CN216687961U - Separation device containing mixed solvent of 2-methyltetrahydrofuran, methanol and water - Google Patents
Separation device containing mixed solvent of 2-methyltetrahydrofuran, methanol and water Download PDFInfo
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- CN216687961U CN216687961U CN202220218543.0U CN202220218543U CN216687961U CN 216687961 U CN216687961 U CN 216687961U CN 202220218543 U CN202220218543 U CN 202220218543U CN 216687961 U CN216687961 U CN 216687961U
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Abstract
The utility model relates to a separation device containing a mixed solvent of 2-methyltetrahydrofuran, methanol and water, which comprises: the device comprises an extraction rectifying tower, an azeotropic rectifying tower and a methanol refining tower, wherein the top of the extraction rectifying tower is connected with an extraction rectifying tower laminator, and the extraction rectifying tower laminator is communicated with a middle feed inlet of the azeotropic rectifying tower; the tower top of the azeotropic distillation tower is connected with an azeotropic distillation tower condenser, the outlet end of the azeotropic distillation tower condenser is connected with an azeotropic distillation tower delayer, and the azeotropic distillation tower delayer is communicated with the extraction distillation tower; the utility model realizes the separation of the mixed solvent containing 2-methyltetrahydrofuran, methanol and water by combining the extraction rectifying tower, the azeotropic rectifying tower and the phase splitting operation, has the advantages of high recovery purity, low energy consumption and the like, and simultaneously takes the existing deionized water in the solvent as an extracting agent to avoid the influence of the introduction of a third component on the use of the recovered solvent.
Description
Technical Field
The utility model relates to the field of chemical solvent separation, in particular to a separation device containing a mixed solvent of 2-methyltetrahydrofuran, methanol and water.
Background
Prothioconazole is a novel broad-spectrum triazolethione bactericide, is mainly used for preventing and treating diseases of crops such as cereals, wheat and beans, has the advantages of good biological and ecological toxicity, low toxicity, no teratogenicity and mutagenicity, no toxicity to embryos, safety to human bodies and environments and the like, and is widely applied.
2-chloro-a- (1-chlorocyclopropyl) -a- (chloromethyl) -phenethyl alcohol (TM-5 for short) is used as one of important intermediates for synthesizing prothioconazole, and the molecular formula is as follows: c12H13Cl3O, molecular weight: 279.59, CAS: 134818-67-0. TM-5 is prepared by using o-chlorobenzyl chloride and magnesium metal as raw materials, preparing Grignard solution through Grignard reaction, then performing addition reaction with 2-chloro-1- (1-chlorocyclopropyl) -ethanone, and finally dropwise adding hydrochloric acid to quench and refine. In the process of Grignard reaction and addition reaction, a large amount of 2-methyltetrahydrofuran is required to be used as a solvent, and byproducts such as methanol and the like are generated at the same time; during the quenching, a mixed solvent containing 2-methyltetrahydrofuran, methanol and water is finally formed due to the introduction of water. Therefore, the mixed solvent needs to be separated, and the 2-methyltetrahydrofuran can be recycled.
For the above mixed solvent, the separation of 2-methyltetrahydrofuran is a very difficult problem. This is because the system has multiple groups of binary azeotropes under normal pressure, specifically: the 2-methyltetrahydrofuran and the methanol have binary azeotropy, the azeotropic temperature is 62.8 ℃, and the 2-methyltetrahydrofuran content in the azeotropic component is 43 percent; meanwhile, the 2-methyltetrahydrofuran and the water have binary azeotropy, the azeotropic temperature is 71 ℃, and the 2-methyltetrahydrofuran content in the azeotropic component is 89.6%. Therefore, it is difficult to remove methanol and water in the mixed solvent by ordinary distillation, and a special separation technique such as distillation is required. The selection of the extractant or entrainer in a particular rectification is particularly important.
SUMMERY OF THE UTILITY MODEL
Technical problem to be solved
In order to solve the above problems of the prior art, the present invention provides a separation apparatus comprising a mixed solvent of 2-methyltetrahydrofuran, methanol and water.
(II) technical scheme
In order to achieve the purpose, the utility model adopts the main technical scheme that:
a separation device containing a mixed solvent of 2-methyltetrahydrofuran, methanol and water is characterized by comprising: the device comprises an extraction rectifying tower, an azeotropic rectifying tower and a methanol refining tower, wherein the upper part and the lower part of the extraction rectifying tower are respectively provided with an upper part feed inlet and a lower part feed inlet, and the top of the extraction rectifying tower is connected with a rectifying tower condenser; the outlet end of the condenser of the rectifying tower is connected with an extraction rectifying tower delayer, the water phase outlet end of the extraction rectifying tower delayer is communicated with a reflux port at the top of the extraction rectifying tower, and the oil phase outlet end of the extraction rectifying tower delayer is communicated with the middle feed inlet of the azeotropic rectifying tower;
the top of the azeotropic distillation tower is connected with an azeotropic distillation tower condenser, the outlet end of the azeotropic distillation tower condenser is connected with an azeotropic distillation tower delayer, the oil phase outlet end of the azeotropic distillation tower delayer is communicated with a reflux port at the top of the azeotropic distillation tower, and the water phase outlet end of the azeotropic distillation tower delayer is communicated with a feed inlet at the lower part of the extractive distillation tower; the bottom of the azeotropic distillation tower is provided with a 2-methyltetrahydrofuran product outlet;
the tower kettle of the extraction rectifying tower is connected with the feed end of the methanol refining tower, the top of the methanol refining tower is connected with a methanol refining tower condenser, the tower kettle outlet of the methanol refining tower is communicated with the upper feed inlet of the extraction rectifying tower, or/and the tower kettle outlet of the methanol refining tower is connected with an external drain pipe.
Furthermore, the theoretical plate number of the extractive distillation tower is 24-42, the operating pressure is 100-110 kPa, the reflux ratio is 1-4, and the temperature of the tower top condensate is 45-55 ℃.
Furthermore, the theoretical plate number of the azeotropic distillation tower is 12-32, the operating pressure is 100-110 kPa, the reflux ratio is 4-10, and the temperature of the condensate liquid at the top of the tower is 45-55 ℃.
Further, the bottom of the extractive distillation column is connected with an extractive distillation column reboiler.
Further, the bottom of the azeotropic distillation tower is connected with an azeotropic distillation tower reboiler.
Further, the bottom of the methanol refining tower is connected with a methanol refining tower reboiler.
(III) advantageous effects
The utility model has the beneficial effects that: (1) the separation process combining extractive distillation, azeotropic distillation and split phase is adopted, the separation of the 2-methyltetrahydrofuran from the methanol and the water in the mixed solvent is realized, and the separation problem of multi-group binary azeotropy in the system is solved.
(2) The utility model adopts the existing water in the system as the extracting agent, thereby effectively avoiding the problem that the introduction of the third component influences the recycling of the recovered solvent.
(3) The purity of the 2-methyltetrahydrofuran recovered by the method is more than 99.8 percent, and the content of methanol and water is less than 0.1 percent.
(4) The purity of the methanol recovered by the method is more than 99.8 percent, and the content of 2-methyltetrahydrofuran and water is less than 0.1 percent.
Drawings
Fig. 1 is a schematic structural diagram of an embodiment of the present invention.
Detailed Description
For the purpose of better explaining the present invention and to facilitate understanding, the present invention will be described in detail by way of specific embodiments with reference to the accompanying drawings.
A separation apparatus containing a mixed solvent of 2-methyltetrahydrofuran, methanol and water according to an embodiment of the present invention, as shown in fig. 1, includes: the device comprises an extraction rectifying tower T1, an azeotropic rectifying tower T2 and a methanol refining tower T3, wherein the upper part and the lower part of the extraction rectifying tower T1 are respectively provided with an upper feed inlet and a lower feed inlet, and the top of the extraction rectifying tower T1 is connected with a rectifying tower condenser E2; the outlet end of the rectifying tower condenser E2 is connected with an extraction rectifying tower delayer SP1, the water phase outlet end of the extraction rectifying tower delayer SP1 is communicated with a reflux port at the top of an extraction rectifying tower T1, and the oil phase outlet end of the extraction rectifying tower delayer SP1 is communicated with the middle feed inlet of an azeotropic rectifying tower T2;
the top of the azeotropic distillation tower T2 is connected with an azeotropic distillation tower condenser E4, the outlet end of the azeotropic distillation tower condenser E4 is connected with an azeotropic distillation tower delayer SP2, the oil phase outlet end of the azeotropic distillation tower delayer SP2 is communicated with the top reflux port of the azeotropic distillation tower T2, and the water phase outlet end of the azeotropic distillation tower delayer SP2 is communicated with the lower feed inlet of the extractive distillation tower T1; the bottom of the azeotropic distillation tower T2 is provided with a 2-methyltetrahydrofuran product outlet;
the tower kettle of the extraction rectifying tower T1 is connected with the feed end of a methanol refining tower T3, the top of the methanol refining tower T3 is connected with a methanol refining tower condenser E6, the tower kettle outlet of the methanol refining tower T3 is communicated with the upper feed inlet of the extraction rectifying tower T1, or/and the tower kettle outlet of the methanol refining tower T3 is connected with an external drain pipe.
The separation method of the embodiment comprises the following steps:
step S1: deionized water is used as an extracting agent, the deionized water and a mixed solvent containing 2-methyltetrahydrofuran, methanol and water respectively enter an extraction rectifying tower T1 from an upper feed inlet and a lower feed inlet of the extraction rectifying tower T1, a gas phase at the top of the extraction rectifying tower T1 enters an extraction rectifying tower delayer SP1 for phase separation after being condensed by an extraction rectifying tower condenser E2, a water phase returns to the extraction rectifying tower T1 as a reflux, an oil phase is a 2-methyltetrahydrofuran crude product, and the content of methanol is less than 2%; a methanol crude product with the 2-methyltetrahydrofuran content of less than 0.1 percent is obtained at the tower bottom of the extraction rectifying tower T1;
step S2: 2-methyltetrahydrofuran crude product enters from the middle part of an azeotropic rectifying tower T2 to purify 2-methyltetrahydrofuran, the gas phase at the top of the azeotropic rectifying tower T2 is 2-methyltetrahydrofuran, water azeotrope, 2-methyltetrahydrofuran and methanol azeotrope, the gas phase is condensed by an azeotropic rectifying tower condenser E4 and then enters an azeotropic rectifying tower delayer SP2 for phase separation, the oil phase returns to the azeotropic rectifying tower T2 as reflux, the water phase is sent to an extractive rectifying tower T1 for recovery, and the 2-methyltetrahydrofuran product with the methanol and water contents less than 0.1 percent is obtained at the tower bottom of the azeotropic rectifying tower T2;
step S3: and (3) feeding a methanol crude product from the middle part of a methanol refining tower T3 for methanol refining, obtaining a methanol product with 2-methyltetrahydrofuran and water content less than 0.1% from the top of the methanol refining tower T3, cooling an extractant with methanol content less than 0.1% obtained from the bottom of the methanol refining tower T3, returning the extractant to an extraction rectifying tower T1 for recycling as the extractant, and discharging the redundant part.
Further, the bottom of the extractive distillation column T1 is connected with an extractive distillation column reboiler E1, and the extractive distillation column reboiler E1 vaporizes the liquid material in the bottom of the extractive distillation column T1 to provide rising gas for the extractive distillation column T1, so that gas-liquid contact is performed in the column, and the separation effect is realized; the bottom of the azeotropic distillation tower T2 is connected with an azeotropic distillation tower reboiler E3, the azeotropic distillation tower reboiler E3 vaporizes the liquid material in the tower kettle of the azeotropic distillation tower T2, and provides rising gas for the azeotropic distillation tower T2, so that gas-liquid contact is carried out in the tower, and the separation effect is realized; the bottom of the methanol refining tower T3 is connected with a methanol refining tower reboiler E5, the methanol refining tower reboiler E5 vaporizes liquid materials at the tower bottom of the methanol refining tower T3, and rising gas is provided for the methanol refining tower T3, so that gas-liquid contact is performed in the tower, and the separation effect is realized.
The top of the methanol refining tower T3 is connected to a methanol refining tower condenser E6 for condensing the gas rising at the top of the tower into a liquid and subcooling to a desired temperature.
The azeotropic distillation tower condenser E4 is used for condensing the gas rising from the tower top into liquid and supercooling the liquid to a required temperature (such as 45 ℃), the liquid enters the azeotropic distillation tower delayer SP2 for phase splitting, the oil phase returns to the azeotropic distillation tower T2 as reflux, the water phase is sent to the extraction distillation tower T1 for recovery, and the 2-methyltetrahydrofuran product with the methanol and water content less than 0.1 percent is obtained in the tower bottom of the azeotropic distillation tower T2.
In this embodiment, the operating conditions of the extractive distillation column T1 are as follows: the theoretical plate number is 24-42, the operation pressure is 100-110 kPa, the reflux ratio is 1-4, the volume ratio of the extracting agent to the mixed solvent containing 2-methyltetrahydrofuran, methanol and water is 0.5-4.0, and the temperature of the condensate at the top of the tower is 45-55 ℃.
In this embodiment, the operating conditions of the azeotropic distillation column T2 are as follows: the theoretical plate number is 12-32, the operation pressure is 100-110 kPa, the reflux ratio is 4-10, and the temperature of the tower top condensate is 45-55 ℃.
The following are two specific examples of the present embodiment.
Example 1:
the material of the extractive distillation column T1 is SUS304, 752Y-standard plate corrugated packing is filled in the column, the diameter of the column is 400mm, the number of theoretical plates is 32, an extracting agent is fed from the 6 th theoretical plate, and a mixed solvent to be separated is fed from the 24 th theoretical plate; the azeotropic distillation column T2 was made of SUS304, and 752Y-gauge corrugated packing was packed in the column, and the column diameter was 300mm, the number of theoretical plates was 20, and the feed was from the 8 th theoretical plate. The methanol purification column T3 was made of SUS304, and 752Y-gauge corrugated plate packing was packed in the column, and the column diameter was 400mm, the number of theoretical plates was 30, and the column was fed from the 20 th theoretical plate.
The mixed solvent to be separated enters from a lower feed inlet of an extractive distillation tower T1, the feed flow is 500kg/h, and the feed composition is as follows: 10% of methanol, 15% of 2-methyltetrahydrofuran and 75% of water. The extractant water enters from an upper feed inlet of the extractive distillation column T1, the feed flow is 1000kg/h, and the operation conditions of the extractive distillation column T1 are as follows: the operation pressure is 101kPa, the reflux ratio is 2.0, the tower top temperature is 71 ℃, the tower bottom temperature is 98.3 ℃, and the tower top condensate temperature is 50 ℃. The operating conditions of the azeotropic distillation column T2 are as follows: the operation pressure is 101kPa, the reflux ratio is 5.6, the tower top temperature is 66.2 ℃, the tower bottom temperature is 80.7 ℃, and the tower top condensate temperature is 45 ℃. The operating conditions of the methanol refining tower T3 are as follows: the operation pressure is 101kPa, the reflux ratio is 10, the tower top temperature is 64.5 ℃, and the tower bottom temperature is 100.7 ℃.
Under the conditions, the flow rate of the 2-methyltetrahydrofuran product recovered from the bottom of the azeotropic distillation tower T2 is 75kg/h, the purity is 99.9%, the methanol content is 80ppm, and the water content is 50ppm, so that the recycling quality index is achieved. The flow rate of a methanol product recovered from the top of the methanol refining tower T3 is 50kg/h, the purity is 99.9 percent, the 2-methyltetrahydrofuran content is 82ppm, and the water content is 135 ppm.
Example 2:
the material of the extractive distillation column T1 is SUS304, 752Y-standard plate corrugated packing is filled in the column, the diameter of the column is 400mm, the number of theoretical plates is 32, the extractant is fed from the 6 th theoretical plate, and the mixed solvent to be separated is fed from the 24 th theoretical plate. The azeotropic distillation column T2 was made of SUS304, and 752Y-gauge corrugated packing was packed in the column, and the column diameter was 300mm, the number of theoretical plates was 20, and the feed was from the 8 th theoretical plate. The methanol purification column T3 was made of SUS304, and 752Y-gauge corrugated plate packing was packed in the column, and the column diameter was 400mm, the number of theoretical plates was 30, and the column was fed from the 20 th theoretical plate.
The mixed solvent to be separated enters from a lower feed inlet of an extractive distillation tower T1, the feed flow is 600kg/h, and the feed composition is as follows: 10% of methanol, 20% of 2-methyltetrahydrofuran and 70% of water. The extractant water enters from an upper feed inlet of the extractive distillation column T1, the feed flow is 1600kg/h, and the operation conditions of the extractive distillation column T1 are as follows: the operation pressure is 101kPa, the reflux ratio is 2.5, the tower top temperature is 68.5 ℃, the tower bottom temperature is 98.9 ℃, and the tower top condensate temperature is 50 ℃. The operating conditions of the azeotropic distillation column T2 are as follows: the operation pressure is 101kPa, the reflux ratio is 5.0, the tower top temperature is 68.4 ℃, the tower bottom temperature is 80.7 ℃, and the tower top condensate temperature is 45 ℃. The operating conditions of the methanol refining tower T3 are as follows: the operation pressure is 101kPa, the reflux ratio is 10, the tower top temperature is 64.5 ℃, and the tower bottom temperature is 100.7 ℃.
Under the conditions, the flow rate of the 2-methyltetrahydrofuran product recovered from the bottom of the azeotropic distillation tower T2 is 120kg/h, the purity is 99.9%, the methanol content is 100ppm, and the water content is 78ppm, so that the recycling quality index is reached. The flow rate of a methanol product recovered from the top of the methanol refining tower T3 is 50kg/h, the purity is 99.9 percent, the 2-methyltetrahydrofuran content is 66ppm, and the water content is 122 ppm.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (4)
1. A separation device containing a mixed solvent of 2-methyltetrahydrofuran, methanol and water is characterized by comprising: the device comprises an extraction rectifying tower (T1), an azeotropic rectifying tower (T2) and a methanol refining tower (T3), wherein the upper part and the lower part of the extraction rectifying tower (T1) are respectively provided with an upper feed inlet and a lower feed inlet, and the top of the extraction rectifying tower (T1) is connected with a rectifying tower condenser (E2); the outlet end of the rectifying tower condenser (E2) is connected with an extraction rectifying tower delayer (SP 1), the water phase outlet end of the extraction rectifying tower delayer (SP 1) is communicated with a reflux opening at the top of an extraction rectifying tower (T1), and the oil phase outlet end of the extraction rectifying tower delayer (SP 1) is communicated with the middle feed inlet of an azeotropic rectifying tower (T2);
the top of the azeotropic distillation tower (T2) is connected with an azeotropic distillation tower condenser (E4), the outlet end of the azeotropic distillation tower condenser (E4) is connected with an azeotropic distillation tower layering device (SP 2), the oil phase outlet end of the azeotropic distillation tower layering device (SP 2) is communicated with the top reflux opening of the azeotropic distillation tower (T2), and the water phase outlet end of the azeotropic distillation tower layering device (SP 2) is communicated with the lower feed inlet of the extractive distillation tower (T1); the bottom of the azeotropic distillation tower (T2) is provided with a 2-methyltetrahydrofuran product outlet;
the tower kettle of the extraction rectifying tower (T1) is connected with the feed end of a methanol refining tower (T3), the top of the methanol refining tower (T3) is connected with a methanol refining tower condenser (E6), the tower kettle outlet of the methanol refining tower (T3) is communicated with the upper feed inlet of the extraction rectifying tower (T1), or/and the tower kettle outlet of the methanol refining tower (T3) is connected with an external drain pipe.
2. The separation apparatus according to claim 1, wherein the separation apparatus comprises a mixed solvent of 2-methyltetrahydrofuran, methanol and water, and is characterized in that: the bottom of the extractive distillation column (T1) is connected with an extractive distillation column reboiler (E1).
3. The separation apparatus according to claim 1, wherein the separation apparatus comprises a mixed solvent of 2-methyltetrahydrofuran, methanol and water, and is characterized in that: the bottom of the azeotropic distillation tower (T2) is connected with an azeotropic distillation tower reboiler (E3).
4. The separation apparatus according to claim 1, wherein the separation apparatus comprises a mixed solvent of 2-methyltetrahydrofuran, methanol and water, and is characterized in that: the bottom of the methanol refining tower (T3) is connected with a methanol refining tower reboiler (E5).
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114409615A (en) * | 2022-01-26 | 2022-04-29 | 福建技术师范学院 | Separation method of mixed solvent containing 2-methyltetrahydrofuran, methanol and water |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114409615A (en) * | 2022-01-26 | 2022-04-29 | 福建技术师范学院 | Separation method of mixed solvent containing 2-methyltetrahydrofuran, methanol and water |
| CN114409615B (en) * | 2022-01-26 | 2024-07-12 | 福建技术师范学院 | Separation method of mixed solvent containing 2-methyltetrahydrofuran, methanol and water |
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