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A method for preparing methyl mercaptan by extracting aluminum modified composite catalyst from phosphogypsum

A composite catalyst, aluminum modification technology, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of high reaction temperature, low yield of target products, short catalyst reaction life, etc. High performance, enhance the degree of adsorption and dissociation, and alleviate the effect of carbon deposition

Active Publication Date: 2022-04-22
中建西部建设贵州有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to address the above problems, based on the fact that phosphogypsum also contains impurities such as phosphoric acid, aluminum, silicon, and iron in addition to the main component calcium sulfate, and the acid-base precipitation method is now used to extract the aluminum in the phosphogypsum impurities to obtain AlCl 3 ·6H 2 O, synthesize γ-Al with template 2 o 3 Composite with ZSM-5 catalyst to form γ-Al 2 o 3 @ZSM-5 composite catalyst to solve the problems of low target product yield, short catalyst reaction life and high reaction temperature in the synthesis of methyl mercaptan by hydrogen sulfide methanol method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Step 1, preparation of composite catalyst

[0044] Step 1.1: Acid leaching of waste gypsum: Add dilute hydrochloric acid to the dried waste gypsum powder according to the liquid-solid ratio of 20mL / g, stir and leaching for 1 hour at an acid leaching temperature of 80°C, centrifuge, take the supernatant, and obtain Add sodium hydroxide solution to the obtained supernatant, carry out solid-liquid separation, take its supernatant and add dilute hydrochloric acid, until the white precipitate is completely dissolved, generate aluminum chloride solution, evaporate and concentrate, cool and crystallize, filter to obtain AlCl 3 ·6H 2 O solution; wherein the dilute hydrochloric acid concentration is 1mol / L,

[0045] Step 1.2: γ-Al 2 o 3 Preparation: AlCl according to the molar ratio of raw materials 3 ·6H 2 O:CTAB=12.9-13.2:1-3, add cetyltrimethylammonium bromide CTAB to the AlCl prepared in step 1.1 3 ·6H 2 O solution, stir until dissolved, use a peristaltic pump at 5mL·...

Embodiment 2

[0051] Step 1, preparation of composite catalyst

[0052] Step 1.1: Acid leaching of waste gypsum: Add dilute hydrochloric acid to the dried waste gypsum powder according to the liquid-solid ratio of 20mL / g, stir and leaching for 1 hour at an acid leaching temperature of 80°C, centrifuge, take the supernatant, and obtain Add sodium hydroxide solution to the obtained supernatant, carry out solid-liquid separation, take its supernatant and add dilute hydrochloric acid, until the white precipitate is completely dissolved, generate aluminum chloride solution, evaporate and concentrate, cool and crystallize, filter to obtain AlCl 3 ·6H 2 O solution; wherein the dilute hydrochloric acid concentration is 1mol / L,

[0053] Step 1.2: γ-Al 2 o 3 Preparation: AlCl according to the molar ratio of raw materials 3 ·6H 2 O:CTAB=12.9-13.2:1-3, add cetyltrimethylammonium bromide CTAB to the AlCl prepared in step 1.1 3 ·6H 2 O solution, stir until dissolved, use a peristaltic pump at 5mL·...

Embodiment 3

[0059] Step 1, preparation of composite catalyst

[0060] Step 1.1: Acid leaching of waste gypsum: Add dilute hydrochloric acid to the dried waste gypsum powder according to the liquid-solid ratio of 20mL / g, stir and leaching for 1 hour at an acid leaching temperature of 80°C, centrifuge, take the supernatant, and obtain Add sodium hydroxide solution to the obtained supernatant, carry out solid-liquid separation, take its supernatant and add dilute hydrochloric acid, until the white precipitate is completely dissolved, generate aluminum chloride solution, evaporate and concentrate, cool and crystallize, filter to obtain AlCl 3 ·6H 2 O solution; wherein the dilute hydrochloric acid concentration is 1mol / L,

[0061] Step 1.2: γ-Al 2 o 3 Preparation: AlCl according to the molar ratio of raw materials 3 ·6H 2 O:CTAB=12.9-13.2:1-3, add cetyltrimethylammonium bromide CTAB to the AlCl prepared in step 1.1 3·6H 2 O solution, stir until dissolved, use a peristaltic pump at 5mL·m...

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Abstract

The invention discloses a method for preparing methyl mercaptan by extracting aluminum modified composite catalyst from phosphogypsum, comprising the following steps: acid leaching waste gypsum, separating and purifying aluminum to prepare γ-Al 2 o 3 , with the prepared γ‑Al 2 o 3 The sample was modified on ZSM-5 to obtain a composite catalyst, hydrogen sulfide gas and methanol gas fully contacted and reacted with the catalyst to obtain the product methyl mercaptan. On the one hand, this method removes some impurities in phosphogypsum, realizes the recycling of phosphogypsum solid waste, and at the same time utilizes the properties of the impurities themselves to prepare γ‑Al 2 o 3 The @ZSM‑5 composite catalyst has a long service life, a high selectivity of the product methyl mercaptan, and a lower reaction temperature.

Description

technical field [0001] The invention relates to a method for preparing methyl mercaptan with an aluminum-modified composite catalyst extracted from phosphogypsum, and belongs to the field of methyl mercaptan preparation. Background technique [0002] my country CH 3 The contradiction between supply and demand in the SH market is very prominent, CH 3 The annual output of SH is less than 20,000 tons, while the annual demand reaches hundreds of thousands of tons. Guizhou is rich in coal resources, how to solve coal-based CH in the process of vigorously developing the coal chemical industry 3 OH supply exceeds demand, and a large amount of H 2 The problem of resource utilization of S gas is very urgent. Therefore, according to the characteristics of mineral resources in Guizhou, H 2 S and CH 3 Catalytic synthesis of CH from OH 3 SH has strong regional resource advantages. Not only has the advantages of sufficient raw materials and low cost, but also solves the problem of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/40C07C321/04C07C319/08
CPCB01J29/40C07C319/08C07C321/04
Inventor 王乐李小涛林喜华袁义进赵士豪路东义何凯
Owner 中建西部建设贵州有限公司
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