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Reaction system for continuously preparing polyoxymethylene dialkyl ether, and process thereof

A polymethoxydialkyl ether and reaction system technology, which is applied to chemical methods, chemical instruments and methods, ether preparation and other directions for reacting liquids with liquids, can solve problems such as low catalyst recovery rate, and achieve simple post-processing. , to achieve the effect of regeneration and recycling

Inactive Publication Date: 2014-05-07
LANZHOU 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

The process catalyst recovery rate is low

Method used

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  • Reaction system for continuously preparing polyoxymethylene dialkyl ether, and process thereof
  • Reaction system for continuously preparing polyoxymethylene dialkyl ether, and process thereof
  • Reaction system for continuously preparing polyoxymethylene dialkyl ether, and process thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0081] in the attached figure 1 In the shown reaction process, the volume of the reactor R1 is 1000mL, and the reactor R1 is connected to the heat exchanger in circulation, and the reaction liquid circulates between the reactor and the heat exchanger.

[0082] Purge with high-purity nitrogen to replace the system air. Add ionic liquid catalyst I in the flow reaction system, feed rate is 1.0g / h, until the catalyst starts to circulate, stop feeding, ensure that the catalyst concentration is not less than 4%; add the paraformaldehyde of purity 98.5wt%, purity 99% Methanol raw material reaction, the feeding rate is 15.0mL / h, 10.0mL / h respectively. The operating conditions of the reactor R1 are controlled at 115-120° C. and 2.5-3.5 MPa.

[0083] The reaction liquid is sent into the extraction tower V8, and the feed rate of the extractant benzene is 25mL / h. The heavy phase (catalyst aqueous solution) enters the film evaporator V12 continuously from the bottom of the tower, dehydr...

Embodiment 2

[0088] The basic process steps and equipment configuration are the same as in Example 1, except that the addition of ionic liquid II is a catalyst, and the feed rate is 0.6g / h. When the catalyst starts to circulate, the feed is stopped; the reaction raw material is 80wt% formaldehyde solution, purity 99% of the methanol raw material is reacted, the feed rates are 10.8mL / h and 5.8mL / h respectively, and the operating conditions of the reactor R1 are controlled at 125-130°C and 3.5-4.0MPa. The continuous acetalization reaction was carried out for 100 hours, and the results are listed in Table 2.

[0089] Table 2

[0090]

[0091] Note: Catalyst 13.3% is contained in the aqueous catalyst solution (14) after extraction.

Embodiment 3

[0093] The basic process steps, equipment configuration and parameters thereof are the same as those in Example 1, except that toluene is used as the extraction agent and the process is run continuously for 100 hours. 9.1mL / h DMM was obtained 3-8 Product (from line 21).

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Abstract

The invention discloses a process apparatus system for preparing polyoxymethylene dialkyl ether (RO(CH2O)nR, n=1-8) through a continuous acetalation reaction of formaldehyde and fatty alcohol under the catalysis of an acidic ionic liquid, and a process thereof. A process apparatus used in the method comprises an acetalation reaction unit, a product separation unit and a catalyst regeneration unit. The adoption of the extraction and rectification combined separation mode in the invention effectively realizes the separation of circulating materials and the above catalyst and makes the recovery rate of the catalyst reach above 99%; the separation of byproduct water from the reaction system is realized, and the azeotropy of water, alcohol, aldehyde and RO(CH2O)nR is destroyed, so the product separation is simple; and a catalyst regeneration technology is simple, so catalytic cycle is realized.

Description

technical field [0001] The present invention relates to a new reaction system and process method for continuously preparing polymethoxydialkyl ethers, more precisely, the present invention relates to a continuous acetalization of formaldehyde and fatty alcohol by using acidic ionic liquid as catalyst A new reaction system and process method for preparing polymethoxy dialkyl ether by reaction. Background technique [0002] Polymethoxy dialkyl ether (RO(CH 2 O) n R) is a new type of clean oil blending component with a high cetane number (H 3 CO(CH 2 O) 2 CH 3 : 63,H 3 CO(CH 2 O) 3 CH 3 : 78,H 3 CO(CH 2 O) 4 CH 3 : 90, H 3 CO(CH 2 O) 5 CH 3 : 100, H 5 C 2 O(CH 2 O) 2 C 2 h 5 : 77,H 5 C 2 O(CH 2 O) 3 C 2 h 5 : 89) and oxygen content (methyl series 42% ~ 49%, ethyl series 30% ~ 43%), adding 10% ~ 20% to diesel can significantly improve the combustion characteristics of diesel and effectively improve thermal efficiency , significantly reducing NO x a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/30C07C41/56
CPCC07C43/30B01J14/00C07C41/56C07C41/01C07C41/50C07C41/58Y02P20/584C07C43/303B01J19/2465B01J19/00C07C41/60
Inventor 陈静宋河远夏春谷康美荣靳荣华
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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