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Preparation method of durable and stable titanium silicalite molecular sieve catalyst for producing 2-nitropropane

A technology of titanium-silicon molecular sieve and nitropropane, applied in molecular sieve catalysts, catalyst activation/preparation, molecular sieve compounds, etc., can solve the problems of poor durability and service life, high deactivation rate, etc., to improve diffusion problems and increase efficiency , Optimizing the effect of pressure and temperature

Active Publication Date: 2021-04-09
宁波四明化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to improve the problems of high deactivation rate, poor durability and service life of titanium-silicon molecular sieve catalysts, the application provides a method for preparing durable and stable titanium-silicon molecular sieve catalysts for the production of 2-nitropropane, including the following preparation steps: S1 1. Taking wood pulp as a raw material, after being modified by acidolysis solution, collecting the acidolysis modified fiber and dissolving it into the solution to prepare a cellulose solution; S2, taking the cellulose solution prepared in step S1 and adding it dropwise to the regeneration solution , forming and collecting the cellulose microsphere template; S3, taking the cellulose solution and vacuum defoaming, vacuum cooling and placing it in a tubular atmosphere furnace, calcining and collecting the matrix carbon airgel template; S4, Take tetraethyl orthosilicate, water, cellulose microsphere template and matrix carbon airgel template, put them in a blender, stir and mix, collect the mixed solution, add tetrabutyl titanate dropwise to the mixed solution, stir and mix and concentrate , collect the concentrated mixed solution and crystallize it, filter and collect the filter cake; S5, wash the filter cake to remove the cellulose microsphere template, and after roasting and forming, collect the roasted blank and calcinate it in a muffle furnace to remove matrix carbon gas Gel template, standing and cooling to room temperature, can prepare durable and stable titanium silicate molecular sieve catalyst for the production of 2-nitropropane

Method used

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  • Preparation method of durable and stable titanium silicalite molecular sieve catalyst for producing 2-nitropropane
  • Preparation method of durable and stable titanium silicalite molecular sieve catalyst for producing 2-nitropropane

Examples

Experimental program
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Effect test

Embodiment 1

[0033] S1. Take the wood pulp and place it in the acid hydrolysis solution, heat and stir it at 70°C for 3 hours, collect the reaction solution and filter to obtain the filter cake, wash it with deionized water until the washing solution is neutral, then collect the acid hydrolysis solution Modified material, described acidolysis liquid is the hydrochloric acid ethanol solution mixed by mass ratio 1:20, and described hydrochloric acid concentration is 0.5mol / L, and described ethanol is the ethanol solution of mass concentration 75%; In parts by weight, Weigh 45 parts of deionized water, 1 part of 0.8 mol / L sodium hydroxide solution, 3 parts of urea and 15 parts of acid hydrolyzed modified materials and place them in a Erlenmeyer flask, stir to mix and collect the cellulose solution.

[0034] S2. According to the mass ratio of 1:50:100, the cellulose solution, 1-allyl-3-methylimidazolium chloride salt and absolute ethanol were stirred and mixed and added dropwise to the regenera...

Embodiment 2

[0039] S1. Take the wood pulp pulp and place it in the acid hydrolysis solution, heat and stir it at 75°C for 4 hours, collect the reaction solution and filter to obtain the filter cake, wash it with deionized water until the washing solution is neutral, then collect the acid hydrolysis solution Modified material, described acidolysis liquid is the hydrochloric acid ethanol solution mixed by mass ratio 1:20, and described hydrochloric acid concentration is 0.7mol / L, and described ethanol is the ethanol solution of mass concentration 77%; In parts by weight, Weigh 47 parts of deionized water, 1 part of 0.8 mol / L sodium hydroxide solution, 4 parts of urea and 17 parts of acid hydrolyzed modified materials and put them into Erlenmeyer flask, stir and mix and collect the cellulose solution.

[0040] S2. According to the mass ratio of 1:50:100, the cellulose solution, 1-allyl-3-methylimidazolium chloride salt and absolute ethanol were stirred and mixed and added dropwise to the rege...

Embodiment 3

[0045] S1. Take the wood pulp pulp and place it in the acid hydrolysis solution, heat and stir it at 80°C for 5 hours, collect the reaction solution and filter to obtain the filter cake, wash it with deionized water until the washing solution is neutral, then collect the acid hydrolysis solution Modified material, described acidolysis liquid is the hydrochloric acid ethanol solution mixed by mass ratio 1:20, and described hydrochloric acid concentration is 0.8mol / L, and described ethanol is the ethanol solution of mass concentration 80%; By weight parts, Weigh 50 parts of deionized water, 2 parts of 0.8 mol / L sodium hydroxide solution, 5 parts of urea and 15 parts of acid-hydrolyzed modified materials and place them in a Erlenmeyer flask, stir and mix and collect the cellulose solution.

[0046] S2. According to the mass ratio of 1:50:100, the cellulose solution, 1-allyl-3-methylimidazolium chloride salt and absolute ethanol were stirred and mixed and added dropwise to the rege...

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Abstract

The invention relates to the field of chemical materials, and particularly discloses a preparation method of a durable and stable titanium silicalite molecular sieve catalyst for producing 2-nitropropane. The durable and stable titanium silicalite molecular sieve catalyst is prepared by the following steps: S1, taking wood pulp as a raw material, carrying out acidolysis modification and dissolving treatment to prepare a cellulose solution; S2, dropwise adding the cellulose solution serving as a main raw material into regenerated liquid to prepare a cellulose microsphere template; S3, calcining the cellulose solution to obtain a matrix carbon aerogel template; S4, preparing a catalyst material by using the cellulose microsphere template and the matrix carbon aerogel template; and S5, respectively removing the cellulose microsphere template and the matrix carbon aerogel template to prepare the durable and stable titanium silicalite molecular sieve catalyst for producing 2-nitropropane. According to the durable and stable titanium silicalite molecular sieve catalyst, the catalyst deactivation phenomenon caused by pore channel blockage is improved, the service life of the catalyst is prolonged, and the durability of a catalyst material is improved.

Description

technical field [0001] The application relates to the field of chemical materials, more specifically, it relates to a preparation method of a durable and stable titanium-silicon molecular sieve catalyst for the production of 2-nitropropane. Background technique [0002] 2-Nitropropane is an important solvent and pharmaceutical intermediate. It is often used in the synthesis of chloronitroalkane pesticides. The 2-amino-2-methyl-1-propanol obtained by its reduction is also a very important surfactant group. Therefore, how to produce high-purity and high-yield 2-nitropropane has become the main research direction of 2-nitropropane preparation. Among them, acetone is used as raw material, and the purity and yield can be produced during the catalytic reaction process of the catalyst. Higher rate of 2-nitropropane, so catalysts are often used to produce 2-nitropropane now. In the catalytic reaction used to produce 2-nitropropane from acetone, catalysts are essential in this type o...

Claims

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Application Information

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IPC IPC(8): C01B37/06C01B39/08B01J29/89B01J35/10B01J37/00B01J37/08
CPCC01B37/065C01B39/085B01J29/89B01J37/0018C01P2006/12C01P2006/14B01J35/617B01J35/635Y02P20/584
Inventor 俞阳晨陶彬彬柳圣境
Owner 宁波四明化工有限公司
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