CN111793046B - Method for rectifying and recovering tetrahydrofuran from industrial waste tetrahydrofuran - Google Patents
Method for rectifying and recovering tetrahydrofuran from industrial waste tetrahydrofuran Download PDFInfo
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- CN111793046B CN111793046B CN202010709392.4A CN202010709392A CN111793046B CN 111793046 B CN111793046 B CN 111793046B CN 202010709392 A CN202010709392 A CN 202010709392A CN 111793046 B CN111793046 B CN 111793046B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/04—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having no double bonds between ring members or between ring members and non-ring members
- C07D307/06—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having no double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to ring carbon atoms
- C07D307/08—Preparation of tetrahydrofuran
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Abstract
The invention belongs to the technical field of tetrahydrofuran recovery, and particularly relates to a method for rectifying and recovering tetrahydrofuran from industrial waste tetrahydrofuran, which comprises the steps of carrying out crude distillation on industrial waste tetrahydrofuran mother liquor to obtain a tetrahydrofuran crude product, then introducing inert gas, separating low-boiling-point substances through pressure rectification, and continuing pressurization to carry out rectification dehydration until tetrahydrofuran with the water content of less than 0.1% is obtained. The method effectively utilizes the low boiling point to remove most of water, avoids using other organic extracting agents for secondary recovery, reduces the cost, has simple and convenient operation and good product quality, and improves the product quality and the yield.
Description
Technical Field
The invention belongs to the technical field of tetrahydrofuran recovery, and particularly relates to a method for rectifying and recovering tetrahydrofuran from industrial waste tetrahydrofuran.
Background
Tetrahydrofuran, also known as 1, 4-oxirane or tetramethyleneoxide (abbreviated as Thr F), is a common organic solvent, has strong toxicity, can be poisoned by being inhaled by steam or being contacted with skin, has the explosion limit of 2.3-11.8 in air, can generate peroxide like diethyl ether, and is extremely easy to explode. Tetrahydrofuran is generally used to dissolve the organic material and react therein, without itself participating in the reaction. The product is separated after the reaction, and the residual tetrahydrofuran can not be used due to the impurity, which causes great economic loss and pollutes the environment if directly discarded. At present, the recovery and purification of tetrahydrofuran has great difficulty in purification due to extraction by using an extraction solvent and rectification, and no domestic report exists for directly recovering and extracting pure tetrahydrofuran from industrial waste tetrahydrofuran.
Disclosure of Invention
The invention aims to provide a method for recovering tetrahydrofuran from industrial waste tetrahydrofuran by rectification, which solves the problem that the existing recovery and purification of tetrahydrofuran is more difficult due to extraction by using an extraction solvent and rectification.
The realization process of the invention is as follows:
a method for rectifying and recovering tetrahydrofuran from industrial waste tetrahydrofuran comprises the steps of carrying out crude distillation on industrial waste tetrahydrofuran mother liquor to obtain a tetrahydrofuran crude product, then introducing inert gas, carrying out pressure rectification to separate low-boiling-point substances, and continuing pressurization to carry out rectification dehydration until tetrahydrofuran with the water content of less than 0.1% is obtained.
The method for rectifying and recovering tetrahydrofuran from industrial waste tetrahydrofuran specifically comprises the following steps:
(1) Crude tetrahydrofuran is obtained by crude distillation:
adding industrial waste tetrahydrofuran mother liquor into a rough distillation kettle, and heating and distilling to obtain a tetrahydrofuran crude product;
(2) Introducing inert gas to separate low-boiling-point raw materials:
introducing inert gas into a rectifying tower kettle, pumping the tetrahydrofuran crude product obtained in the step (1) into a rectifying tower, controlling the pressure in the kettle to be 0.1-0.6 MPa through pressurization, and heating, rectifying and separating a low-boiling-point raw material;
(3) Introducing inert gas for pressure dehydration:
continuously introducing inert gas into the rectifying tower kettle, controlling the pressure in the kettle to be 0.1-0.6 MPa, and heating, rectifying and dehydrating to obtain tetrahydrofuran mixed liquor with the water content of less than 6%;
(4) Keeping the pressure, heating and rectifying to obtain a tetrahydrofuran finished product:
and continuously introducing inert gas, controlling the pressure in the kettle to be 0.1-0.6 MPa, heating and rectifying to obtain a tetrahydrofuran finished product with the water content of less than 0.1 percent.
Further, the industrial waste tetrahydrofuran mother liquor in the step (1) is a mixed liquor containing tetrahydrofuran, low-boiling-point raw materials and water.
Further, in the step (1), the distillation temperature is 80-90 ℃.
Further, in the step (2), the temperature of the top of the rectifying tower is 40-50 ℃ when the low boiling point raw material is separated by heating and rectifying.
Further, in the step (3), the temperature of the top of the rectifying tower is 80-100 ℃ when the rectifying tower is heated, rectified and dehydrated.
Further, in the step (4), the temperature of the top of the rectifying tower is 100-120 ℃ when the rectifying tower is heated and rectified.
Further, in the step (1), the step (2), the step (3) and the step (4), steam is used for heating.
Further, in the step (2), the step (3) and the step (4), the inert gas is nitrogen or argon.
The invention has the following positive effects:
the method effectively utilizes the low boiling point to remove most of water, avoids using other organic extracting agents and then carrying out secondary recovery, reduces the cost, has simple and convenient operation and good product quality, and improves the product quality and the yield.
Detailed Description
The present invention is further illustrated by the following examples.
The low boiling point raw material contained in the industrial waste tetrahydrofuran is dichloromethane with the boiling point of 39.75.
Example 1
(1) Adding 6000L of industrial waste tetrahydrofuran mother liquor into the rough steaming kettle, starting the rough steaming kettle for stirring, opening circulating water of a condenser, opening a feeding valve of a crude product receiving tank, starting the rough steaming kettle for steam heating, and stopping rough steaming when the temperature of the rough steaming kettle reaches 85 ℃.
(2) Introducing nitrogen into the rectifying tower kettle, pressing a tetrahydrofuran crude product (the tetrahydrofuran purity is 78.98 percent, and the moisture content is 16.1 percent) into the rectifying tower kettle, pressurizing to 0.3Mpa, opening steam to heat the tower top temperature to 40 ℃, heating and refluxing for 60 minutes, detecting that the purity of the low-boiling-point raw material at the tower top is 95.2 percent, and the moisture content is 13.12 percent, and separating the low-boiling-point raw material dichloromethane.
(3) And continuously introducing nitrogen into the rectifying tower kettle, controlling the pressure in the rectifying tower kettle to be 0.3MPa, heating the temperature at the top of the tower by steam to be 80 ℃, and detecting the purity of the tetrahydrofuran in the rectifying tower kettle to be 98.23% and the water content to be 4.16% after the tetrahydrofuran is extracted from the top of the tower for 1 hour.
(4) And continuously introducing nitrogen into the rectifying tower kettle, controlling the pressure in the rectifying tower kettle to be 0.3MPa, continuously rectifying the tetrahydrofuran mixed solution with the moisture of 4.16 percent, detecting the tetrahydrofuran purity of the rectifying tower kettle to be 99.77 percent and the moisture content to be 0.01 percent at the temperature of 120 +/-2 ℃ at the tower top, and extracting the tetrahydrofuran mixed solution to a finished product tank.
Example 2
(1) And (3) pumping 6000L of industrial waste tetrahydrofuran mother liquor into the rough steaming kettle, starting a motor of the rough steaming kettle for stirring, opening a condenser for circulation, opening a crude product receiving tank feed valve, starting steam heating of the rough steaming kettle, and stopping rough steaming when the temperature of the rough steaming kettle reaches 90 ℃.
(2) Introducing argon into the rectifying tower kettle, pressing a tetrahydrofuran crude product (the tetrahydrofuran purity is 79.4 percent, and the moisture content is 15.6 percent) into the rectifying tower kettle, pressurizing to 0.1Mpa, opening steam to heat the tower top temperature to 50 ℃, heating and refluxing for 50 minutes, detecting that the purity of the low-boiling-point raw material at the tower top is 97.5 percent, and the moisture content is 11.85 percent, and separating the low-boiling-point raw material dichloromethane.
(3) And (3) continuously introducing argon into the rectifying tower kettle, controlling the pressure in the rectifying tower kettle to be 0.1MPa, heating the temperature at the top of the tower by steam to be 90 ℃, and detecting the purity of tetrahydrofuran in the rectifying tower kettle to be 97.54% and the water content to be 4.25% after the tetrahydrofuran is extracted from the top of the tower for 1.5 hours.
(4) And (3) continuously introducing argon into the rectifying tower kettle, controlling the pressure in the rectifying tower kettle to be 0.1MPa, continuously rectifying the tetrahydrofuran mixed solution with the moisture of 4.25%, detecting that the purity of the tetrahydrofuran is 99.71% and the moisture content is 0.03% at the tower top temperature of 110 +/-2 ℃, and extracting to a finished product tank.
Example 3
(1) Adding 6000L of industrial waste tetrahydrofuran mother liquor into the rough steaming kettle, starting a motor of the rough steaming kettle for stirring, opening a condenser for circulation, opening a crude product receiving tank feed valve, starting steam heating of the rough steaming kettle, and stopping rough steaming when the temperature of the rough steaming kettle reaches 80 ℃.
(2) Introducing nitrogen into the rectifying tower kettle, pressing a tetrahydrofuran crude product (the tetrahydrofuran purity is 79.1 percent, and the moisture content is 15.9 percent) into the rectifying tower kettle, pressurizing to 0.6Mpa, opening steam to heat the tower top temperature to 45 ℃, heating and refluxing for 30 minutes, detecting that the purity of the low-boiling-point raw material at the tower top is 96.3 percent, and the moisture content is 11.21 percent, and separating the low-boiling-point raw material dichloromethane.
(3) And continuously introducing nitrogen into the rectifying tower kettle, controlling the pressure in the rectifying tower kettle to be 0.6MPa, heating the temperature at the top of the tower by steam to be 100 ℃, and detecting that the purity of the tetrahydrofuran in the rectifying tower kettle is 97.76% and the moisture content is 5.28% after the tetrahydrofuran is extracted from the top of the tower for 2 hours.
(4) And continuously introducing nitrogen into the kettle of the rectifying tower, controlling the pressure in the kettle to be 0.6MPa, continuously rectifying the tetrahydrofuran mixed solution with the moisture of 5.28 percent, detecting that the purity of the tetrahydrofuran is 99.77 percent and the moisture content is 0.03 percent at the temperature of 100 +/-2 ℃ at the top of the tower, and extracting the tetrahydrofuran mixed solution to a finished product tank.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and is not intended to limit the invention to the particular forms disclosed. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (3)
1. A method for rectifying and recovering tetrahydrofuran from industrial waste tetrahydrofuran is characterized by comprising the following steps:
(1) Crude tetrahydrofuran is obtained by crude distillation:
putting industrial waste tetrahydrofuran mother liquor into a rough distillation kettle, and heating and distilling to obtain a tetrahydrofuran crude product;
(2) Introducing inert gas to separate low-boiling-point raw materials:
introducing inert gas into a rectifying tower kettle, pumping the tetrahydrofuran crude product obtained in the step (1) into a rectifying tower, controlling the pressure in the kettle to be 0.1-0.6 MPa through pressurization, and heating, rectifying and separating a low-boiling-point raw material;
(3) Introducing inert gas for pressure dehydration:
continuously introducing inert gas into the rectifying tower kettle, controlling the pressure in the kettle to be 0.1-0.6 MPa, and heating, rectifying and dehydrating to obtain tetrahydrofuran mixed liquor with the water content of less than 6%;
(4) Keeping the pressure, heating and rectifying to obtain a tetrahydrofuran finished product:
continuously introducing inert gas, controlling the pressure in the kettle to be 0.1-0.6 MPa, heating and rectifying to obtain a tetrahydrofuran finished product with the water content of less than 0.1%;
wherein the industrial waste tetrahydrofuran mother liquor in the step (1) is a mixed liquor containing tetrahydrofuran, a low-boiling-point raw material and water; in the step (1), the distillation temperature is 80-90 ℃;
in the step (2), the temperature of the top of the rectifying tower is 40-50 ℃ when the low boiling point raw material is separated by heating, rectifying and distilling;
in the step (3), the temperature of the top of the rectifying tower is 80-100 ℃ when the heating, rectifying and dehydrating are carried out;
in the step (4), the temperature of the top of the rectifying tower is 100-120 ℃ when the temperature is raised and the rectifying tower is heated and rectified.
2. The method for rectifying and recovering tetrahydrofuran from industrial waste tetrahydrofuran according to claim 1, wherein the method comprises the following steps: in the step (1), the step (2), the step (3) and the step (4), steam is used for heating.
3. The method for rectifying and recovering tetrahydrofuran from industrial waste tetrahydrofuran according to claim 1, wherein the method comprises the following steps: in the step (2), the step (3) and the step (4), the inert gas is nitrogen or argon.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010709392.4A CN111793046B (en) | 2020-07-22 | 2020-07-22 | Method for rectifying and recovering tetrahydrofuran from industrial waste tetrahydrofuran |
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| CN202010709392.4A CN111793046B (en) | 2020-07-22 | 2020-07-22 | Method for rectifying and recovering tetrahydrofuran from industrial waste tetrahydrofuran |
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| CN111793046B true CN111793046B (en) | 2023-01-06 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2000143652A (en) * | 1998-11-13 | 2000-05-26 | Mitsubishi Chemicals Corp | Purification of crude tetrahydrofuran |
| CN106543112B (en) * | 2016-11-02 | 2019-06-21 | 宁夏美邦寰宇化学有限公司 | A kind of infiltrating and vaporizing membrane coupling variable-pressure rectification tetrahydrofuran dewatering process |
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