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 r

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0036] Example 1: Catalytic distillation of methanol dehydration to produce dimethyl ether

[0037] MCM-22 zeolite powder (SiO 2 / Al 2 O 3 For 26) mix with SB powder (a kind of pseudo-boehmite imported from Germany) at a ratio of 70:30 (dry basis weight) and appropriate amount of Sesbania powder, add appropriate amount of nitric acid and deionized water, and extrude into the product. To form a strip with a diameter of 1.6 mm, dry at 120°C for 2 hours, fire in a muffle furnace at 540°C for 3 hours, and then use 0.8M NH 4 NO 3 The aqueous solution was exchanged 3 times at 85°C, washed with deionized water 3 times, dried at 120°C for 4 hours, and calcined at 530°C for 2 hours, and then broken into 4-6 mm long strip catalysts for later use.

[0038] The catalytic distillation tower includes a condenser reflux at the top of the tower, a rectification section, a reaction section, a stripping section and a tower kettle. The inner diameter of the tower body is 25 mm, and the effective hei...

Example Embodiment

[0040] Example 2: Production of dimethyl ether by methanol dehydration in a fixed bed

[0041] The original beta zeolite powder (SiO 2 / Al 2 O 3 It is 30) and SB powder (a kind of pseudo-boehmite imported from Germany) at a ratio of 70:30 (dry basis weight) and an appropriate amount of sesame powder, add an appropriate amount of nitric acid and deionized water, and extrude into the shape. To form a strip with a diameter of 1.6 mm, dry at 120°C for 2 hours, fire in a muffle furnace at 540°C for 3 hours, and then use 0.8M NH 4 NO 3 The aqueous solution was exchanged 3 times at 85°C, washed with deionized water 3 times, dried at 120°C for 4 hours, and calcined at 530°C for 2 hours to break into 2 to 3 mm long particles.

[0042] 26 ml of the above catalyst was charged into a lower feed fixed bed reactor with an inner diameter of 15 mm, and after activation in a nitrogen stream at 250°C for 1 hour, the reaction of methanol dehydration to dimethyl ether was carried out.

[0043] Under ...

Example Embodiment

[0044] Example 3 Preparation of dimethyl ether by methanol dehydration in a fixed bed

[0045] The ZSM-5 zeolite powder (SiO 2 / Al 2 O 3 For 38) and SB powder (a kind of pseudo-boehmite imported from Germany) at a ratio of 80:20 (dry basis weight) and an appropriate amount of sesame powder, add an appropriate amount of nitric acid and deionized water, and extrude into the product. To form a strip with a diameter of 1.6 mm, dry at 120°C for 2 hours, fire in a muffle furnace at 540°C for 3 hours, and then use 0.8M NH 4 NO 3 The aqueous solution is exchanged 3 times at 90°C, washed with deionized water 3 times, dried at 120°C for 4 hours, and calcined at 550°C for 3 hours, and broken into 2 to 3 mm long particles.

[0046] 24 ml of the above catalyst was charged into a lower feed fixed bed reactor with an inner diameter of 15 mm, and after activation in a nitrogen stream at 250°C for 1 hour, the reaction of methanol dehydration to dimethyl ether was carried out.

[0047] Under the co...

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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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