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Method and equipment for continuous esterification production of adipic acid dimethyl ester

A technology of dimethyl adipate and adipic acid is applied in the field of continuous esterification to produce dimethyl adipate and equipment, and can solve problems such as pollution and corrosion

Active Publication Date: 2008-03-05
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a kind of method that adopts solid acid as catalyst, carries out continuous esterification to produce dimethyl adipate, overcomes the corrosion and pollution problem that the inorganic liquid acid catalyst of traditional esterification technology brings

Method used

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  • Method and equipment for continuous esterification production of adipic acid dimethyl ester

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Experimental program
Comparison scheme
Effect test

Embodiment 1-4

[0025] The used equipment of the inventive method comprises pre-esterification kettle (1), raw material tank (2), raw material pump (3), preheater (4), methanol tank (5), methanol pump (6), vaporizer (7), Continuous esterification tower (8), condenser (9), storage tank (10);

[0026] The pre-esterification kettle equipped with agitator is connected to the feed port of the raw material tank through the pipeline, the discharge port of the raw material tank is connected to the feed port of the raw material pump through the pipeline, and the discharge port of the raw material pump is connected to the pre-esterification tank through the pipeline. The feed port of the heater is connected, and the discharge port of the preheater is connected with the feed port on the upper part of the continuous esterification tower through a pipeline;

[0027] The methanol tank is connected to the inlet of the methanol pump through the pipeline, the outlet of the methanol pump is connected to the in...

Embodiment 5-6

[0037] Utilize the pre-esterification product of embodiment 1, 2 to carry out continuous esterification, normal pressure, under the condition of 70~150 ℃, liquid space velocity is 0.34 tons / Kg h, concrete result is as follows:

[0038] Table 3 Results of continuous esterification experiments with different methanol space velocities

[0039] liquid space velocity

Embodiment 7-8

[0041] Utilize the product of embodiment 3,4 pre-esterification to carry out continuous esterification, normal pressure, under the condition of 70~150 ℃, methanol space velocity is 0.37Kg / Kg h, concrete result is as follows:

[0042] Table 4 Different liquid space velocity continuous esterification experimental results

[0043] liquid space velocity

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Abstract

The present invention relates to continuous esterification process and apparatus for producing dimethyl adipate in the presence of solid acid catalyst. The process includes the following steps: setting solid acid catalyst, adipic acid and methanol into pre-esterifying kettle; heating to 50-100 deg.c to react at normal pressure to obtain lean ester; feeding the supernatant with lean ester to the upper part of one continuous esterifying tower and methanol vapor to its lower part for countrecurrent reaction in the catalyst section at the temperature of 70-150 deg.c, liquid space velocity of 0.1-0.7 kg / kg.hr and methanol space velocity of 0.1-1.0 kg / kg.hr; rectifying the resultant at operation pressure of 0-0.01 MPa to obtain dimethyl adipate. The present invention has adipic acid converting rate up to 99 % and dimethyl adipate purity up to 99.8 %.

Description

Technical field: [0001] The invention relates to a method and equipment for producing dimethyl adipate through continuous esterification using solid acid as a catalyst. Background technique: [0002] Dimethyl adipate is an excellent cold-resistant plasticizer, which can endow products with excellent low-temperature softness, and has certain light and heat stability and water resistance. Dimethyl adipate is also an intermediate in the synthesis of 1,6-hexanediol. [0003] The relevant literature report of the method for producing dimethyl adipate has: 1. Japanese patent (JP03115249), discloses acid and alcohol under higher pressure (0.25~2.5MPa) and higher temperature (150~350 ℃). And flow into the reactor from top to bottom. 2. British patent (GB143069), disclosed is a kind of comparatively original technological method, uses concentrated sulfuric acid as catalyzer, adopts the method for still reactor reactive distillation to remove water. Using sulfuric acid or other ino...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/44C07C67/08
Inventor 程光剑石鸣彦赵建国史君张元礼李凤鸣黄集钺李民任建平娄阳
Owner PETROCHINA CO LTD
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