Method for recovering chloromethane from acid methanol tail gas

A tail gas recovery and methyl chloride technology, which is applied in chemical recovery, chemical instruments and methods, climate sustainability, etc., can solve the problems of reduced catalyst activity and poor stability, so as to prolong catalyst life, improve reaction selectivity, The effect of high specific surface area

Pending Publication Date: 2022-08-05
ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the carbon deposit layer covers the active center or blocks the pores, it prevents the reactants from approaching the active center, which reduces the activity of the catalyst and deteriorates the stability.

Method used

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  • Method for recovering chloromethane from acid methanol tail gas
  • Method for recovering chloromethane from acid methanol tail gas

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The preparation method of solid-phase catalyst comprises the following steps:

[0034] (1) Preparation of ZSM-5: add 100g of sodium silicate, 1g of sodium metaaluminate, and 10,000mL of deionized water into the reactor, stir evenly, add 30g of tetrapropylammonium bromide, stir evenly, add sulfuric acid to adjust pH , heated to 150°C, hydrothermally crystallized for 48h, washed with water, dried, and calcined in a muffle furnace to obtain ZSM-5;

[0035] (2) Preparation of modified ZSM-5: 65mL of N,N-dimethylformamide, 10g of ZSM-5, 8g of 2-bromopropionic acid, and 600mL of dichloromethane were added to the reactor, stirred mechanically, and reacted at room temperature for 12h, Filter under reduced pressure, wash and dry to obtain modified ZSM-5;

[0036](3) prepare phosphorus-modified ZSM-5: 4g triphenylphosphine, 10g toluene are added in the reactor, mechanical stirring is dissolved, and 0.7g potassium iodide aqueous solution, 10g modified ZSM-5 are added, and the pot...

Embodiment 2

[0039] The preparation method of solid-phase catalyst comprises the following steps:

[0040] (1) Preparation of ZSM-5: add 100g sodium silicate, 25g sodium metaaluminate, and 15000mL deionized water to the reaction kettle, stir mechanically, add 45g tetrapropylammonium bromide, stir mechanically, add sulfuric acid to adjust pH , heated to 165°C, hydrothermally crystallized for 60h, washed with water, dried, and calcined in a muffle furnace to obtain ZSM-5;

[0041] (2) Preparation of modified ZSM-5: 85mL of N,N-dimethylformamide, 10g of ZSM-5, 9g of 2-bromopropionic acid, and 1000mL of dichloromethane were added to the reactor, stirred mechanically, and reacted at room temperature for 15h, Filter under reduced pressure, wash and dry to obtain modified ZSM-5;

[0042] (3) prepare phosphorus-modified ZSM-5: 5.5g triphenylphosphine, 14g toluene are added in the reactor, mechanical stirring is dissolved, and 1g potassium iodide aqueous solution, 10g modified ZSM-5 are added, and...

Embodiment 3

[0045] The preparation method of solid-phase catalyst comprises the following steps:

[0046] (1) Preparation of ZSM-5: add 100g of sodium silicate, 50g of sodium metaaluminate, and 20,000mL of deionized water into the reactor, stir evenly, add 60g of tetrapropylammonium bromide, stir evenly, add sulfuric acid to adjust pH , heated to 180°C, hydrothermally crystallized for 72h, washed with water, dried, and calcined in a muffle furnace to obtain ZSM-5;

[0047] (2) Preparation of modified ZSM-5: 105mL of N,N-dimethylformamide, 10g of ZSM-5, 10g of 2-bromopropionic acid, and 1500mL of dichloromethane were added to the reactor, stirred mechanically, and reacted at room temperature for 18h, Filter under reduced pressure, wash and dry to obtain modified ZSM-5;

[0048] (3) Preparation of phosphorus-modified ZSM-5: 6.5g of triphenylphosphine and 17g of toluene were added to the reactor, mechanically stirred to dissolve, 1.4g of potassium iodide aqueous solution and 10g of modified...

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Abstract

The invention discloses a method for recovering chloromethane from acid methanol tail gas, and relates to the technical field of chemical production, sodium silicate and sodium metaaluminate are used as raw materials to prepare a ZSM-5 molecular sieve, the ZSM-5 molecular sieve, 2-bromopropionic acid and triphenylphosphine are used as raw materials, surface groups of the ZSM-5 molecular sieve are modified to obtain phosphorus modified ZSM-5, and the phosphorus modified ZSM-5 is used as a catalyst for recovering chloromethane from acid methanol tail gas. And finally, preparing the solid-phase catalyst by taking the phosphorus-modified ZSM-5 and tetraethoxysilane as raw materials, thereby obtaining the solid-phase catalyst which takes the phosphorus-modified ZSM-5 as a core and silicon dioxide as a shell and has a core-shell structure. The solid-phase catalyst prepared by the invention is used in the process of recovering chloromethane from acid methanol tail gas, and has the advantages of difficulty in carbon deposition, high catalytic activity and the like.

Description

technical field [0001] The invention relates to the technical field of chemical production, in particular to a method for recovering methyl chloride from acid methanol tail gas. Background technique [0002] Acid methanol solution is a methanol solution of hydrogen chloride. It is a colorless or light yellow fuming liquid. The content of hydrogen chloride in industrial acid methanol solution is generally 20-35%. It can be used for acetal reaction to protect aldehyde groups, and it can also be used for anhydrous Reaction acid addition is a pharmaceutical intermediate and is widely used in the pharmaceutical industry. The acid methanol solution contains hydrogen chloride gas and methanol gas in the exhaust gas generated by a large amount of exothermic heat during the preparation process. [0003] Methyl chloride is a major raw material for the production of silicones. Polymer organosilicon compounds are widely used in electrical cables, textiles, papermaking and medicine due...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/16C07C19/03B01J29/40B01J31/02B01J33/00
CPCC07C17/16B01J29/40B01J33/00B01J31/0267B01J2229/34C07C19/03Y02P20/584
Inventor 雷忠裕方明光彭义霞马军汪志成王喜邵小苗吴兆平
Owner ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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