preparation of organic compounds, physical/chemical process catalysts, organic chemistry, etc., can solve the problems of unsafe use of skeleton nickel, environmental pollution, etc., and achieve easy industrial scale-up The effect of production, no pollution, and simple preparation method

Inactive Publication Date: 2003-11-19
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the disadvantages of unsafe use and environmental pollution of framework nickel, it is urgent to develop a new catalyst with high efficiency and environmental friendliness.

Method used

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  • Amorphous alloy catalyst for hydrogenating cyclobufene sultone and its prepn. and application
  • Amorphous alloy catalyst for hydrogenating cyclobufene sultone and its prepn. and application
  • Amorphous alloy catalyst for hydrogenating cyclobufene sultone and its prepn. and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] 268K, under the protection of nitrogen, add nickel nitrate solution (85ml, 0.4mol / l) dropwise to KBH at a speed of 6ml / min 4 (60ml) solution. After the reaction, centrifuge, wash with water until neutral, and then protect in ethanol. In its X-ray diffraction pattern (Figure 1), a broadened diffuse peak appears near 2θ=45°, which is the characteristic diffraction peak of NiB amorphous alloy, indicating that the synthesized NiB alloy is indeed amorphous. The broadened diffuse peak around 2θ=22° belongs to the characteristic peak of amorphous metalloid B. The scanning electron microscope (Fig. 2a) shows that the NiB amorphous alloy particles are approximately spherical, with an average particle size of about 15nm. Product atomic composition: Ni 69 B 31 .

[0016] The present invention uses a 250ml high-pressure reactor to carry out the sulfolene hydrogenation reaction. Reaction conditions: ratio of sulfolene to catalyst 10-1; hydrogen pressure 3MPa; reaction temperat...

Embodiment 2

[0018] Add 24 grams of nickel hypophosphite, 2 grams of sodium acetate, and 4 grams of sodium citrate into 100 ml of distilled water at 300K, and adjust the pH of the solution to 7-8 with sodium hydroxide. Add a few drops of KBH while stirring 4 The solution initiates the reaction. The product was centrifuged, washed with water until neutral, and placed in ethanol for protection. In its X-ray diffraction pattern (Figure 1), a broadened diffuse peak appears near 2θ=45°, which is the characteristic diffraction peak of NiP amorphous alloy, indicating that the synthesized NiP alloy is indeed amorphous. The transmission electron microscope image (Fig. 3a) shows that the NiP amorphous alloy particles are spherical, with an average particle size of about 30nm. Product atomic composition: Ni 65 P 35 .

[0019] The reaction conditions are the same as in Example 1.

Embodiment 3

[0021] KBH under 300K 4 The solution (26ml) was dripped into the nickel hypophosphite solution (50ml, 1mol / l) at a rate of 0.9ml / min. The product was centrifuged, washed with water until neutral, and placed in ethanol for protection. In its X-ray diffraction pattern (Figure 1), a broadened diffuse peak appears near 2θ=45°, which is the characteristic diffraction peak of NiPB amorphous alloy, indicating that the synthesized NiPB alloy is indeed amorphous. Transmission electron microscopy (Figure 3b) shows that NiPB particles are irregular in shape, with an average particle size of about 20nm, which is between NiP and NiB. Product atomic composition: Ni 69 B 20 P 11 .

[0022] The reaction conditions are the same as in Example 1.

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Abstract

The present invention relates to a catalyst for cyclobutenesulfphone hydrogenation, its general formula is NixCoyBmPn, in which x=0-80, y=0.70, m=0-50 and n=0-50. It is an amorphous alloy, and possesses high low-temp. activity, and is easy to industrial production.

Description

Technical field: [0001] The invention relates to a catalyst for the hydrogenation of sulfolene, specifically an amorphous alloy catalyst composed of metal Ni or Co and B or P, a preparation method and an application in the reaction of hydrogenation of sulfolene to prepare sulfolane technology. Background technique [0002] Sulfolane, also known as tetramethylene sulfone, is an important solvent with excellent performance. Most organic compounds and polymers are soluble or miscible with sulfolane. Sulfolane is generally used as aromatic hydrocarbon extraction solvent, polymer spinning or casting solvent; natural gas, synthesis gas and refinery gas purification, desulfurization solvent, plastic and rubber solvent; in addition, it can also be used in textile and printing and dyeing industries as printing and dyeing aids, Can make the color bright and bright. [0003] The industrial production of sulfolane originated in the UK in the early 1940s. It is obtained by using butad...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/185C07C315/00C07C317/10
Inventor 李伟马延风张明慧周瑛陶克毅
Owner NANKAI UNIV
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