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

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

CN110026232BActive Publication Date: 2022-04-22中建西部建设贵州有限公司
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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

Patent Timeline
22 Apr 2022
Publication
CN110026232B
IPC
B01J29/40; C07C321/04; C07C319/08
CPC
B01J29/40; C07C319/08; C07C321/04
Inventors
王乐; 李小涛