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Method for separating saturated fatty acid monoalkyl ester

A technology for alkyl esters and fatty acids, which is applied in the field of separation and production of saturated fatty acid monoalkyl esters, can solve the problems of high energy consumption for crystallization and solvent recovery, product purity needs to be improved, complicated operation process, etc. The effect of regular grain and high purity

Active Publication Date: 2020-05-08
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Lei Zhanlan (Development and application of fractionation of methyl palmitate, a by-product of tallow biodiesel [D]. Nanchang University, 2007.) Static crystallization and separation of saturated fatty acid methyl ester in tallow biodiesel in methanol or ethanol solvent, in When the mass ratio of biodiesel:ethanol is 1:2, a single crystallization can obtain a saturated fatty acid methyl ester product with a content of 91.4%, but this method requires a large amount of solvent and the purity of the product needs to be improved
[0006] CN 101747185 A puts biodiesel in a large amount of ethanol solvent to stand and crystallize, then washes the filter cake with mixed solvent for many times, can obtain high-purity saturated fatty acid methyl ester, but The method is complex in operation and requires a large amount of solvent
[0007] In summary, the existing technology uses a large amount of solvent, the energy consumption of crystallization and solvent recovery is high, and the purity of saturated fatty acid monoalkyl esters also needs to be improved, so it is urgent to develop low Low-cost, high-purity production method of saturated fatty acid monoalkyl ester

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach

[0029] According to one embodiment of the present invention, in step (3), the temperature of the cooling circulation medium is set to (T1-T3), and maintained at this temperature for (0.1-6) h, preferably (0.2-2) h. Wherein T3 is between 0-6, preferably between 0.5-3.

[0030] According to one embodiment of the present invention, in step (4), the temperature of the cooling circulation medium is set to (T1-T4)°C, and the crystallization is continued, wherein T4 is between 0.5-40, preferably 1-30, more preferably 2 ~20, and T4>T3; the temperature drop rate of the cooling cycle medium is (0.1~20)°C / h, preferably (0.5~10)°C / h, more preferably (1~5)°C / h. After cooling down to the set temperature, the crystallization time is maintained at 0-24 hours, preferably 0.5-6 hours, more preferably 0.5-2 hours.

[0031] After the crystallization is completed, the saturated fatty acid monoalkyl ester solid is obtained by filtration, and the saturated fatty acid monoalkyl ester product is obta...

Embodiment 1

[0036] The palm oil fatty acid methyl ester and ethanol with a mass ratio of 1.86:1 were added to the crystallizer, and the initial crystallization temperature T1 of the methyl ester solution was measured in advance as 19.8°C. Start stirring in the crystallizer, raise the temperature, and raise the temperature of the methyl ester solution to 25°C. After the palm oil fatty acid methyl ester is completely dissolved, reduce the temperature of the cooling circulation medium of the crystallizer to 18°C ​​at a cooling rate of 15°C / h , after the crystals appeared in the methyl ester solution, set the temperature of the circulating cooling medium at 18.5°C and maintain it for 1h, then lower the temperature of the circulating cooling medium to 12°C at a rate of 3°C / h, continue to crystallize for 0.5h, filter and collect As for the filter cake, the saturated fatty acid methyl ester was obtained after recovering the solvent, and the saturated fatty acid ester content was 94.37% as determi...

Embodiment 2

[0038] The palm oil fatty acid methyl ester and ethanol with a mass ratio of 1.86:1 were added to the crystallizer, and the initial crystallization temperature T1 of the methyl ester solution was measured in advance as 19.8°C. Start stirring in the crystallizer, raise the temperature, and raise the temperature of the methyl ester solution to 25°C. After the palm oil fatty acid methyl ester is completely dissolved, reduce the temperature of the cooling circulation medium of the crystallizer to 18°C ​​at a cooling rate of 15°C / h , after crystals appear in the methyl ester solution, set the temperature of the circulating cooling medium at 17.5°C and maintain it for 1 hour, then lower the temperature of the circulating cooling medium to 12°C at a rate of 3°C / h, continue to crystallize for 0.5h, filter and collect As for the filter cake, the saturated fatty acid methyl ester was obtained after recovering the solvent, and the saturated fatty acid ester content was 93.56% as determine...

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Abstract

The invention discloses a method for separating saturated fatty acid monoalkyl ester from mixed fatty acid monoalkyl ester. The method comprises the following steps: dissolving mixed fatty acid monoalkyl ester in a solvent, cooling to a certain temperature under a stirring condition, maintaining for a period of time, cooling to a certain temperature, maintaining for a certain time, filtering, andrecovering the solvent in the filtered solid to obtain a saturated fatty acid monoalkyl ester product. The method has the advantages of low solvent consumption, high saturated fatty acid monoalkyl ester content and the like.

Description

technical field [0001] The invention relates to a method for separating and producing saturated fatty acid monoalkyl esters from mixed fatty acid monoalkyl esters. Background technique [0002] Fatty acid monoalkyl ester refers to a fatty acid ester compound formed by combining one fatty acid group and one ester group. When the fatty acid group is derived from natural oils such as animal and vegetable oils and microbial oils, the carbon chain length is C8-C24; the ester group of C1-C4 is derived from monohydric alcohols, such as methanol and ethanol. The most common C8-C24 monoalkyl ester is fatty acid methyl ester, that is, biodiesel. [0003] Saturated fatty acid monoalkyl esters can produce a variety of oleochemicals, such as methyl chloride, butyl stearate, glyceryl stearate, stearate, etc. Fatty acid monoalkyl esters produced from natural oils are a mixture of saturated fatty acid esters and unsaturated fatty acid esters. The content of saturated fatty acid esters is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/48C07C69/24
CPCC07C67/48C07C69/24Y02E50/10
Inventor 曾建立杜泽学
Owner CHINA PETROLEUM & CHEM CORP
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