Method and equipment for continuous esterification production of adipic acid dimethyl ester
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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: 2009-09-09
PETROCHINA CO LTD
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[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
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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
[0038] 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 0.34Kg / Kg h, concrete result is as follows:
[0039] Table 3 Experimental results of continuous esterification with different methanol space velocities
[0040] liquid space velocity
Embodiment 7-8
[0042] 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:
[0043] Table 4 Experimental results of continuous esterification with different liquid space velocities
[0044] liquid space velocity
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Abstract
The present invention relates to a method and equipment for producing dimethyl adipate through continuous esterification. A solid acid catalyst, adipic acid and methanol are added to a pre-esterification kettle; the pre-esterification reaction kettle is heated at a temperature of 50-100°C , react under normal pressure to obtain lean ester, the addition amount of solid acid catalyst is 1-10% of the mass of adipic acid, the molar ratio of methanol to adipic acid is 1-10, the solid acid catalyst is a strong acid type cation exchange resin; The supernatant liquid of the ester is sent to the upper part of the continuous esterification tower, and the methanol vaporized into steam enters the lower part of the continuous esterification tower, so that the two do a countercurrent reaction in the catalyst section of the continuous esterification tower, and the reaction temperature is 70 ~ 150°C, the liquid space velocity is 0.1-0.7Kg / Kg h, the methanol space velocity is 0.1-1.0Kg / Kg h; the obtained reactant is obtained by rectification to obtain dimethyl adipate, and the operating pressure is 0~ 0.01MPa; the conversion rate of adipic acid is 99%.
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...
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