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In-tower pumping-type high vacuum distillation method and device for separation of heat sensitive oil

A heat-sensitive, high-vacuum technology, applied in the field of chemical mass transfer and separation, can solve the problems of inability to solve the problem of pressure drop in high-vacuum rectification towers, increase the production cost of heat-sensitive substances, and cannot control the vacuum degree of the tower kettle. The effect of damage, heating temperature reduction, and equipment cost reduction

Active Publication Date: 2016-08-10
天津领碳能源环保科技有限责任公司
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  • Application Information

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Problems solved by technology

[0005] 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 subsequent recovery of inhibitors and Whether the inhibitor pollutes the environment will increase the production cost of the 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

Method used

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  • In-tower pumping-type high vacuum distillation method and device for separation of heat sensitive oil
  • In-tower pumping-type high vacuum distillation method and device for separation of heat sensitive oil
  • In-tower pumping-type high vacuum distillation method and device for separation of heat sensitive oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] The raw material used in this example is waste rapeseed oil, and the acid value measured by the national standard GB-T5530-2005 method is 13.6mgKOH / g.

[0060] (1) Pretreatment of waste rapeseed oil, the specific steps are:

[0061](a) Take the ionic liquid [Bmim]Br-CuCl with a mass ratio of 1:2:34, waste rapeseed oil and methanol and add them together into a reaction vessel; place the reaction vessel in an oil bath at 50°C, and stir in the vessel Mix the liquid until the waste rapeseed oil and methanol fully react under the catalysis of the ionic liquid [Bmim]Br-CuCl to generate a variety of pretreatment products with an acid value less than 1;

[0062] (b) After the reaction is over, separate the ionic liquid and the pretreated product with an acid value less than 1 by decantation;

[0063] (c) After the isolated [Bmim]Br-CuCl ionic liquid is removed by rotary evaporation at 90°C to remove a small amount of methanol and water, it is recovered and reused; the obtained...

Embodiment 2

[0071] The raw material that this example adopts is the waste rapeseed oil of embodiment 1.

[0072] (1) Pretreatment of waste rapeseed oil, the specific steps are:

[0073] (a) Take H with a mass ratio of 1:3:27 2 SO 4 , waste rapeseed oil and methanol are added to the reaction vessel together; the reaction vessel is placed in an oil bath at 40°C, and the mixed solution in the container is stirred until the waste rapeseed oil and methanol are in the H 2 SO 4 Fully react under the catalysis to obtain the pretreatment product;

[0074] (b) After the reaction finishes, the pretreated product is separated from the mixture in the reaction vessel;

[0075] (c) Recycle the remaining substances in the reaction vessel after recovering a small amount of methanol and water by rotary evaporation at 90° C.;

[0076] (2) High-vacuum fine separation of the pretreatment product, the specific steps are:

[0077] (a) Put the pretreated product obtained in step 1 into the raw material tan...

Embodiment 3

[0083] The raw material used in this example is a certain waste palm oil, whose acid value is 10.1 mgKOH / g as measured by the national standard GB-T5530-2005 method.

[0084] (1) Pretreatment of waste palm oil, the specific steps are:

[0085] (a) Take the ionic liquid [BTBD]OH with a mass ratio of 1:6:20, waste palm oil and methanol and add them together to the reaction vessel; place the reaction vessel in an oil bath at 55°C, and stir the mixed solution in the vessel until Waste palm oil and methanol fully react under the catalysis of ionic liquid [BTBD]OH to form a pretreatment product with an acid value less than 1;

[0086] (b) After the reaction is over, separate the ionic liquid and the pretreated product with an acid value less than 1 by decantation;

[0087] (c) After the isolated [BTBD]OH ionic liquid was removed by rotary evaporation at 100°C to remove a small amount of methanol and water, it was recovered and reused; the acid value of the obtained pretreated produ...

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Abstract

The invention discloses an in-tower pumping-type high vacuum distillation method and device for separation of heat sensitive oil. The method uses oil rich in high added value heat sensitive material as the raw material, and uses acid, alkali or ionic liquid as a catalyst; the heat sensitive oil is pretreated to obtain a mixture of a plurality of fatty acid methyl esters; by in-tower pumping-type high vacuum technology effectively controls the pressure drop in the tower, so as to finely divide the mixture of the plurality of fatty acid methyl esters; the fatty acid methyl esters are respectively purified to obtain methyl stearate, methyl oleate, methyl linoleate, methyl linolenate, methyl arachidonate and erucic acid methyl ester single component heat sensitive material with mass percent higher than 98%. The method is energy-saving, simple for operation and easy for enlargement.

Description

technical field [0001] The invention belongs to the field of chemical mass transfer and separation, in particular to an in-tower pump-suction high-vacuum rectification method and device for separating heat-sensitive oil. Background technique [0002] Our country is rich in natural resources, and the output of freshwater fish in marine resources ranks among the top in the world. Therefore, a large amount of fish oil is produced in various production activities, and fish oil still contains a large amount of high value-added fatty acids, namely 20 carbon five Both EPA and DHA are essential nutrients for the human body. In addition to fish oil, cells such as seaweed oil, plant seeds, pulp, and corn germ are rich in oils. Some vegetable oils such as peanut oil and castor oil contain fatty acids of triglycerides in addition to general palmitic acid, stearic acid, oil In addition to linoleic acid, linoleic acid, linolenic acid, etc., there are sometimes special erucic acid, arachi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D3/14B01D3/10
CPCB01D3/106B01D3/14B01D2202/00
Inventor 丁辉齐金龙施民育徐世民
Owner 天津领碳能源环保科技有限责任公司
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