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Catalyst for dimethyl ether preparation through low-temperature methanol dehydration and preparation method as well as applications thereof

A low-temperature methanol and catalyst technology, applied in the field of catalysts for dimethyl ether synthesis, can solve the problems of unsatisfactory high temperature resistance performance and activity of the catalyst, insufficient ability of the catalyst to process raw materials, and inability to better conform to green chemical industry, etc. Environmental friendliness and economy, easy to obtain preparation method, good environment, good low temperature reaction effect

Active Publication Date: 2013-03-13
ENN XINNENG BEIJING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Such harsh conditions undoubtedly increase the difficulty of material selection and increase the cost of catalysts, which cannot better meet the concept of green chemical industry
In addition, the high temperature resistance and activity of the catalyst prepared by this patented technology are still not ideal, and the ability of the catalyst to process raw materials is not high enough
[0008] In the prior art, there is also AlCl 3 A report on the preparation of solid superacid catalyst supported on ion exchange resin [Li Pengfei, Loading AlCl on ion exchange resin 3 The development of solid superacid catalyst, Fine Petrochemical Industry, 1993 (1)], but the Al content in the prepared catalyst is far lower than the theoretical complexing amount of aluminum, and the catalytic activity is still not high

Method used

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  • Catalyst for dimethyl ether preparation through low-temperature methanol dehydration and preparation method as well as applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] 1. Preparation of macroporous sulfonic acid cation exchange resin

[0041]a. Polymerization: In a 2L stainless steel polymerization kettle, add 1200g of water and 2.5g of polyvinyl alcohol, heat and stir to completely dissolve the additives in the kettle. Heat up to 60°C, add 180g styrene (styrene content ≥ 99%), 130g divinylbenzene (divinylbenzene content 50%), 120g32 # White oil, an organic phase mixture composed of 2.6 g of benzoyl peroxide, stirred and heated to 86° C., and reacted at a constant temperature for 10 hours. The reaction product was filtered and dried at room temperature (moisture content ≤ 3%) to obtain 400 g of dry polymer white balls, of which 85.2% were polymers with particle sizes ranging from 0.3 mm to 1.0 mm.

[0042] b. Purification of pore structure: Take 100 g of dry white balls with a particle size of 0.3 mm to 1.0 mm and place them in a Soxhlet extractor. Extract for 2.5 hours. Then move the white ball into another 1000mL flask, add 500mL...

Embodiment 2

[0060] 1. During the preparation of the resin catalyst, the steps of polymerization, pore structure purification, sulfonation, filtration and drying are the same as those in Example 1.

[0061] 2. Fluorination of macroporous sulfonic acid resin:

[0062] 1) Load the dried macroporous sulfonic acid resin into the exchange column replaced by nitrogen, and pass through the fluorine-nitrogen mixed gas with a fluorine content of 7%, and the space velocity of the fluorine-nitrogen mixed gas is 20h -1 , the ventilation time is 15h;

[0063] 2) Replace the exchange column with nitrogen again after fluorination.

[0064] 3. Complexation loading AlCl on the fluorinated macroporous sulfonic acid resin 3 The steps are the same as in Example 1.

[0065] Through the above steps, the target catalyst R2 is finally obtained. Catalyst specific surface area (determined by BET method), pore volume and pore diameter are respectively: 39.01m 2 / g, 0.44mL / g, 45.12nm. The weight percent content...

Embodiment 3

[0069] 1. During the preparation of the resin catalyst, the steps of polymerization, pore structure purification, sulfonation, filtration and drying are the same as those in Example 1.

[0070] 2. The fluorination step of the macroporous sulfonic acid resin is the same as in Example 1.

[0071] 3. Complexation loading AlCl on the fluorinated macroporous sulfonic acid resin 3 : Add 100g of fluorinated resin, 160g of absolute ethanol and 4.5g of anhydrous aluminum chloride into a three-necked flask, stir and control the reaction temperature to 78°C with a constant temperature water bath, and the reaction time is 4.5h.

[0072] Through the above steps, the target catalyst R3 is finally obtained. Catalyst specific surface area (determined by BET method), pore volume and pore diameter are: 39.25m 2 / g, 0.44mL / g, 44.84nm. The weight percent content of aluminum in the catalyst is 2.86%.

[0073] The application mode of catalyst is consistent with embodiment 1.

[0074] It was de...

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Abstract

The invention provides a catalyst for dimethyl ether preparation through low-temperature methanol dehydration and a preparation method as well as applications thereof. The catalyst is a modified macroporous temperature resistance sulfoacid cation exchange resin; and a general macroporous sulfoacid cation exchange resin is prepared or purchased, and subjected to fluorine substitution, complexation of a load AlCl3 and the like to obtain the target catalyst. The preparation method is characterized in that before fluorination, electron withdrawing groups do not need to be introduced to benzene rings of the macroporous sulfoacid cation exchange resin, and therefore, the catalyst is easy in availability of raw materials and environment-friendly; the fluorated macroporous resin catalyst has a good temperature resistance; and a solid superacid catalyst is obtained after the fluorated macroporous resin is subjected to complexation of AlCl3 and substitution, and has a good reaction activity on the dimethyl ether preparation through methanol dehydration at a low temperature, so that the yield of dimethyl ether is high, and the handling capacity of a reaction raw material is great.

Description

technical field [0001] The invention relates to the field of catalysts for synthesizing dimethyl ether, in particular to a macroporous temperature-resistant sulfonic acid cation exchange resin catalyst used for low-temperature methanol dehydration, as well as its preparation method and application. Background technique [0002] Dimethyl ether is a widely used ether in the chemical industry. It has the characteristics of non-toxicity, safety, and high calorific value. It can be used as rocket propellant, diesel engine fuel, and civil fuel. It is also an intermediate of coal-based liquid fuel. At the same time, it is also an important basic chemical intermediate, which has a wide range of uses in pharmaceuticals, pesticides, dyes, and daily chemicals. [0003] The initial production of dimethyl ether uses concentrated sulfuric acid as a dehydration catalyst. This method has relatively large environmental pollution and serious corrosion of equipment. The traditional production...

Claims

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Application Information

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IPC IPC(8): B01J31/26C07C41/09C07C43/04
Inventor 史立杰李晨佳马超段妮丽
Owner ENN XINNENG BEIJING TECH
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