Method for preparing para-xylene catalyst by amino-modified methanol

A technology of xylene catalyst and amino modification, which is applied in the direction of catalyst activation/preparation, catalyst, carbon compound catalyst, etc. It can solve the problems of uneven bed temperature, poor catalyst stability, easy deactivation, etc., and achieve improved surface properties and Effects of stability, increase in adsorption capacity, and increase in one-way yield

Active Publication Date: 2018-04-17
XUZHOU NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In industry, p-xylene is generally produced by separating aromatics from petroleum cracking products, disproportionating toluene, or transalkylating heavy aromatics. Because these methods produce a large amount of benzene by-product, and the economic value of benzene is low, it affects p-xylene to a certain extent. Economics of Toluene Preparation Process
The traditional method mostly adopts fixed bed technology, the bed temperature is not uniform, the catalyst is poor in stability, easy to deactivate and difficult to regenerate. value, so the cost is high; the preparation and modification steps of the catalyst are cumbersome and expensive

Method used

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  • Method for preparing para-xylene catalyst by amino-modified methanol

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Embodiment 1

[0017] A preparation method of an amino-modified methanol-based p-xylene catalyst, comprising the following steps:

[0018] Step 1. Freeze-dry 100g of COF-1 nanomaterials and pulverize them, place them in a tube furnace, blow nitrogen gas for 10min, flow rate is 0.5L / min, and rapidly raise the temperature to 350°C and keep the constant temperature for 5h to obtain a thermally expandable porous material;

[0019] Step 2, put the above COF-1 nanomaterials in 1mol / L dilute hydrochloric acid, stir at constant temperature, and filter to obtain a solid; take 100g of the solid, add a mixed solution of 50ml concentrated sulfuric acid and 50ml concentrated nitric acid in a volume ratio, and then mechanically stir for 4 hours , suction filtration,

[0020] wash and dry;

[0021] Step 3. Add the above-mentioned dried product into 25ml of ammonia water, mechanically stir for 15 minutes, add 25g of sodium dithionite, stir at a constant speed for 24 hours, filter with suction, wash and dry...

Embodiment 2

[0029] Step 4, take 20g amino-modified COF-1 nanomaterials, add 160ml containing 15gFeSO 4 ·7H 2 O and 5g PEG-4000 alcohol-water mixed system, in which the volume ratio of water and absolute ethanol is 1:2, pass high-purity nitrogen gas, stir at a constant speed, and add 30ml of KBH with a concentration of 0.5mol / L dropwise at the same time 4 solution, then continuously stirred for 20 min, and vacuum freeze-dried to obtain nano-iron-loaded amino-modified COF-1 catalyst. All the other steps are the same as in Example 1.

Embodiment 3

[0031] Step 4, take 10g amino-modified COF-1 nanomaterials, add 160ml containing 15gFeSO 4 ·7H 2 O and 5g PEG-4000 alcohol-water mixed system, in which the volume ratio of water and absolute ethanol is 1:2, pass high-purity nitrogen gas, stir at a constant speed, and add 30ml of KBH with a concentration of 0.5mol / L dropwise at the same time 4 solution, then continuously stirred for 20 min, and vacuum freeze-dried to obtain nano-iron-loaded amino-modified COF-1 catalyst. All the other steps are the same as in Example 1.

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Abstract

The invention discloses a method for preparing a para-xylene catalyst by amino-modified methanol. The method adopts dioxane, mesitylene, glacial acetic acid, COF-1 nano material, FeSO4.7H2O and KBH4 as main raw materials. The method disclosed by the invention has the beneficial effects that unique processes and technical parameters are adopted, loads are generated by thermal expansion, amino modification and nano-iron reaction, and by thermal-expansion treatment, the surface adhesiveness of COF-1 is improved, and basis is provided for the following amino modification; by amino modification, the surface property is improved and the benefit for fully and uniformly loading the nano-iron generated in reaction onto porous carriers is achieved; by alkylation reaction of methanol, para-xylene isobtained, so that the steps of isomerization and the like in the traditional process are omitted, the process route is shortened and the once-through yield of the para-xylene is greatly increased.

Description

technical field [0001] The invention relates to an amino-modified methanol-to-p-xylene catalyst and a preparation method thereof, belonging to the technical field of catalysts. Background technique [0002] P-xylene is an extremely important bulk chemical raw material, mainly used in the production of terephthalic acid and dimethyl terephthalate. Due to the rapid development of my country's polyester industry, the consumption of p-xylene has also increased rapidly. In industry, p-xylene is generally produced by separating aromatics from petroleum cracking products, disproportionating toluene, or transalkylating heavy aromatics. Because these methods produce a large amount of benzene by-product, and the economic value of benzene is low, it affects p-xylene to a certain extent. Economics of the toluene production process. The traditional method mostly adopts fixed bed technology, the bed temperature is not uniform, the catalyst is poor in stability, easy to deactivate and di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06C07C2/86C07C15/08
CPCB01J31/04B01J31/06B01J35/006B01J37/08B01J37/16C07C2/864C07C2531/06C07C15/08Y02P20/52
Inventor 高光珍
Owner XUZHOU NORMAL UNIVERSITY
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