阅读说明：本技术 一种合成药物中间体产生mtbe废溶剂的回收提纯方法及设备 (Method and equipment for recovering and purifying MTBE waste solvent generated in synthesis of drug intermediate ) 是由 范文林 黄啟虓 张怡 纪王洋 于 2021-06-17 设计创作，主要内容包括：本发明公开了一种合成药物中间体产生MTBE废溶剂的回收提纯方法及设备,本发明的有益效果是,通过精馏,液液萃取等一系列的方法,除去合成药物中间体废溶剂中的杂质,回收其中仍有回用价值的有机溶剂。本发明提供的回收提纯方法,经精馏、萃取的一系列能耗低的工序,将合成药物中间体废溶剂分离,实现对其中有回用价值溶剂的再利用,降低医药行业中废溶剂对环境的污染程度,节约了生产成本。(The invention discloses a method and equipment for recovering and purifying MTBE waste solvent generated by synthesizing a drug intermediate. The recovery and purification method provided by the invention separates the waste solvent of the synthetic drug intermediate through a series of low-energy-consumption processes of rectification and extraction, realizes the reutilization of the solvent with reuse value, reduces the pollution degree of the waste solvent in the pharmaceutical industry to the environment, and saves the production cost.)

1. A recycling and purifying apparatus for producing MTBE waste solvent in the synthesis of pharmaceutical intermediates, comprising: the device comprises a waste liquid tank, a rectification and ethylbenzene removal tower, a methyl tert-butyl ether and ethanol rectification tower, an ethanol rectification tower, a tetrahydrofuran rectification tower and an extraction tower, and is characterized in that the waste liquid tank is connected to the rectification and ethylbenzene removal tower, the methyl tert-butyl ether and the ethanol rectification tower are connected to the rectification and ethylbenzene removal tower, the ethanol rectification tower and the tetrahydrofuran rectification tower are respectively connected to the methyl tert-butyl ether and the ethanol rectification tower, the extraction tower is connected to the tetrahydrofuran rectification tower, a centrifugal extraction structure is installed in the extraction tower, and rectification structures are installed in the rectification and ethylbenzene removal tower, the methyl tert-butyl ether and ethanol rectification tower, the ethanol rectification tower and the tetrahydrofuran rectification tower;

the centrifugal extraction structure comprises: the extraction device comprises a plurality of extraction plates, an extraction driving rod, a plurality of arc limiting blocks, a plurality of arc supporting blocks, a plurality of driving bevel gears, a plurality of transfer bevel gears, a plurality of intermediate rotating shafts, a transfer driving machine, a plurality of transmission bevel gears, a plurality of reverse rotating rods, a plurality of reverse rotating sheets and a plurality of forward rotating sheets;

the extraction plates are uniformly arranged in the extraction tower, the extraction driving rod is inserted in the extraction tower and the extraction plates through bearings, the arc limiting blocks are uniformly arranged on the extraction driving rod respectively, the arc supporting blocks are uniformly arranged on the extraction driving rod respectively and are positioned at the bottom ends of the arc limiting blocks respectively, the middle rotating shafts are inserted in the arc limiting blocks and the arc supporting blocks respectively through bearings, the middle rotating gears are arranged on the middle rotating shafts respectively, the driving bevel gears are uniformly arranged on the extraction driving rod respectively, the driving bevel gears are respectively engaged with the middle rotating bevel gears, and the reverse rotating rods are respectively inserted in the arc supporting blocks through bearings, the plurality of transmission helical gears are respectively arranged on the plurality of reverse rotating rods, the plurality of reverse rotating pieces are respectively arranged on the plurality of reverse rotating rods, and the plurality of forward rotating pieces are respectively and uniformly arranged on the extraction driving rod.

2. The apparatus for recycling and purifying MTBE waste solvent generated from the synthesis of pharmaceutical intermediates of claim 1, wherein said rectification structure comprises: the system comprises a plurality of flow distribution plates, a plurality of U-shaped drainage tubes, a plurality of U-shaped steam drainage tubes, a plurality of S-shaped anti-backflow tubes, a plurality of flow discharge tubes, a plurality of cooling boxes, a plurality of cooling drainage coiled tubes, a plurality of coolers, cooling liquid and a plurality of discharge flow distribution tubes;

the plurality of the splitter plates are respectively and uniformly arranged on the rectifying and ethylbenzene-removing tower, the methyl tert-butyl ether and ethanol rectifying tower, the ethanol rectifying tower and the tetrahydrofuran rectifying tower, the plurality of U-shaped steam drainage tubes are respectively and uniformly inserted on the plurality of splitter plates, the plurality of S-shaped countercurrent-proof tubes are respectively arranged on the plurality of splitter plates, the plurality of U-shaped drainage tubes are respectively arranged on the plurality of S-shaped countercurrent-proof tubes, the plurality of countercurrent-proof tubes are respectively arranged on the plurality of S-shaped countercurrent-proof tubes, the plurality of cooling boxes are respectively arranged on the rectifying and ethylbenzene-removing tower, the methyl tert-butyl ether and ethanol rectifying tower, the ethanol rectifying tower and the tetrahydrofuran rectifying tower, the plurality of cooling drainage coil tubes are respectively arranged in the plurality of cooling boxes, and the plurality of coolers are respectively arranged in the plurality of cooling boxes, the cooling liquid is respectively arranged in the plurality of cooling boxes, and the plurality of discharge flow dividing pipes are respectively arranged on the plurality of U-shaped steam drainage pipes.

3. The apparatus for recycling and purifying MTBE waste solvent generated from the synthesis of pharmaceutical intermediates of claim 2, wherein said plurality of splitter plates are respectively provided with a plurality of electrical heating tubes.

4. A recovery and purification method for MTBE waste solvent generated in the synthesis of drug intermediates is characterized by comprising the following operation steps of S1, waste solvent rectification; step S2, rectifying and separating the mixture of methyl tert-butyl ether and ethanol from the rest mixture of tetrahydrofuran, tert-butyl alcohol and tert-butyl acetate; step S3, removing impurities by using ethanol; step S4, recovering tert-butyl alcohol and tert-butyl acetate; step S5, collecting tert-butyl acetate;

the step S1: taking an MTBE waste solvent as a synthetic drug intermediate in a waste liquid box, adding the MTBE waste solvent into a rectification and ethylbenzene removal tower for rectification, collecting ethylbenzene from the bottom of the rectification and ethylbenzene removal tower, and collecting the rest substances from the top of the rectification and ethylbenzene removal tower;

the step S2: adding the components extracted from the top of the ethyl benzene removal tower in the step S1 into a methyl tert-butyl ether and ethanol rectifying tower, controlling the rectifying boiling point, extracting a mixture of the methyl tert-butyl ether and ethanol from the top of the methyl tert-butyl ether and ethanol rectifying tower, and extracting a mixture of tetrahydrofuran, tert-butyl alcohol and tert-butyl acetate remained in the bottom of the methyl tert-butyl ether and ethanol rectifying tower;

the step S3: adding the components extracted from the top of the tower in the step S2 into an ethanol rectifying tower, controlling the rectifying boiling point, removing the ethanol impurity by using the methyl tert-butyl ether azeotropy, and extracting industrial-grade methyl tert-butyl ether;

the step S4: adding the components extracted from the tower kettle in the step S2 into a tetrahydrofuran rectifying tower, controlling the rectifying boiling point, extracting industrial-grade tetrahydrofuran from the tower top, and remaining tert-butyl alcohol and tert-butyl acetate in the tower kettle;

the step S5: and (4) adding pure water into the components extracted from the tower bottom in the step S4, performing liquid-liquid extraction through the extraction tower, separating liquid, and obtaining the industrial grade tert-butyl acetate at the upper layer, wherein the lower layer is water and a small amount of tert-butyl alcohol impurities.

5. The method of claim 4, wherein in step S1, the distillation conditions are as follows: the pressure is normal pressure, the temperature of the bottom of the rectifying kettle is 60-145 ℃, the temperature of liquid in the kettle is 56-136 ℃, the temperature of the top of the kettle is 55-135 ℃, and the reflux ratio is controlled to be 30: 1-1: 1.

6. the method of claim 5, wherein the rectification conditions in step S2 are as follows: the pressure is normal pressure, the temperature of the bottom of the rectifying still is 60-105 ℃, the temperature of liquid in the still is 56-99 ℃, the temperature of the top of the still is 55-98 ℃, and the reflux ratio is controlled to be 30: 1-1: 1.

7. the method of claim 6, wherein in step S3, the distillation conditions are as follows: the pressure is normal pressure, the temperature of the bottom of the rectifying kettle is 60-85 ℃, the temperature of liquid in the kettle is 56-79 ℃, the temperature of the top of the kettle is 55-78 ℃, and the reflux ratio is controlled to be 30: 1-1: 1.

8. the method of claim 7, wherein the distillation conditions in step S4 are as follows: the pressure is normal pressure, the temperature of the bottom of the rectifying still is 70-105 ℃, the temperature of liquid in the still is 66-99 ℃, the temperature of the top of the still is 65-98 ℃, and the reflux ratio is controlled to be 30: 1-1: 1.

9. the method of claim 8, wherein the step S5 is performed by liquid-liquid extraction to separate t-butyl acetate and t-butyl alcohol.

10. The method of claim 9, wherein the step of recovering and purifying the waste solvent from the production of MTBE from the synthesis of pharmaceutical intermediates further comprises using reduced pressure and increased pressure to change the distillation column conditions, and the extractant is selected from water, inorganic salts, and the like which are miscible with t-butyl alcohol but insoluble with t-butyl acetate.

Technical Field

The invention relates to the technical field of solvent purification, in particular to a method and equipment for recovering and purifying MTBE waste solvent generated in the synthesis of a drug intermediate.

Background

The reason why pharmaceutical enterprises in chemical synthesis generate very serious pollution every year is that the final product only accounts for 5-15% of the total amount of raw materials due to long synthesis process routes and excessive reaction steps, and the rest of the pharmaceutical enterprises exist in the form of three wastes (waste gas, waste liquid and waste residue). The discharged waste liquid has the following characteristics: most of the substances containing the biological toxicity are difficult to degrade and inhibit the growth of microorganisms; the chroma is higher; contains a large amount of organic solvents, such as benzene, aliphatic compounds, ammonia nitrogen, esters, alcohols, sulfides, and the like; and other waste such as salt, starch, various metal ions, antibiotic residues, etc. The waste solvent has complex components, high CODCr, SS and BOD5 concentrations and large fluctuation of water quality and water quantity, belongs to high-concentration organic wastewater, can not be treated by the conventional method, and can cause serious pollution to the environment. In conventional chemical synthesis pharmaceutical wastewater treatment, physicochemical treatment, chemical treatment, biochemical treatment and combination of various methods are generally adopted to treat pharmaceutical wastewater so as to achieve the purpose of discharging the wastewater.

In the traditional method for treating the waste solvent of the synthetic drug intermediate, although the waste water reaches the dischargeable index, the waste water still brings huge pressure to the self-regulation capacity of the ecological environment, if the waste solvent in the chemical synthesis pharmaceutical process can be simply classified, the organic solvent in the waste solvent can be recycled and purified, the waste water treatment cost is extremely high, the environmental pressure is reduced, the organic solvent is recycled, and the additional value of the organic solvent is increased.

Disclosure of Invention

The invention aims to solve the problems, designs a method and equipment for recovering and purifying the MTBE waste solvent generated by synthesizing the drug intermediate, and separates and purifies the organic solvent in the drug intermediate waste solvent through methods such as rectification, liquid-liquid extraction and the like, thereby realizing the reutilization of the solvent with recycling value.

The technical scheme of the invention for realizing the aim is as follows: a recycling and purifying apparatus for producing MTBE waste solvent in the synthesis of pharmaceutical intermediates, comprising: the device comprises a waste liquid tank, a rectification and ethylbenzene removal tower, a methyl tert-butyl ether and ethanol rectification tower, an ethanol rectification tower, a tetrahydrofuran rectification tower and an extraction tower, wherein the waste liquid tank is connected to the rectification and ethylbenzene removal tower, the methyl tert-butyl ether and ethanol rectification tower is connected to the rectification and ethylbenzene removal tower, the ethanol rectification tower and the tetrahydrofuran rectification tower are respectively connected to the methyl tert-butyl ether and the ethanol rectification tower, the extraction tower is connected to the tetrahydrofuran rectification tower, a centrifugal extraction structure is installed in the extraction tower, and rectification structures are installed in the rectification and ethylbenzene removal tower, the methyl tert-butyl ether and ethanol rectification tower, the ethanol rectification tower and the tetrahydrofuran rectification tower;

the centrifugal extraction structure comprises: the extraction device comprises a plurality of extraction plates, an extraction driving rod, a plurality of arc limiting blocks, a plurality of arc supporting blocks, a plurality of driving bevel gears, a plurality of transfer bevel gears, a plurality of intermediate rotating shafts, a transfer driving machine, a plurality of transmission bevel gears, a plurality of reverse rotating rods, a plurality of reverse rotating sheets and a plurality of forward rotating sheets;

the extraction plates are uniformly arranged in the extraction tower, the extraction driving rod is inserted in the extraction tower and the extraction plates through bearings, the arc limiting blocks are uniformly arranged on the extraction driving rod respectively, the arc supporting blocks are uniformly arranged on the extraction driving rod respectively and are positioned at the bottom ends of the arc limiting blocks respectively, the middle rotating shafts are inserted in the arc limiting blocks and the arc supporting blocks respectively through bearings, the middle rotating gears are arranged on the middle rotating shafts respectively, the driving bevel gears are uniformly arranged on the extraction driving rod respectively, the driving bevel gears are respectively engaged with the middle rotating bevel gears, and the reverse rotating rods are respectively inserted in the arc supporting blocks through bearings, the plurality of transmission helical gears are respectively arranged on the plurality of reverse rotating rods, the plurality of reverse rotating pieces are respectively arranged on the plurality of reverse rotating rods, and the plurality of forward rotating pieces are respectively and uniformly arranged on the extraction driving rod.

Preferably, the rectification structure comprises: the system comprises a plurality of flow distribution plates, a plurality of U-shaped drainage tubes, a plurality of U-shaped steam drainage tubes, a plurality of S-shaped anti-backflow tubes, a plurality of flow discharge tubes, a plurality of cooling boxes, a plurality of cooling drainage coiled tubes, a plurality of coolers, cooling liquid and a plurality of discharge flow distribution tubes;

the plurality of the splitter plates are respectively and uniformly arranged on the rectifying and ethylbenzene-removing tower, the methyl tert-butyl ether and ethanol rectifying tower, the ethanol rectifying tower and the tetrahydrofuran rectifying tower, the plurality of U-shaped steam drainage tubes are respectively and uniformly inserted on the plurality of splitter plates, the plurality of S-shaped countercurrent-proof tubes are respectively arranged on the plurality of splitter plates, the plurality of U-shaped drainage tubes are respectively arranged on the plurality of S-shaped countercurrent-proof tubes, the plurality of countercurrent-proof tubes are respectively arranged on the plurality of S-shaped countercurrent-proof tubes, the plurality of cooling boxes are respectively arranged on the rectifying and ethylbenzene-removing tower, the methyl tert-butyl ether and ethanol rectifying tower, the ethanol rectifying tower and the tetrahydrofuran rectifying tower, the plurality of cooling drainage coil tubes are respectively arranged in the plurality of cooling boxes, and the plurality of coolers are respectively arranged in the plurality of cooling boxes, the cooling liquid is respectively arranged in the plurality of cooling boxes, and the plurality of discharge flow dividing pipes are respectively arranged on the plurality of U-shaped steam drainage pipes.

Preferably, a plurality of electric heating tubes are respectively arranged on the plurality of flow distribution plates.

A recovery and purification method for MTBE waste solvent generated in the synthesis of drug intermediates comprises the following operation steps of S1, waste solvent rectification; step S2, rectifying and separating the mixture of methyl tert-butyl ether and ethanol from the rest mixture of tetrahydrofuran, tert-butyl alcohol and tert-butyl acetate; step S3, removing impurities by using ethanol; step S4, recovering tert-butyl alcohol and tert-butyl acetate; step S5, collecting tert-butyl acetate;

the step S1: taking an MTBE waste solvent as a synthetic drug intermediate in a waste liquid box, adding the MTBE waste solvent into a rectification and ethylbenzene removal tower for rectification, collecting ethylbenzene from the bottom of the rectification and ethylbenzene removal tower, and collecting the rest substances from the top of the rectification and ethylbenzene removal tower;

the step S2: adding the components extracted from the top of the ethyl benzene removal tower in the step S1 into a methyl tert-butyl ether and ethanol rectifying tower, controlling the rectifying boiling point, extracting a mixture of the methyl tert-butyl ether and ethanol from the top of the methyl tert-butyl ether and ethanol rectifying tower, and extracting a mixture of tetrahydrofuran, tert-butyl alcohol and tert-butyl acetate remained in the bottom of the methyl tert-butyl ether and ethanol rectifying tower;

the step S3: adding the components extracted from the top of the tower in the step S2 into an ethanol rectifying tower, controlling the rectifying boiling point, removing the ethanol impurity by using the methyl tert-butyl ether azeotropy, and extracting industrial-grade methyl tert-butyl ether;

the step S4: adding the components extracted from the tower kettle in the step S2 into a tetrahydrofuran rectifying tower, controlling the rectifying boiling point, extracting industrial-grade tetrahydrofuran from the tower top, and remaining tert-butyl alcohol and tert-butyl acetate in the tower kettle;

the step S5: and (4) adding pure water into the components extracted from the tower bottom in the step S4, performing liquid-liquid extraction through the extraction tower, separating liquid, and obtaining the industrial grade tert-butyl acetate at the upper layer, wherein the lower layer is water and a small amount of tert-butyl alcohol impurities.

In the step S1, the rectification conditions are as follows: the pressure is normal pressure, the temperature of the bottom of the rectifying kettle is 60-145 ℃, the temperature of liquid in the kettle is 56-136 ℃, the temperature of the top of the kettle is 55-135 ℃, and the reflux ratio is controlled to be 30: 1-1: 1.

in step S2, the rectification conditions are: the pressure is normal pressure, the temperature of the bottom of the rectifying still is 60-105 ℃, the temperature of liquid in the still is 56-99 ℃, the temperature of the top of the still is 55-98 ℃, and the reflux ratio is controlled to be 30: 1-1: 1.

in the step S3, the rectification conditions are as follows: the pressure is normal pressure, the temperature of the bottom of the rectifying kettle is 60-85 ℃, the temperature of liquid in the kettle is 56-79 ℃, the temperature of the top of the kettle is 55-78 ℃, and the reflux ratio is controlled to be 30: 1-1: 1.

in the step S4, the rectification conditions are as follows: the pressure is normal pressure, the temperature of the bottom of the rectifying still is 70-105 ℃, the temperature of liquid in the still is 66-99 ℃, the temperature of the top of the still is 65-98 ℃, and the reflux ratio is controlled to be 30: 1-1: 1.

in the step S5, tert-butyl acetate and tert-butyl alcohol are separated by liquid-liquid extraction.

The method also comprises changing the conditions of the rectifying tower by adopting a decompression and pressurization mode, and the extracting agent can be water, inorganic salt and the like which are mutually soluble with the tertiary butyl alcohol but not soluble with the tertiary butyl acetate.

The method and the equipment for recovering and purifying the MTBE waste solvent generated by the synthetic drug intermediate manufactured by the technical scheme of the invention remove impurities in the synthetic drug intermediate waste solvent and recover the organic solvent with reuse value through a series of methods such as rectification, liquid-liquid extraction and the like. The recovery and purification method provided by the invention separates the waste solvent of the synthetic drug intermediate through a series of low-energy-consumption processes of rectification and extraction, realizes the reutilization of the solvent with reuse value, reduces the pollution degree of the waste solvent in the pharmaceutical industry to the environment, and saves the production cost.

Drawings

FIG. 1 is a schematic flow diagram of a method and an apparatus for recovering and purifying MTBE waste solvent generated from the synthesis of pharmaceutical intermediates according to the present invention.

FIG. 2 is a schematic sectional view of the recovery and purification method and apparatus for MTBE waste solvent generated from the synthesis of pharmaceutical intermediates according to the present invention.

Fig. 3 is an enlarged view of a portion "a" in fig. 2.

Fig. 4 is an enlarged view of a portion "B" in fig. 2.

In the figure: 1. a waste liquid tank; 2. a rectifying and ethylbenzene-removing tower; 3. methyl tert-butyl ether and ethanol rectifying tower; 4. an ethanol rectification column; 5. a tetrahydrofuran rectification column; 6. an extraction tower; 7. extracting the plate; 8. an extraction driving rod; 9. an arc limiting block; 10. a circular arc supporting block; 11. driving the helical gear; 12. transferring the helical gear; 13. a middle rotating shaft; 14. transferring a driver; 15. a transmission bevel gear; 16. a reverse rotating rod; 17. a reverse rotation piece; 18. the sheet is rotated positively.

Detailed Description

The present invention will be described in detail with reference to the accompanying drawings, as shown in fig. 1 to 4, a recovery and purification apparatus for producing MTBE waste solvent from the synthesis of pharmaceutical intermediates, comprising: the device comprises a waste liquid tank, a rectification and ethylbenzene removal tower, a methyl tert-butyl ether and ethanol rectification tower, an ethanol rectification tower, a tetrahydrofuran rectification tower and an extraction tower, wherein the waste liquid tank is connected to the rectification and ethylbenzene removal tower, the methyl tert-butyl ether and ethanol rectification tower is connected to the rectification and ethylbenzene removal tower, the ethanol rectification tower and the tetrahydrofuran rectification tower are respectively connected to the methyl tert-butyl ether and the ethanol rectification tower, the extraction tower is connected to the tetrahydrofuran rectification tower, a centrifugal extraction structure is installed in the extraction tower, and rectification structures are installed in the rectification and ethylbenzene removal tower, the methyl tert-butyl ether and ethanol rectification tower, the ethanol rectification tower and the tetrahydrofuran rectification tower; the centrifugal extraction structure comprises: the extraction device comprises a plurality of extraction plates, an extraction driving rod, a plurality of arc limiting blocks, a plurality of arc supporting blocks, a plurality of driving bevel gears, a plurality of transfer bevel gears, a plurality of intermediate rotating shafts, a transfer driving machine, a plurality of transmission bevel gears, a plurality of reverse rotating rods, a plurality of reverse rotating sheets and a plurality of forward rotating sheets; the extraction plates are uniformly arranged in the extraction tower, the extraction driving rod is inserted in the extraction tower and the extraction plates through bearings, the arc limiting blocks are uniformly arranged on the extraction driving rod respectively, the arc supporting blocks are uniformly arranged on the extraction driving rod respectively and are positioned at the bottom ends of the arc limiting blocks respectively, the middle rotating shafts are inserted in the arc limiting blocks and the arc supporting blocks respectively through bearings, the middle rotating gears are arranged on the middle rotating shafts respectively, the driving bevel gears are uniformly arranged on the extraction driving rod respectively, the driving bevel gears are respectively engaged with the middle rotating bevel gears, and the reverse rotating rods are respectively inserted in the arc supporting blocks through bearings, the plurality of transmission bevel gears are respectively arranged on the plurality of reverse rotating rods, the plurality of reverse rotating pieces are respectively arranged on the plurality of reverse rotating rods, and the plurality of forward rotating pieces are respectively and uniformly arranged on the extraction driving rod; the rectification structure comprises: the system comprises a plurality of flow distribution plates, a plurality of U-shaped drainage tubes, a plurality of U-shaped steam drainage tubes, a plurality of S-shaped anti-backflow tubes, a plurality of flow discharge tubes, a plurality of cooling boxes, a plurality of cooling drainage coiled tubes, a plurality of coolers, cooling liquid and a plurality of discharge flow distribution tubes; the plurality of the splitter plates are respectively and uniformly arranged on the rectifying and ethylbenzene-removing tower, the methyl tert-butyl ether and ethanol rectifying tower, the ethanol rectifying tower and the tetrahydrofuran rectifying tower, the plurality of U-shaped steam drainage tubes are respectively and uniformly inserted on the plurality of splitter plates, the plurality of S-shaped countercurrent-proof tubes are respectively arranged on the plurality of splitter plates, the plurality of U-shaped drainage tubes are respectively arranged on the plurality of S-shaped countercurrent-proof tubes, the plurality of countercurrent-proof tubes are respectively arranged on the plurality of S-shaped countercurrent-proof tubes, the plurality of cooling boxes are respectively arranged on the rectifying and ethylbenzene-removing tower, the methyl tert-butyl ether and ethanol rectifying tower, the ethanol rectifying tower and the tetrahydrofuran rectifying tower, the plurality of cooling drainage coil tubes are respectively arranged in the plurality of cooling boxes, and the plurality of coolers are respectively arranged in the plurality of cooling boxes, the cooling liquid is respectively arranged in the plurality of cooling boxes, and the plurality of discharge flow dividing pipes are respectively arranged on the plurality of U-shaped steam drainage pipes; a plurality of electric heating pipes are respectively arranged on the plurality of splitter plates.

A recovery and purification method for MTBE waste solvent generated in the synthesis of drug intermediates comprises the following operation steps of S1, waste solvent rectification; step S2, rectifying and separating the mixture of methyl tert-butyl ether and ethanol from the rest mixture of tetrahydrofuran, tert-butyl alcohol and tert-butyl acetate; step S3, removing impurities by using ethanol; step S4, recovering tert-butyl alcohol and tert-butyl acetate; step S5, collecting tert-butyl acetate;

the step S1: taking an MTBE waste solvent as a synthetic drug intermediate in a waste liquid box, adding the MTBE waste solvent into a rectification and ethylbenzene removal tower for rectification, collecting ethylbenzene from the bottom of the rectification and ethylbenzene removal tower, and collecting the rest substances from the top of the rectification and ethylbenzene removal tower;

the step S2: adding the components extracted from the top of the ethyl benzene removal tower in the step S1 into a methyl tert-butyl ether and ethanol rectifying tower, controlling the rectifying boiling point, extracting a mixture of the methyl tert-butyl ether and ethanol from the top of the methyl tert-butyl ether and ethanol rectifying tower, and extracting a mixture of tetrahydrofuran, tert-butyl alcohol and tert-butyl acetate remained in the bottom of the methyl tert-butyl ether and ethanol rectifying tower;

the step S3: adding the components extracted from the top of the tower in the step S2 into an ethanol rectifying tower, controlling the rectifying boiling point, removing the ethanol impurity by using the methyl tert-butyl ether azeotropy, and extracting industrial-grade methyl tert-butyl ether;

the step S4: adding the components extracted from the tower kettle in the step S2 into a tetrahydrofuran rectifying tower, controlling the rectifying boiling point, extracting industrial-grade tetrahydrofuran from the tower top, and remaining tert-butyl alcohol and tert-butyl acetate in the tower kettle;

the step S5: and (4) adding pure water into the components extracted from the tower bottom in the step S4, performing liquid-liquid extraction through the extraction tower, separating liquid, and obtaining the industrial grade tert-butyl acetate at the upper layer, wherein the lower layer is water and a small amount of tert-butyl alcohol impurities.

In the step S1, the rectification conditions are as follows: the pressure is normal pressure, the temperature of the bottom of the rectifying kettle is 60-145 ℃, the temperature of liquid in the kettle is 56-136 ℃, the temperature of the top of the kettle is 55-135 ℃, and the reflux ratio is controlled to be 30: 1-1: 1.

in step S2, the rectification conditions are: the pressure is normal pressure, the temperature of the bottom of the rectifying still is 60-105 ℃, the temperature of liquid in the still is 56-99 ℃, the temperature of the top of the still is 55-98 ℃, and the reflux ratio is controlled to be 30: 1-1: 1.

in the step S3, the rectification conditions are as follows: the pressure is normal pressure, the temperature of the bottom of the rectifying kettle is 60-85 ℃, the temperature of liquid in the kettle is 56-79 ℃, the temperature of the top of the kettle is 55-78 ℃, and the reflux ratio is controlled to be 30: 1-1: 1.

in the step S4, the rectification conditions are as follows: the pressure is normal pressure, the temperature of the bottom of the rectifying still is 70-105 ℃, the temperature of liquid in the still is 66-99 ℃, the temperature of the top of the still is 65-98 ℃, and the reflux ratio is controlled to be 30: 1-1: 1.

in the step S5, tert-butyl acetate and tert-butyl alcohol are separated by liquid-liquid extraction.

The method also comprises changing the conditions of the rectifying tower by adopting a decompression and pressurization mode, and the extracting agent can be water, inorganic salt and the like which are mutually soluble with the tertiary butyl alcohol but not soluble with the tertiary butyl acetate.

The present embodiment is characterized by comprising: the device comprises a waste liquid tank, a rectification and ethylbenzene removal tower, a methyl tert-butyl ether and ethanol rectification tower, an ethanol rectification tower, a tetrahydrofuran rectification tower and an extraction tower, wherein the waste liquid tank is connected to the rectification and ethylbenzene removal tower; the centrifugal extraction structure comprises: the extraction device comprises a plurality of extraction plates, an extraction driving rod, a plurality of arc limiting blocks, a plurality of arc supporting blocks, a plurality of driving bevel gears, a plurality of transfer bevel gears, a plurality of intermediate rotating shafts, a transfer driving machine, a plurality of transmission bevel gears, a plurality of reverse rotating rods, a plurality of reverse rotating sheets and a plurality of forward rotating sheets; the extraction plates are uniformly arranged in the extraction tower, the extraction driving rod is inserted on the extraction tower and the extraction plates through a bearing, the arc limiting blocks are respectively and uniformly arranged on the extraction driving rod, the arc supporting blocks are respectively and uniformly arranged on the extraction driving rod and are respectively positioned at the bottom ends of the arc limiting blocks, the middle rotating shafts are respectively inserted on the arc limiting blocks and the arc supporting blocks through bearings, the transfer bevel gears are respectively arranged on the middle rotating shafts, the drive bevel gears are respectively and uniformly arranged on the extraction driving rod and are respectively engaged with the transfer bevel gears, the reverse rotating rods are respectively inserted on the arc supporting blocks through bearings, the transmission bevel gears are respectively arranged on the reverse rotating rods, and the reverse rotating pieces are respectively arranged on the reverse rotating rods, the plurality of positive rotating pieces are respectively and uniformly arranged on the extraction driving rod; through a series of methods such as rectification, liquid-liquid extraction and the like, impurities in the waste solvent for synthesizing the drug intermediate are removed, and the organic solvent still having recycling value is recovered. The recovery and purification method provided by the invention separates the waste solvent of the synthetic drug intermediate through a series of low-energy-consumption processes of rectification and extraction, realizes the reutilization of the solvent with reuse value, reduces the pollution degree of the waste solvent in the pharmaceutical industry to the environment, and saves the production cost.

All the electrical components in the present application are connected with the power supply adapted to the electrical components through the wires, and an appropriate controller should be selected according to actual conditions to meet the control requirements, and specific connection and control sequences should be obtained.

Example 1: taking a synthetic drug intermediate waste solvent from a waste liquid tank, adding the waste solvent into a rectification ethylbenzene removal tower, rectifying under normal pressure, heating at 145 ℃, controlling the reflux ratio to be 15: 1, extracting substances at the top of the tower, canning the rectified liquid after the rectified liquid is detected to be qualified when the temperature at the top of the tower is 136 ℃, filling nitrogen for storage, thus obtaining industrial grade ethylbenzene with the content of more than or equal to 99.8 percent, extracting components at the top of the middle rectification ethylbenzene removal tower, adding the components into a methyl tert-butyl ether and ethanol rectification tower, rectifying under normal pressure, heating at 105 ℃, controlling the reflux ratio to be 20: 1, extracting the mixture of the methyl tert-butyl ether and ethanol when the temperature at the top of the rectification tower is 50-56 ℃, extracting the components at the top of the middle tower, adding the components into the ethanol rectification tower, rectifying under normal pressure, heating at 85 ℃, controlling the reflux ratio to be 10: 1, removing ethanol impurities, extracting 55 ℃ methyl tert-butyl ether at the top of an ethanol rectifying tower to remove ethanol impurities by azeotropy, filling distilled liquid into a tank after detection is qualified, filling nitrogen for storage to obtain industrial grade methyl tert-butyl ether with the content of more than or equal to 99.0 percent, extracting components from a tower bottom in the ethanol rectifying tower, adding the components into a tetrahydrofuran rectifying tower, rectifying under normal pressure, heating to 105 ℃, controlling the reflux ratio to be 20: 1, extracting the components at the top of the tetrahydrofuran rectifying tower at the temperature of 66 ℃, filling the distilled liquid into the tank after detection is qualified, filling nitrogen for storage to obtain industrial grade tetrahydrofuran with the content of more than or equal to 99.0 percent, adding pure water liquid into the components extracted from the tower bottom in the tetrahydrofuran rectifying tower for liquid-liquid extraction, separating liquid after the upper layer is detected to be qualified, filling nitrogen for storage to obtain industrial grade tert-butyl acetate with the content of more than or equal to 99.5 percent, through the operation of the transfer driving machine on the bottom end of the extraction tower, drive the operation of the extraction actuating lever on the transfer driving machine drive end, it rotates to drive a plurality of drive helical gears on the extraction actuating lever, it rotates with its gear engagement's transfer helical gear to drive respectively through a plurality of drive helical gears, drive transmission helical gear rotation on it respectively through a pair of transfer helical gears, drive reverse dwang on it respectively through a plurality of transmission helical gears, drive a plurality of reverse rotation pieces on it respectively through a plurality of rotatory reverse rotation pieces and provide positive rotation piece through a plurality of reverse dwang, carry out the multi-angle rotation with the equipment in the extraction tower and mix. A

Example 2: taking a synthetic drug intermediate waste solvent from a waste liquid tank, adding the waste solvent into a rectification ethylbenzene removal tower, rectifying under normal pressure, heating at 145 ℃, controlling the reflux ratio to be 10: 1, extracting substances at the top of the tower, canning the rectified liquid after the rectified liquid is detected to be qualified when the temperature at the top of the tower is 136 ℃, filling nitrogen for storage, thus obtaining industrial grade ethylbenzene with the content of more than or equal to 99.8 percent, extracting components at the top of the rectification ethylbenzene removal tower, adding the extracted components into a methyl tert-butyl ether and ethanol rectification tower, rectifying under normal pressure, heating at 105 ℃, controlling the reflux ratio to be 15: 1, extracting the mixture of the methyl tert-butyl ether and ethanol when the temperature at the top of the tower is 50-56 ℃, remaining the mixture of tetrahydrofuran, tert-butyl alcohol and tert-butyl acetate in the tower kettle, adding the extracted components at the top of the tower into the ethanol rectification tower, rectifying under normal pressure, heating at 85 ℃, controlling the reflux ratio to be 10: 1, removing the ethanol by utilizing the methyl tert-butyl ether as an azeotropic mixture, and filling the qualified rectification liquid into a tank, filling nitrogen for storage to obtain industrial grade methyl tert-butyl ether with the content of more than or equal to 99.0%, extracting components from a tower kettle in a methyl tert-butyl ether and ethanol rectification tower, adding the components into a tetrahydrofuran rectification tower, rectifying at normal pressure, heating at 105 ℃, controlling the reflux ratio to be 10: 1, extracting the components when the boiling point of the tower top is 66 ℃, filling the qualified rectification liquid into the tank, filling the nitrogen for storage to obtain the industrial grade tetrahydrofuran with the content of more than or equal to 99.0%, remaining tert-butyl alcohol and tert-butyl acetate in the tower kettle, extracting the components from the tower kettle in the tetrahydrofuran rectification tower, adding pure water for liquid-liquid extraction, separating liquid after the qualified detection of the upper layer, filling the nitrogen for storage to obtain the industrial grade tert-butyl acetate with the content of more than or equal to 99.5%.

The technical indexes of the industrial grade methyl tert-butyl ether purified in the embodiment 1-2 are shown in the table I:

watch 1

The technical indexes of the industrial grade ethylbenzene purified in the examples 1-2 are shown in the following table two:

watch two

The technical indexes of the industrial-grade tetrahydrofuran purified in the embodiments 1-2 are shown in the third table:

watch III

The technical indexes of the industrial grade methyl tert-butyl ether purified in the embodiment 1-2 are shown in the fourth table:

watch four

The technical solutions described above only represent the preferred technical solutions of the present invention, and some possible modifications to some parts of the technical solutions by those skilled in the art all represent the principles of the present invention, and fall within the protection scope of the present invention.