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After-treatment technology of Beckmann gas-phase rearrangement S-1 full-silica molecular sieve based catalyst

An all-silicon molecular sieve, S-1 technology, used in molecular sieve catalysts, catalyst activation/preparation, physical/chemical process catalysts, etc. Problems such as small selection range, to achieve the effect of reducing energy consumption and saving equipment costs

Active Publication Date: 2013-08-14
CHINA TIANCHEN ENG +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problems in the prior art, the present invention provides a post-treatment process of Beckmann gas-phase rearrangement S-1 all-silicon molecular sieve catalyst, which solves the problems in the prior art that hydrofluoric acid is highly corrosive at high temperature and the selection range of heat exchanger materials is small , the problem of high cost of using high-cost Monel alloy heat exchanger

Method used

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  • After-treatment technology of Beckmann gas-phase rearrangement S-1 full-silica molecular sieve based catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Dilute hydrochloric acid with deionized water until the H+ concentration is 0.02 mol / l, add hydrofluoric acid with deionized water and dilute to 0.02% by mass fraction, and then mix the two solutions at a volume ratio of 1:3 for later use.

[0026] Weigh 40g of S-1 all-silicon molecular sieve catalyst and put it into a reactor made of polytetrafluoroethylene or polypropylene, measure 200ml of the mixed solution of strong acid and hydrofluoric acid and pour it into the reactor, start stirring, and the speed is 50r / min, react at room temperature for 2h, stop stirring, and wash with deionized water until neutral. Repeat this process 3 times. After the reaction is completed, the S-1 all-silicon molecular sieve is dried and calcined at 500°C for 3 hours to obtain the S-1 all-silicon molecular sieve catalyst product.

[0027] Table 1 shows the catalyst evaluation results for the gas-phase Beckmann rearrangement of S-1 all-silicon molecular sieve for the synthesis of caprolac...

Embodiment 2

[0029] Dilute sulfuric acid with deionized water to H + The concentration is 0.03 mol / l, and the hydrofluoric acid is added to deionized water to dilute to a mass fraction of 0.06%, and then the two solutions are mixed at a volume ratio of 1:2 for later use.

[0030] Weigh 60g of S-1 all-silicon molecular sieve catalyst and put it into a reactor made of polytetrafluoroethylene or polypropylene, measure 400ml of the mixed solution of strong acid and hydrofluoric acid and pour it into the reactor, start stirring, and the speed is 80r / min, react at room temperature for 3h, stop stirring, and wash with deionized water until neutral. Then, this reaction was repeated 3 times under the same conditions. After the reaction is completed, the S-1 all-silicon molecular sieve is dried and calcined at 550° C. for 4 hours to obtain the S-1 all-silicon molecular sieve catalyst product.

[0031] Table 1 shows the catalyst evaluation results for the gas-phase Beckmann rearrangement of S-1 all...

Embodiment 3

[0033] Dilute hydrochloric acid with deionized water to H + The concentration is 0.05 mol / l, adding deionized water to dilute hydrofluoric acid to a mass fraction of 0.1%, and then mixing the two solutions at a volume ratio of 1:1 for later use.

[0034]Weigh 80g of S-1 all-silicon molecular sieve catalyst and put it into a reactor made of polytetrafluoroethylene or polypropylene, measure 800ml of the mixed solution of strong acid and hydrofluoric acid and pour it into the reactor, start stirring, and the speed is 100r / min, react at room temperature for 4h, stop stirring, and wash with deionized water until neutral. Repeat this process 3 times. After the reaction is completed, the S-1 all-silicon molecular sieve is dried and calcined at 600°C for 5 hours to obtain the S-1 all-silicon molecular sieve catalyst product.

[0035] Table 1 shows the catalyst evaluation results for the gas-phase Beckmann rearrangement of S-1 all-silicon molecular sieve for the synthesis of caprolac...

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Abstract

The invention discloses an after-treatment technology of a Beckmann gas-phase rearrangement S-1 full-silica molecular sieve based catalyst, which comprises the following steps of: preparing a mixed solution of strong acid with a certain concentration and hydrofluoric acid in proportion, weighing a certain mass of S-1 full-silica molecular sieve based catalyst and putting into a reactor, measuringout the prepared mixed solution of strong acid and hydrofluoric acid based on the mass of the catalyst and pouring into the reactor, starting stirring, maintaining a certain rotation speed, stopping stirring after reacting for a period of time at room temperature, and washing by using de-ionized water to be neutral. According to the invention, By changing the formula of an S-1 full-silica molecular sieve after-treatment solution and using the mixed solution of strong acid and hydrofluoric acid as an after-treatment solution, the after treatment is carried out at room temperature dropping fromabout 100 DEG C in conventional processes, the problem that the material of a heat exchanger must be made of an expensive Monel metal due to strong corrosivity of the hydrofluoric acid in the conventional after-treatment process is solved, and equipment cost is substantially saved.

Description

technical field [0001] The invention belongs to the field of catalyst preparation, and relates to a new post-treatment process of S-1 all-silicon molecular sieve in caprolactam synthesized by Beckmann vapor phase rearrangement, more specifically, relates to a low-cost process for treating S-1 all-silicon molecular sieve. Background technique [0002] Caprolactam is an important chemical raw material and a monomer for the synthesis of nylon 6 and engineering plastics. Currently, there are two main processes for the synthesis of caprolactam, liquid-phase and gas-phase Beckmann rearrangement. At present, in industrial production, sulfuric acid is mainly used to catalyze the liquid phase rearrangement process. The process is that cyclohexanone oxime undergoes a Beckmann rearrangement reaction at a certain temperature under the action of concentrated sulfuric acid or oleum, and then uses ammonia to neutralize the acidity of the reaction system to generate caprolactam. The proce...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/035B01J37/00C07D223/10C07D201/04
Inventor 刘文张媛袁海鹏王绍伟钱震王志文宋辉王元平张蒙王海国刘俊生梁莹史文涛张舜光曹振岩孙世谦袁学民周明生
Owner CHINA TIANCHEN ENG
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