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Method for preparing dimethyl ether from methanol

A technology for dimethyl ether and methanol, which is applied in the field of catalytic distillation for producing dimethyl ether from methanol dehydration, can solve the problems of reduced single-pass conversion rate, equipment corrosion, unfavorable catalyst stability, etc. Effect

Active Publication Date: 2007-02-07
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In the above inventions, the use of liquid acids such as sulfuric acid as catalysts will cause equipment corrosion and environmental pollution problems, and it is difficult to obtain high-purity dimethyl ether products by directly synthesizing dimethyl ether from synthesis gas
Using a solid acid catalyst to produce dimethyl ether from methanol gas-phase dehydration can obtain dimethyl ether with a purity of 99.9%, but the reaction temperature is relatively high, generally 200-380°C, and the single-pass conversion rate is about 70-80%, which has a great impact on the purity of methanol raw materials. There are also certain requirements. When the methanol reaction raw material has a high water content, it will inevitably lead to a decrease in the conversion rate per pass, and a high reaction temperature is not good for the stability of the catalyst.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Example 1: Dehydration of Methanol by Catalytic Distillation to Produce DME

[0037] MCM-22 zeolite raw powder (SiO 2 / Al 2 o 3 26) and SB powder (a kind of pseudo-boehmite imported from Germany) are uniformly mixed with an appropriate amount of kale powder in a ratio of 70:30 (dry basis weight), added an appropriate amount of nitric acid and deionized water, extruded into strips, and prepared into strips with a diameter of 1.6 mm, dried at 120°C for 2 hours, calcined in a muffle furnace at 540°C for 3 hours, and then treated with 0.8M NH 4 NO 3 The aqueous solution was exchanged three times at 85°C, washed three times with deionized water, dried at 120°C for 4 hours, calcined at 530°C for 2 hours, and broken into strip-shaped catalysts with a length of 4 to 6 mm for future use.

[0038] The catalytic distillation column includes a top condensation reflux device, a rectification section, a reaction section, a stripping section and a tower still. The inner diameter ...

Embodiment 2

[0040] Embodiment 2: Dehydration of fixed-bed methanol to produce dimethyl ether

[0041] Beta zeolite raw powder (SiO 2 / Al 2 o 3 30) and SB powder (a kind of pseudo-boehmite imported from Germany) are mixed evenly with an appropriate amount of kale powder in a ratio of 70:30 (dry basis weight), added an appropriate amount of nitric acid and deionized water, extruded into strips, and prepared into strips with a diameter of 1.6 mm, dried at 120°C for 2 hours, calcined in a muffle furnace at 540°C for 3 hours, and then treated with 0.8M NH 4 NO 3 The aqueous solution was exchanged three times at 85°C, washed three times with deionized water, dried at 120°C for 4 hours, calcined at 530°C for 2 hours, and broken into 2-3 mm long particles.

[0042] 26 milliliters of the above-mentioned catalysts were loaded into a bottom-feeding fixed-bed reactor with an inner diameter of 15 mm, and after activation for 1 hour at 250° C. in a nitrogen stream, the reaction of methanol dehydrat...

Embodiment 3

[0044] Example 3 Dehydration of fixed-bed methanol to produce dimethyl ether

[0045] The ZSM-5 zeolite raw powder (SiO 2 / Al 2 o 3 38) and SB powder (a kind of pseudo-boehmite imported from Germany) are uniformly mixed with an appropriate amount of kale powder in a ratio of 80:20 (dry basis weight), added an appropriate amount of nitric acid and deionized water, and extruded into strips to produce into strips with a diameter of 1.6 mm, dried at 120°C for 2 hours, calcined in a muffle furnace at 540°C for 3 hours, and then treated with 0.8M NH 4 NO 3 The aqueous solution was exchanged 3 times at 90°C, washed 3 times with deionized water, dried at 120°C for 4 hours, calcined at 550°C for 3 hours, and broken into 2-3 mm long particles.

[0046] 24 milliliters of the above-mentioned catalysts were loaded into a bottom-feeding fixed-bed reactor with an inner diameter of 15 mm, activated in nitrogen flow at 250° C. for 1 hour, and the reaction of methanol dehydration to dimethy...

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PUM

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Abstract

This invention relates to a preparation method for dimethyl ether by dehydrating methanol under liquid phase or gas-liquid mixing state in a catalytic distillation tower loaded with a solid acid catalyst in reaction section, wherein the methanol has a content of 5~99.99 wt.%. Catalytic distillation tower operating conditions include pressure of 0.6~5.0 MPa, column top temperature of 30~124DEG C, reaction section central temperature of 120~220DEG C, column reactor temperature of 160~270DEG C, the reflux ratio at 3~50, and feed volume space velocity of 0.1-10 ml methanol / ml catalyst, Or the reactions are carried out in one fixed bed rector or 2~4 fixed bed reactors in series with reaction conditions of temperature 120~220DEG C, pressure 0.6~8.0 MPa, and feed volume space velocity 0.1-10 ml methanol / ml catalyst.

Description

technical field [0001] The invention relates to a method for producing dimethyl ether from methanol, specifically, in the presence of a solid acid catalyst, dehydrating methanol in a liquid phase or in a gas-liquid mixed state to produce dimethyl ether, in particular to A catalytic distillation method for producing dimethyl ether from methanol dehydration. Background technique [0002] Chinese patent CN 1036199A discloses a method for producing dimethyl ether from methanol. Methanol vapor is dehydrated on a γ-alumina catalyst containing a small amount of silicon dioxide, and the dehydrated product is sent to a rectification tower for rectification. Pure dimethyl ether Ether and impurities are withdrawn as side products on certain trays of the tower. [0003] Chinese patent CN 1125216 discloses a method for producing dimethyl ether from methanol. After methanol with a content of 72-99.9% is removed from high boilers and impurities in a gasification separation tower, gas-phas...

Claims

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Application Information

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IPC IPC(8): C07C43/04C07C41/09
CPCC07C41/09Y02P20/10C07C43/043
Inventor 刘中民孙新德许磊孟霜鹤朱书魁吕志辉
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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