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Phosphorous catalyst for synthesizing methyl mercaptan and preparation method thereof

A technology of methyl mercaptan and catalyst, which is applied in the field of catalysts, can solve the problems of increasing post-treatment procedures, difficult removal, low selectivity, etc., and achieve the effects of improving pore structure properties, high conversion rate, and reducing reaction temperature

Inactive Publication Date: 2011-11-23
XIAMEN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] German patent DE-C1193038 discloses a method that can separate DMS, in a separate reactor, using MoO 3 / Al 2 o 3 As a catalyst, the technology to convert DMS into methyl mercaptan, but requires excess H 2 S, and low selectivity
U.S. Patent No. 4005149 discloses a method for synthesizing methyl mercaptan from methyl sulfide and hydrogen sulfide by using sulfonamide as a catalyst, adding carbon disulfide as a promoter, but the presence of carbon disulfide increases the complicated post-treatment process, and Not easy to remove

Method used

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  • Phosphorous catalyst for synthesizing methyl mercaptan and preparation method thereof
  • Phosphorous catalyst for synthesizing methyl mercaptan and preparation method thereof
  • Phosphorous catalyst for synthesizing methyl mercaptan and preparation method thereof

Examples

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Effect test

Embodiment 1

[0019] Embodiment 1: Take by weighing 73.68g aluminum nitrate nonahydrate, dissolve with 200.0ml distilled water, be made into the Al(NO of 0.5mol / L 3 ) 3 solution, heated to 70°C under constant stirring, and added 0.5mL PEG400 and 0.18g (NH 4 ) 2 HPO 4 , increase the stirring speed, add 25% ammonia water drop by drop to form a gel, adjust the pH value to 6.5, continue stirring for 1 hour, aging at room temperature for 24 hours, drying in an oven at 80°C for 24 hours, and calcining in a muffle furnace at 550°C for 3 hours. 1% phosphorus modified γ-Al 2 o 3 (A).

[0020] The activity evaluation of the catalyst was carried out on a fixed-bed reaction system. The loading amount of the catalyst was 1mL, the particle size was 30-60 mesh, and the molar ratio of hydrogen sulfide to methyl sulfide was 4; the space velocity of the reactant material was 1000h -1 , the reaction pressure of the reaction system is 0.5MPa, the reaction temperature is 320 and 360°C, the conversion rate...

Embodiment 2、3

[0023] Embodiment 2,3: the 0.18g (NH 4 ) 2 HPO 4 Respectively changed to 0.54g (NH 4 ) 2 HPO 4 and 0.90g (NH 4 ) 2 HPO 4 , the rest of the preparation method is the same as in Example 3 to obtain 3% phosphorus-modified γ-Al 2 o 3 and 5% phosphorus-modified γ-Al 2 o 3 (A). The activity evaluation of the catalyst is the same as in Example 1, and the results are shown in Table 1.

Embodiment 4

[0025] Embodiment 4: Weigh 47.28g aluminum chloride hexahydrate, dissolve with 200.0ml distilled water, and make 0.5mol / L AlCl 3 solution, heated to 70°C under constant stirring, and added 0.5mL PEG400 and 0.18g (NH 4 ) 2 HPO 4 , increase the stirring rate, add 25% ammonia water dropwise to form a gel, adjust the pH value to 6.5, continue stirring for 1 hour, aging at room temperature for 24 hours, drying in an oven at 80°C for 24 hours, and calcining at 500°C for 5 hours. 1% phosphorus modified γ-Al 2 o 3 (B). The activity evaluation of the catalyst is the same as in Example 1, and the results are shown in Table 2.

[0026] Catalyst composition and activity evaluation result of table 2 embodiment 4~8 and comparative example 2

[0027]

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Abstract

The invention relates to a catalyst and provides a phosphorous catalyst with higher methyl sulfide transformation rate and methyl mercaptan selectivity for synthesizing the methyl mercaptan, and a preparation method thereof. The phosphorous catalyst is phosphorus modified alumina, the content of phosphorus contained in the phosphorous catalyst is 1-10 percent and preferably 3-5 percent, and the balance is alumina. The preparation method comprises the following steps of: dissolving a metered aluminum precursor by using water to prepare an aluminum solution; heating the aluminum solution, and then adding a metered phosphorus precursor solution and a dispersing agent, stirring, and adding a precipitator to form a gel solution at the same time; regulating the pH value of the gel solution to 5-9, and then ageing; drying the aged gel to constant weight, and then calcining to obtain the phosphorous catalyst for synthesizing the methyl mercaptan.

Description

technical field [0001] The invention relates to a catalyst, in particular to a catalyst for synthesizing methyl mercaptan by reacting methyl sulfide and hydrogen sulfide and a preparation method thereof. Background technique [0002] Methyl mercaptan is an important chemical intermediate for the synthesis of methionine, pharmaceuticals and pesticides. Its traditional manufacturing method is produced by the reaction of methanol and hydrogen sulfide. The catalyst is generally supported by transition metals and promoted by alkali metals, such as K 2 WO 4 -Al 2 o 3 . Excess hydrogen sulfide in this reaction is accompanied by the formation of by-product methyl sulfide (DMS) and other polysulfide compounds (such as dimethyl disulfide DMDS). These sulfur-containing by-products can be removed as waste gas in the stripping process of gas products , such treatment not only consumes energy but also has no utilization value, which reduces the total selectivity of the product methyl ...

Claims

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Application Information

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IPC IPC(8): B01J27/14B01J35/10C07C321/04C07C319/08
Inventor 杨意泉陈世萍张元华郑道敏姚如杰方维平
Owner XIAMEN UNIV
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