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Preparation method of catalyst for directly synthesizing dimethyl ether from synthesis gas

A catalyst and synthesis gas technology, applied in the direction of ether preparation, molecular sieve catalyst, chemical instruments and methods, etc., can solve the problems of poor catalyst activity, low solubility of oxalic acid, complicated preparation process, etc., and achieve easy automation, good selectivity, and simple process Effect

Inactive Publication Date: 2015-05-27
CHIA TAI ENERGY MATERIALS DALIAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalyst activity of mechanical mixing is poor, and the coprecipitation method introduces Na + ions, need multiple washes, complex preparation process, poor reproducibility
Gel impregnation method, using anhydrous ethanol, n-propanol or isopropanol as solvent, the solubility of oxalic acid in ethanol or propanol is low, the amount of alcohol is high, the precipitate needs to be filtered and washed with alcohol, and then dried, the process is complicated and costly high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Weigh 13.6 grams of copper nitrate, 6.7 grams of zinc nitrate, and 4.2 grams of aluminum nitrate, and dissolve them in 60 mL of anhydrous methanol, which is the raw material solution A.

[0027] Add 1.7 g of HY molecular sieves to the raw material solution A, and stir to form the raw material solution B.

[0028] 9.5 g of oxalic acid was dissolved in 70 mL of anhydrous methanol to form a transparent solution, which was the raw material solution C.

[0029] Add the raw material liquid C to the raw material liquid B to form a light blue suspension, add 1.5 grams of silica sol (mass solid content 30%), stir and mix, pour it into a rotary evaporation bottle, and vacuum rotary evaporation to dryness, anhydrous Methanol was recovered by condensation, and the dried solid was ground into a powder and calcined at 350°C for 4 hours.

[0030] Take 9.000 grams of calcined powder and 0.009 grams of graphite, grind and mix, extrude and shape by extrusion molding machine to obtain 20...

Embodiment 2

[0032] Weigh 14.3 grams of copper sulfate, 7.1 grams of zinc sulfate, and 5.5 grams of aluminum sulfate, and dissolve them in 60 mL of anhydrous ethanol to obtain raw material solution A.

[0033] Add 6.7 grams of α-Al to the raw material solution A 2 O 3 , stirring to form raw material liquid B

[0034] 12.9 g of oxalic acid was dissolved in 70 mL of absolute ethanol to form a transparent solution, which was the raw material solution C.

[0035] Add the raw material liquid C to the raw material liquid B to form a light blue suspension, add 10 grams of aluminum sol (solid content 25%), stir and mix evenly, then pour it into a rotary evaporation bottle, and vacuum rotary evaporation to dryness. The hydroethanol was recovered by condensation, and the dried solid was ground into powder and calcined at 350°C for 4 hours.

[0036] 9.9 grams of the calcined powder was mixed with 5g of hydroxymethyl cellulose aqueous solution (2% by mass), dried, ground into powder, calcined at 30...

Embodiment 3

[0038] Weigh 8.4 grams of copper chloride, 4.5 grams of zinc chloride, and 1.1 grams of aluminum chloride, and dissolve them in 60 mL of anhydrous isopropanol to obtain raw material solution A.

[0039] 2.9 g of H-ZSM-5 molecular sieve (Si / Al=30) was added to the raw material liquid A, and the raw material liquid B was formed by stirring.

[0040] 9.2 g of oxalic acid was dissolved in 70 mL of anhydrous isopropanol to form a transparent solution, which was the raw material solution C.

[0041] Add the raw material liquid C to the raw material liquid B to form a light blue suspension, add 1.1 g of white carbon black, stir and mix evenly, then spray dry to obtain catalyst particles, the dried solid is ground into powder, and calcined at 350 ° C 4 hours.

[0042] 9.8 grams of calcined powder was mixed with 10 g of hydroxymethyl cellulose aqueous solution (2% by mass), dried, ground into powder, calcined at 300°C for 4 hours, and extruded by an extrusion molding machine to obtain...

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PUM

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Abstract

The present invention relates to a preparation method of a catalyst for directly synthesizing dimethyl ether from synthesis gas, wherein the problems of high catalyst synthesis cost and low dimethyl ether selectivity in the prior art are mainly solved through the preparation method of the present invention. According to the preparation method of the present invention, inorganic salts of Cu, Zn and Al are adopted as a methanol synthesis active component raw material, an HY molecular sieve, alpha-Al2O3, or an H-ZSM-5 molecular sieve is adopted as a methanol dehydration active component, a low carbon alcohol is adopted as a solvent, a silica sol, an alumina sol or white carbon black is adopted as a binder, a method selected from rotary evaporation, spray drying method and flash evaporation is adopted to dry, the obtained powder is calcined, then is added with graphite or cellulose ether and other processing aids, and is subjected to extrusion forming to prepare catalyst particles, and calcination is performed again so as to prepare the catalyst. According to the present invention, the catalyst production process is simple, the catalyst has characteristics of high activity, good selectivity, excellent activity at high space velocity, and high dimethyl ether time space yield, and the preparation method can be used for the industrial production of direct preparation of the dimethyl ether from the synthesis gas.

Description

technical field [0001] The invention relates to a preparation method of a catalyst for directly synthesizing dimethyl ether from synthesis gas. Background technique [0002] DME is a simple organic ether compound. It is a colorless gas with a slight fragrance under normal temperature and pressure. Currently, it is mainly used as spray paint, hair spray, air freshener and vehicle atomizer. In addition, DME is also a clean energy, which can be used as automobile and domestic fuel. DME fuel has the advantages of high efficiency, environmental friendliness, safe use and wide application, and has broad industrial prospects. [0003] At present, there are two-step and one-step methods for the production of dimethyl ether. The two-step process is to convert the syngas to methanol and then dehydrate the methanol to dimethyl ether. The one-step synthesis of dimethyl ether is a new technology developed in recent years, that is, a bifunctional catalyst is used, which includes methan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/46B01J29/14B01J23/80C07C43/04C07C41/09
Inventor 邓忠华吴宗斌徐燕刘禹李秀清
Owner CHIA TAI ENERGY MATERIALS DALIAN
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