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A kind of refining method of di-isooctyl dodecanedioate

A technology of diisooctyl dodecanedioate and a refining method, which is applied in the preparation of carboxylate, separation/purification of carboxylate, chemical instruments and methods, etc., can solve the problem of reducing product yield, losing crude product, The acid value of the crude product is not ideally reduced, and the effect of reducing the acid value, improving the purity and yield, and shortening the standing and stratification time is achieved.

Active Publication Date: 2016-06-08
江苏兰博士新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

When the crude product of diisooctyl dodecanedioate was cleaned by the traditional alkaline washing process, it was found that the crude product and lye were easily emulsified, and the static delamination time was as little as 2 days, as long as 1 week, and the acid value of the crude product was not reduced. Ideal, but part of the crude product is also lost, reducing the product yield

Method used

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  • A kind of refining method of di-isooctyl dodecanedioate

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specific Embodiment approach

[0017] like figure 1 A specific embodiment of the refining process flow of a kind of dodecanedioic acid diisooctyl ester provided by the invention is shown, comprising the following steps:

[0018] A, with solid super acid SO 4 2- / ZrO 2 -TiO 2 As a catalyst, dodecanedioic acid and isooctyl alcohol are used to prepare a crude product of diisooctyl dodecanedioate, the acid value is 2-60 mgKOH / g, and the content is 65-85%;

[0019] B. Mix the organic solvent and the crude product from step A according to the volume ratio of (0.1-5.0): 1, and then stir with the lye solution with a mass concentration of 0.1-55.0%. Coarse product layer;

[0020] C. Under vacuum, control the temperature at 30-200° C., distill the crude product from step B under reduced pressure, remove excess isooctyl alcohol and organic solvent, and obtain high-purity diisooctyl dodecanedioate.

[0021] Preferably, the organic solvent described in step B of the present invention is any one or a combination of...

Embodiment 1

[0023] In a 250ml three-necked flask, sequentially add 50ml crude product of diisooctyl dodecanedioate, 50ml ethanol and 100ml saturated sodium bicarbonate solution, stir evenly, transfer to a 250ml separating funnel and let stand for 15min to separate the oil layer; Under negative pressure (-0.096)~(-0.099)MPa and 150℃, the crude product was distilled under reduced pressure for 30min, the acid value of the product decreased from 14.82mgKOH / g to 0.27mgKOH / g, and the ester content increased from 70.02% to 97.28% .

Embodiment 2

[0025] In a 250ml three-necked flask, sequentially add 50ml of crude diisooctyl dodecanedioate, 50ml of methanol and 50ml of sodium carbonate solution with a mass concentration of 5%, stir evenly, transfer to a 250ml separatory funnel and let stand for 20min, Separate the oil layer; under the negative pressure (-0.096)~(-0.099)MPa and 160℃, the crude product was distilled under reduced pressure for 25min, the acid value of the product decreased from 33.10mgKOH / g to 0.09mgKOH / g, and the ester content decreased from 70.67% increased to 98.35%.

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Abstract

The invention discloses a refining method for diisooctyl dodecanedioate. According to the refining method, an organic solvent is used for diluting a diisooctyl dodecanedioate crude product, and the mixture of the organic solvent and the diisooctyl dodecanedioate crude product is uniformly mixed with relatively mild alkali liquor, so that the phenomenon of emulsification of esters and the alkali liquor is relieved, the standing demixing time and the loss of the crude product are reduced, the acid value of a product is effectively reduced, and the purity and yield of the product are improved; a process and equipment are simple, the method is high in yield and suitable for industrial production, and the inorganic solvent can be recycled.

Description

technical field [0001] The invention relates to a method for purifying esters in the field of organic chemical industry, in particular to a method for purifying diisooctyl dodecanedioate. Background technique [0002] Diisooctyl dodecanedioate is a new type of ester synthetic base oil with high viscosity index, high flash point, low pour point, good low temperature fluidity, wider operating temperature range, small evaporation loss, high temperature stability It has the advantages of good properties, good oxidation stability, less carbon residue, excellent lubricating performance, extremely low toxicity, environmental protection and good biodegradability. At present, my country mainly relies on imports. Nowadays, the application field of ester synthetic oil has been expanded to precision instrumentation oil, synthetic compressor oil, automobile engine oil, marine engine oil, hydraulic oil, gear oil, metal processing oil and synthetic lubricating ester. It can also be used as...

Claims

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Application Information

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IPC IPC(8): C07C69/34C07C67/48C07C67/62
CPCC07C67/48C07C69/34
Inventor 姚明忠徐吉上胡锦猛
Owner 江苏兰博士新材料有限公司
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