Intra-tower pump suction type high vacuum distillation method and device for precise separation of C16-C22 fatty acids

A technology for precision separation and fatty acid, which is applied in the field of pump-suction high vacuum rectification in the tower, which can solve the problem of hindering the research and application of high-purity fatty acid methyl ester, can not solve the problem of pressure drop in high vacuum rectification tower, and increase the production cost of heat-sensitive substances and other problems, to achieve the effect of lower heating temperature, lower equipment cost, and shorter residence time

Active Publication Date: 2016-06-22
TIANJIN UNIV
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Problems solved by technology

[0006] But for the first method, although the addition of inhibitors can improve the product purity of heat-sensitive substances to a certain extent and slow down the rate of deterioration of heat-sensitive substances during production, the addition of inhibitors not only increases the cost, but also the follow-up recovery of inhibitors and Whether the inhibitor pollutes the environment will increase the production cost of separation and purification of heat-sensitive substances; for the second method, the existing technology can improve the vacuum degree of the corresponding rectification column tower top, but the vacuum degree of the tower still cannot be controlled, and to obtain For heat-sensitive substances with high purity and high yield, the height of the rectification tower needs to be increased accordingly, while the vacuum degree of the tower kettle will decrease accordingly, and the temperature of the tower kettle will increase accordingly, and the heat-sensitive substances will be in danger of deterioration at this time
Therefore, in this case, in order to increase the vacuum degree of the tower reactor, multi-tower series operation is often used to reduce the temperature of the tower reactor and increase the vacuum degree of the tower reactor, but the equipment cost will increase accordingly, and huge energy consumption will be generated.
In addition, another technique to increase the vacuum degree of the rectification tower is to add a pressure regulator inside the rectification tower to reduce the pressure drop, but the pressure regulator in the rectification tower has a small compression ratio due to the structure of its fan blades , it has a certain effect at a lower vacuum degree. As the vacuum degree increases, the pressure regulating effect of the fan blades gradually loses, so it cannot solve the problem of high vacuum rectification tower pressure drop
Due to the small resistance of molecular distillation, substances can be separated under extremely high vacuum conditions. Therefore, molecular distillation can also be used to purify heat-sensitive substances, but molecular distillation only has the separation efficiency of a single-stage tray, and it is still not possible. to efficient separation
[0007] In summary, methyl eicosapentaenoate and methyl docosahexaenoate or methyl stearate, methyl oleate and methyl linoleate are completely separated to obtain a single The technology of fatty acid methyl ester is rarely reported, which seriously hinders the further research and application of high-purity fatty acid methyl ester

Method used

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  • Intra-tower pump suction type high vacuum distillation method and device for precise separation of C16-C22 fatty acids
  • Intra-tower pump suction type high vacuum distillation method and device for precise separation of C16-C22 fatty acids
  • Intra-tower pump suction type high vacuum distillation method and device for precise separation of C16-C22 fatty acids

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] The raw material used in this example is a high acid value vegetable oil, and the acid value is 23.6 mgKOH / g as determined by the national standard GB-T5530-2005 method.

[0064] (1) Pretreatment of vegetable oil, the specific steps are:

[0065] (a) Take the ionic liquid [Bmim]Br-CuCl, vegetable oil and methanol with a mass ratio of 1:2:34 into the reaction vessel; place the reaction vessel in a 50°C water bath, and stir the mixture in the vessel until Vegetable oil and methanol fully react under the catalysis of ionic liquid [Bmim]Br-CuCl to produce a mixture of fatty acid methyl esters with an acid value of less than 1;

[0066] (b) After the reaction, the ionic liquid and the mixture of fatty acid methyl esters with an acid value of less than 1 are separated by decantation, and the mixture of fatty acid methyl esters is biodiesel;

[0067] (c) Rotary evaporate the separated [Bmim]Br-CuCl ionic liquid at 90°C to remove a small amount of methanol and water, and then recycle i...

Embodiment 2

[0075] The raw material used in this example is a certain high acid value vegetable oil of Example 1.

[0076] (1) Pretreatment of vegetable oil, the specific steps are:

[0077] (a) Take CaO, vegetable oil and methanol with a mass ratio of 1:2:28 into the reaction vessel; place the reaction vessel in a 100°C water bath, and stir the mixture in the vessel until the vegetable oil and methanol are catalyzed by CaO Fully react to obtain a mixture of fatty acid methyl esters;

[0078] (b) After the reaction, the pretreatment products of various fatty acid methyl ester mixtures are separated from the mixture in the reaction vessel, and the multiple fatty acid methyl ester mixtures are biodiesel;

[0079] (c) The remaining material in the reaction vessel is rotary evaporated at 100° C. to recover a small amount of methanol and water, and then recover and treat.

[0080] (2) High vacuum fine separation of C16~C18 fatty acid methyl esters, the specific steps are:

[0081] (a) Take the mixture o...

Embodiment 3

[0087] The raw material used in this example is a certain waste corn oil, and the acid value is 10.1 mgKOH / g determined by the national standard GB-T5530-2005 method.

[0088] (1) Pretreatment of waste corn oil, the specific steps are:

[0089] (a) Take the ionic liquid [BTBD]OH with a mass ratio of 1:6:20, waste corn oil, and methanol into the reaction vessel; place the reaction vessel in a 55°C water bath, and stir the mixture in the vessel until Vegetable oil and methanol fully react under the catalysis of ionic liquid [BTBD]OH to produce a mixture of fatty acid methyl esters with an acid value of less than 1.

[0090] (b) After the reaction, the ionic liquid and the mixture of fatty acid methyl esters with an acid value of less than 1 are separated by decantation, and the mixture of fatty acid methyl esters is biodiesel;

[0091] (c) The separated [BTBD]OH ionic liquid is rotary evaporated at 100℃ to remove a small amount of methanol and water, and then recycled and reused; the ac...

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Abstract

The invention discloses an intra-tower pump suction type high vacuum distillation method and device for precise separation of C16-C22 fatty acids. The high vacuum distillation method comprises the following steps: firstly taking heat sensitive materials with a high additional value, such as animal and vegetable oil, as raw materials, adopting plasma liquid and the like as an esterification and transesterification catalyst, and obtaining mixture of multiple fatty acid methyl esters with high yield in one step; secondly, in a distillation tower with almost zero pressure drop, carrying out high vacuum distillation operation on the formed multiple fatty acid methyl esters through catalysis; and finally separating and purifying, so that single fatty acid methyl esters such as timnodonic acid methyl ester, docosahexoenoic acid methyl ester, methyl palmitate, methyl stearate, methyl oleate and methyl linoleate with the mass fraction more than 98% respectively are obtained. The whole technological method is simple and clear, the operation is simple, the equipment cost is low, the energy is saved, and the enlargement can be easily realized.

Description

Technical field [0001] The invention relates to the field of chemical mass transfer and separation, in particular to an in-tower pump suction high vacuum rectification method and device for precise separation of C16-C22 series fatty acids. Background technique [0002] China is rich in marine resources, and the output of freshwater fish is among the highest in the world. Therefore, the amount of fish oil produced in various production activities is huge, and fish oil still contains a large amount of high value-added fatty acids, namely eicosapentaenoic acid. (EPA) and docosahexaenoic acid (DHA), both of which are important nutrients indispensable to the human body. Among them, eicosapentaenoic acid can effectively help reduce the content of cholesterol and triglycerides, and promote Saturated fatty acid metabolism in the body reduces blood viscosity, improves blood circulation, improves tissue oxygen supply and relieves fatigue; for docosahexaenoic acid, it plays an important rol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C11C1/10B01D3/10B01D3/14B01D3/32B01D3/42C07C69/003C07C67/54
CPCB01D3/10B01D3/106B01D3/143B01D3/32B01D3/322B01D3/4205C11C1/007C11C1/10C07C67/54C07C69/003Y02P20/10
Inventor 丁辉齐金龙施民育徐世民
Owner TIANJIN UNIV
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