CN113563364A - Method for removing alcohol ester in 6-APA mother liquor - Google Patents
Method for removing alcohol ester in 6-APA mother liquor Download PDFInfo
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- CN113563364A CN113563364A CN202110856195.XA CN202110856195A CN113563364A CN 113563364 A CN113563364 A CN 113563364A CN 202110856195 A CN202110856195 A CN 202110856195A CN 113563364 A CN113563364 A CN 113563364A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D499/00—Heterocyclic compounds containing 4-thia-1-azabicyclo [3.2.0] heptane ring systems, i.e. compounds containing a ring system of the formula:, e.g. penicillins, penems; Such ring systems being further condensed, e.g. 2,3-condensed with an oxygen-, nitrogen- or sulfur-containing hetero ring
- C07D499/21—Heterocyclic compounds containing 4-thia-1-azabicyclo [3.2.0] heptane ring systems, i.e. compounds containing a ring system of the formula:, e.g. penicillins, penems; Such ring systems being further condensed, e.g. 2,3-condensed with an oxygen-, nitrogen- or sulfur-containing hetero ring with a nitrogen atom directly attached in position 6 and a carbon atom having three bonds to hetero atoms with at the most one bond to halogen, e.g. an ester or nitrile radical, directly attached in position 2
- C07D499/42—Compounds with a free primary amino radical attached in position 6
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D499/00—Heterocyclic compounds containing 4-thia-1-azabicyclo [3.2.0] heptane ring systems, i.e. compounds containing a ring system of the formula:, e.g. penicillins, penems; Such ring systems being further condensed, e.g. 2,3-condensed with an oxygen-, nitrogen- or sulfur-containing hetero ring
- C07D499/04—Preparation
- C07D499/18—Separation; Purification
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Abstract
The invention relates to a method for removing alcohol ester in 6-APA mother liquor. The method realizes the purpose of recovering alcohol, ester and 6-APA from the 6-APA mother liquor by designing a rectifying tower and a soft water heater of a rectifying reaction system device and regulating and controlling the temperature of a feed inlet and a discharge outlet of each device. The invention can obtain high-purity alcohol and ester by controlling the temperature of each part, and can further improve the recovery rate of the alcohol and the ester. The recovered butanol and butyl acetate have high purity, the purity of the butanol and butyl acetate is more than 99.0 percent, and the method can be directly used for penicillin fermentation production, thereby realizing a circular economy system for penicillin production; the high-efficiency recovery of the butanol and the butyl acetate is realized, and the recovery rate of the butanol and the butyl acetate is over 95 percent.
Description
Technical Field
The invention relates to the technical field of 6-APA mother liquor recovery, and particularly relates to a method for removing alcohol ester in 6-APA mother liquor.
Background
6-Aminopenicillanic acid (6-Aminopenicillanic acid) is commonly called side chain-free penicillin, is called 6-APA for short, is white flaky crystal, is a penicillin mother nucleus, is an important intermediate for producing various semi-synthetic penicillins, and has wide application range. Certain by-products in the production process have interference effect on the crystallization process of the 6-APA, and the yield and the product quality of the 6-APA are seriously influenced.
In industrial production, 6-APA is generally prepared by cracking penicillin G salt under the action of penicillin acylase at present, and the waste liquid after the cracking liquid is crystallized still contains about 0.3 percent (mass fraction) of 6-APA, 4.0 to 5.0 percent of butanol, 0.5 percent of butyl acetate, a small amount of phenylacetic acid, a small amount of ammonium chloride, penicillin raw materials and trace other impurities. 6-APA in the crystallization mother liquor still has high economic benefit, and if the 6-APA is directly discharged, the 6-APA in the discharged waste liquor not only causes resource economic waste, but also has certain influence on the environment.
If the residual quantity of alcohol and ester in the 6-APA mother liquor is large, the enzyme activity in the subsequent process can be greatly influenced. There are many methods for extracting 6-APA from 6-APA mother liquor, but there is no process flow for removing butanol and butyl acetate.
Disclosure of Invention
The invention provides a method for removing alcohol ester from 6-APA mother liquor, aiming at the problem that alcohol and ester in the 6-APA mother liquor are difficult to remove in the prior art. The method realizes the purpose of recovering alcohol, ester and 6-APA from the 6-APA mother liquor by designing a rectifying tower and a soft water heater of a rectifying reaction system device and regulating and controlling the temperature of a feed inlet and a discharge outlet of each device.
The technical scheme of the invention is as follows:
a method for removing alcohol ester from 6-APA mother liquor comprises the following steps:
injecting 6-APA mother liquor into a mother liquor tank, feeding the mother liquor into a tube pass of a heat exchanger A at the top of a tower through a feed pump at the temperature of 8-12 ℃, heating the mother liquor to 26-30 ℃, then feeding the mother liquor into a preheater C of a tower kettle, heating the mother liquor to 38-42 ℃, feeding the heated mother liquor into a preheater A at the middle section of the tower, heating the preheated mother liquor to 53-57 ℃ by steam, and then converting the heated mother liquor into a 39-43 ℃ steam-liquid mixture through reduced pressure distillation equipment, and feeding the steam-liquid mixture into a rectification tower from a first plate to the last of a plate tower;
meanwhile, pure water enters a heater through a preheater B, the pure water is changed into steam with the temperature of 80 ℃ in a negative pressure state, the steam enters a rectifying tower from a tower bottom and ascends in the rectifying tower, heat transfer and mass transfer are completed in the rectifying tower, and alcohol and ester in the 6-APA mother liquor are blown to the tower top by the pure water steam;
steam, alcohol and ester flowing out of the top of the rectifying tower enter a shell pass of a heat exchanger A, are cooled into liquid, enter a shell pass of a heat exchanger B, enter a tube pass by circulating water to cool an alcohol ester solution, and the recombined water is divided and enters an intermediate tank from a lower pipeline; the light component alcohol and ester enter a vacuum condenser; condensing alcohol and ester into a middle tank at 40 ℃; the vacuum condenser is connected with the buffer tank through a pipeline, and the vacuum pump is connected behind the buffer tank, so that the whole rectification system is in a negative pressure state, and the negative pressure value range is 40 multiplied by 103-50×103Pa；
Feeding 38-42 ℃ water, alcohol and ester in the intermediate tank into a cooler A through a material passing pump, cooling the alcohol ester solution with circulating water into a phase separation tank, wherein the phase separation tank contains 91-97.9% of water, 2-8% of alcohol and 0.1-1% of ester; water and alcohol in the phase separation tank enter a butanol-removing wastewater system through a lower pipeline; the ester is withdrawn from the upper pipe.
The mixed liquid obtained in the tower kettle after the rectifying tower is reacted enters a preheater C, is cooled to 41-45 ℃ from 52-56 ℃ after being subjected to heat exchange, enters a cooler B, and is cooled to 23-27 ℃ from 41-45 ℃ by circulating water; and then, the mixed solution enters a cooler C, the mixed solution is cooled to 8-12 ℃ from 23-27 ℃ by low-temperature water, and finally the mixed solution of 6-APA, ammonium chloride, phenylacetic acid and the like enters a discharge tank.
The pure water is H2O；
The 6-APA mother liquor comprises 4-5% of butanol, 0.1-1.0% of butyl acetate, 0.01-0.10% of ammonium chloride, 85-95% of phenylacetic acid and 0.1-0.5% of 6-APA by mass concentration.
A device for removing alcohol ester in 6-APA mother liquor comprises a mother liquor tank, a feed pump, a heat exchanger A, a preheater C, a preheater A, reduced pressure distillation equipment, a rectifying tower, a heat exchanger B, a vacuum condenser, a buffer tank and a vacuum pump which are sequentially connected through pipelines;
wherein the pure water pipeline is connected with a preheater B, the preheater B is connected with a heater, and the heater is connected with the bottom of the rectifying tower; the liquid outlet end of the tower kettle of the rectifying tower is connected with a preheater C, and the preheater C is also sequentially connected with a cooler B, a discharge pump, the cooler C and a discharge tank; the preheater C is also connected with the feed inlet of the rectifying tower sequentially through the preheater A and the reduced pressure distillation equipment; the top of the rectifying tower is connected with a heat exchanger A, and the heat exchanger A is also connected with a heat exchanger B and a preheater C respectively; a discharge port at the top end of the heat exchanger B is connected with a butanol-removing wastewater system through the intermediate tank, the cooler A and the phase splitting tank in sequence; a discharge port at the bottom end of the heat exchanger B is also connected with a vacuum condenser, the vacuum condenser is also connected with a buffer tank, and the vacuum condenser and the buffer tank are also respectively connected with an intermediate tank; the mother liquor tank is connected with the heat exchanger A;
the rectifying tower is divided into an upper part and a lower part, the upper layer is a plate tower, the range of tower plates is 5-7, and the distance between plates is 40-60 cm; the lower layer is a packed tower, the packed tower is provided with 2-4 packing layers, the height of each packing layer is 1-4 m, and the packing is the same.
The mother liquor feeding position is the first plate from last of the plate tower. (ii) a
The buffer tank is also connected with a vacuum pump;
the method for removing the alcohol ester from the 6-APA mother liquor enters a rectifying tower after being preheated, and then the alcohol ester is removed through a strict temperature control system. The process fully utilizes energy and meets the standard of green chemistry.
The invention has the beneficial effects that:
the invention can obtain high-purity alcohol and ester by controlling the temperature of each part, and can further improve the recovery rate of the alcohol and the ester.
The invention realizes the high-efficiency recovery of alcohol and ester in the 6-APA cracking waste liquid, and effectively reduces the influence of the alcohol and ester on the subsequent process;
the invention solves the technical problem that alcohol and ester in the 6-APA cracking waste liquid are not easy to recover;
the butanol and butyl acetate recovered by the invention have high purity, the purity of the butanol and butyl acetate is more than 99.0 percent, and the butanol and butyl acetate can be directly used for penicillin fermentation production, thereby realizing a circular economy system for penicillin production;
the invention realizes the high-efficiency recovery of butanol and butyl acetate, and the recovery rate of butanol and butyl acetate is more than 95 percent;
the invention has simple process and low requirement on equipment, and is easy for industrial application.
Drawings
FIG. 1 is a process flow diagram of the present invention.
1 is mother liquor jar, 2 is heat exchanger A, 3 is preheater C, 4 is preheater A, 5 is decompression distillation plant, 6 is the rectifying column, 7 is preheater B, 8 is the heater, 9 is heat exchanger B, 10 is vacuum condenser, 11 is the buffer tank, 12 is the pans, 13 is cooler A, 14 is the phase separation jar, 15 is cooler B, 16 is cooler C, 17 is the ejection of compact jar.
Detailed Description
In the method for removing the alcohol ester in the 6-APA mother liquor, a related system is shown in figure 1 and comprises a mother liquor tank 1, a feed pump, a heat exchanger A8, a preheater C3, a preheater A4, a reduced pressure distillation device 5, a rectifying tower 6, a heat exchanger B9, a vacuum condenser 10, a buffer tank 11 and a vacuum pump which are sequentially connected through pipelines;
wherein the pure water pipeline is connected with a preheater B7, a preheater B7 is connected with a heater 8, and the heater 8 is connected with the bottom of the rectifying tower 6; the liquid outlet end of the tower bottom of the rectifying tower 6 is connected with a preheater C3, and a preheater C3 is further connected with a cooler B15, a discharge pump, a cooler C16 and a discharge tank 17 in sequence; the preheater C3 is also connected with the feed inlet of the rectifying tower 6 through a preheater A4 and a reduced pressure distillation device 5 in sequence; the top of the rectifying tower 6 is connected with a heat exchanger A2, and a heat exchanger A2 is also connected with a heat exchanger B9 and a preheater C3 respectively; a discharge port at the top end of the heat exchanger B9 is connected with a butanol-removing wastewater system through the intermediate tank 12, the cooler A13 and the phase separation tank 14 in sequence; a discharge port at the bottom end of the heat exchanger B9 is also connected with a vacuum condenser 10, the vacuum condenser 10 is also connected with a buffer tank 11, and the vacuum condenser 10 and the buffer tank 11 are also respectively connected with an intermediate tank 12; the mother liquor tank 1 is connected with a heat exchanger A;
the rectifying tower 6 is divided into an upper part and a lower part, the upper layer is a plate tower, the range of tower plates is 5-7, and the distance between plates is 40-60 cm; the lower layer is a packed tower, the packed tower is provided with 2-4 packing layers, the height of each packing layer is 1-4 m, and the packing is the same. The following embodiment is specifically two packing layers, wherein the height of one packing layer is 4 m; the upper layer plate tower aims at removing foam, and the lower layer packed tower can ensure the vapor-liquid contact area, thereby better transferring heat and mass; meanwhile, the purpose of arranging the two-layer packed tower is to prevent channeling in the packed tower.
The mother liquor feeding position is the first plate from last of the plate tower. (ii) a
The buffer tank 11 is provided with a vacuum pumping system;
the method for removing alcohol ester from the 6-APA mother liquor comprises the following steps:
the 6-APA mother liquor enters a mother liquor tank 1, the mother liquor of 10 (+ -2) DEG C enters the tube pass of a heat exchanger A2 at the top of the tower through a feed pump, is heated to 28 (+ -2) DEG C and then enters a preheater C3 at the bottom of the tower, is heated to 40 (+ -2) DEG C and then enters a preheater A4 at the middle section of the tower, is heated to 55 (+ -2) DEG C by steam, and then is changed into a steam-liquid mixture of 41 (+ -2) DEG C through a reduced pressure distillation device 5 and enters a rectifying tower 6 from the first plate at the reciprocal of a plate tower;
the reduced pressure distillation equipment 5 is specifically a reduced pressure rectifying tower.
Meanwhile, pure water is introduced into the heater through a preheater B7, and the pure water is 47.373 multiplied by 103The steam of 80 ℃ is changed into steam in a negative pressure state, enters the rectifying tower from the tower bottom and ascends in the rectifying tower 6, heat transfer and mass transfer are completed in the rectifying tower 6, and alcohol and ester in the 6-APA mother liquor are blown to the tower top by pure water steam;
steam, alcohol and ester flowing out of the top of the rectifying tower 6 enter a shell pass of a heat exchanger A2, are cooled into liquid, enter a shell pass of a heat exchanger B9, enter a tube pass by circulating water to cool an alcohol ester solution, and a recombined water diversion enters an intermediate tank 12 from a lower pipeline; the light component alcohol and ester enter a vacuum condenser 10; condensing both the alcohol and the ester into an intermediate tank 12 at 40 ℃; the vacuum condenser 10 is connected with a buffer tank 11 through a pipeline, and the vacuum pump is connected behind the buffer tank 11, so that the whole rectification system is 47.373 multiplied by 103Pa, negative pressure state.
The water, alcohol and ester in the intermediate tank 12 at 40 (+ -2) DEG C are prepared fromMaterial passing pumpThe alcohol ester solution enters a cooler A13, and is cooled by circulating water to enter a phase separation tank 14, wherein the phase separation tank 14 contains 94% of water, 5% of alcohol and 1% of ester; water and alcohol in the phase separation tank 14 enter a butanol-removing wastewater system through a lower pipeline; ester feeding tubeAnd (4) performing extraction.
Mixed liquor (containing 6-APA, ammonium chloride and phenylacetic acid) obtained in a tower kettle after the reaction of the rectifying tower 6 enters a preheater C3, is cooled to 43 (+ -2) DEG C from 54 (+ -2) DEG C after heat exchange and then enters a cooler B15, and the mixed liquor is cooled to 25 (+ -2) DEG C from 43 (+ -2) DEG C by circulating water; then, the mixed solution enters a cooler C16, the mixed solution is cooled to 10 (+ -2) ℃ from 25 (+ -2) DEG C by low-temperature water, and finally the mixed solution of 6-APA, ammonium chloride, phenylacetic acid and the like enters a discharge tank 17.
The pure water is H2O；
The 6-APA mother liquor comprises 4-5% of butanol, 0.5% of butyl acetate, 0.05% of ammonium chloride, 90% of phenylacetic acid and 0.3% of 6-APA by mass concentration.
Example 1
The mother liquor of 6-APA of 40kmol/h enters a mother liquor tank, the mother liquor of 10 (+ -2) DEG C enters a tube pass of a heat exchanger A at the top of the tower through a feed pump, is heated to 28 (+ -2) DEG C and then enters a preheater C at the bottom of the tower, then is heated to 40 (+ -2) DEG C and enters a preheater A at the middle section of the tower, is heated to 55 (+ -2) DEG C by steam, and then is changed into a vapor-liquid mixture of 41 (+ -2) DEG C through a reduced pressure distillation device and enters a rectifying tower from a 7 th plate of a plate tower.
Pure water enters the heater through the preheater B, the pure water is changed into steam and enters the rectifying tower from the tower bottom, the diameter of the tower is 1m, and heat transfer and mass transfer are carried out in the rectifying tower. Pure water vapor blows alcohol and ester in the 6-APA mother liquor to the top of the tower.
Steam, alcohol and ester enter the shell pass of the heat exchanger A, are cooled into liquid and enter the shell pass of the heat exchanger B, circulating water enters the tube pass to cool the alcohol ester solution, and the recombined water diversion enters the intermediate tank from a lower pipeline. The light components alcohol and ester enter a vacuum condenser. Both the alcohol and the ester were condensed into the intermediate tank. The vacuum condenser is connected with the buffer tank through a pipeline, and the vacuum pump is connected behind the buffer tank, so that the whole rectification system is in a negative pressure state.
Water, alcohol and ester at 40 +/-2 deg.c in the intermediate tank are pumped into cooler A and the alcohol ester solution is cooled with circulating water into phase separating tank. Water and alcohol in the phase separation tank enter a butanol-removing wastewater system through a lower pipeline, the amount of the extracted alcohol is 2.12kmol/h, and the concentration is 99.5%. The ester is extracted from the upper pipeline, the amount of the extracted ester is 0.21kmol/h, and the concentration is 99.1%.
6-APA in the mother liquor of the rectifying tower, mixed liquor of ammonium chloride, phenylacetic acid and the like enters a preheater C from a tower kettle, the mixed liquor is cooled to 43 (+ -2) DEG C from 54 (+ -2) DEG C and then enters a cooler B, and the mixed liquor is cooled to 25 (+ -2) DEG C from 43 (+ -2) DEG C by circulating water. Then the mixed liquid enters a cooler C, the mixed liquid is cooled to 10 (+ -2) DEG C from 25 (+ -2) DEG C by low-temperature water, and finally the mixed solution of 6-APA, ammonium chloride, phenylacetic acid and the like enters a discharging tank, the discharging amount is 38.23kmol/h, the concentration of 6-APA is 0.3%, the concentration of ammonium chloride is 0.05% and the concentration of phenylacetic acid is 90%.
Through the embodiment 1, the invention can be seen that the invention realizes the high-efficiency recovery of alcohol and ester in the 6-APA cracking waste liquid, the purity of butanol and butyl acetate is more than 99.0 percent, and the recovery rate of butanol and butyl acetate is more than 95 percent.
Example 2
The other steps are the same as the example 1, except that the 6-APA mother liquor of 40kmol/h is replaced by the 6-APA mother liquor of 60kmol/h, and the tower diameter of 1m is replaced by the tower diameter of 2 m;
the amount of the finally obtained produced alcohol was 3.21kmol/h and the concentration was 99.6%. The amount of the ester produced was 0.32kmol/h and the concentration was 99.3%.
The invention is not the best known technology.
Claims (5)
1. A method for removing alcohol ester in 6-APA mother liquor is characterized by comprising the following steps:
injecting 6-APA mother liquor into a mother liquor tank, feeding the mother liquor into a tube pass of a heat exchanger A at the top of a tower through a feed pump at the temperature of 8-12 ℃, heating the mother liquor to 26-30 ℃, then feeding the mother liquor into a preheater C of a tower kettle, heating the mother liquor to 38-42 ℃, feeding the heated mother liquor into a preheater A at the middle section of the tower, heating the preheated mother liquor to 53-57 ℃ by steam, and then converting the heated mother liquor into a 39-43 ℃ steam-liquid mixture through reduced pressure distillation equipment, and feeding the steam-liquid mixture into a rectification tower from a first plate to the last of a plate tower;
meanwhile, pure water enters a heater through a preheater B, the pure water is changed into steam with the temperature of 80 ℃ in a negative pressure state, the steam enters a rectifying tower from a tower bottom and ascends in the rectifying tower, heat transfer and mass transfer are completed in the rectifying tower, and alcohol and ester in the 6-APA mother liquor are blown to the tower top by the pure water steam;
steam, alcohol and ester flowing out of the top of the rectifying tower enter a shell pass of a heat exchanger A, are cooled into liquid, enter a shell pass of a heat exchanger B, enter a tube pass by circulating water to cool an alcohol ester solution, and the recombined water is divided and enters an intermediate tank from a lower pipeline; the light component alcohol and ester enter a vacuum condenser; condensing alcohol and ester into a middle tank at 40 ℃; the vacuum condenser is connected with the buffer tank through a pipeline, the vacuum pump is connected behind the buffer tank, and the rectification system is in a negative pressure state;
feeding 38-42 ℃ water, alcohol and ester in the intermediate tank into a cooler A through a material passing pump, cooling the alcohol ester solution with circulating water into a phase separation tank, wherein the phase separation tank contains 91-97.9% of water, 2-8% of alcohol and 0.1-1% of ester; water and alcohol in the phase separation tank enter a butanol-removing wastewater system through a lower pipeline; ester is extracted from the upper pipeline;
the mixed liquid obtained in the tower kettle after the rectifying tower is reacted enters a preheater C, is cooled to 41-45 ℃ from 52-56 ℃ after being subjected to heat exchange, enters a cooler B, and is cooled to 23-27 ℃ from 41-45 ℃ by circulating water; and then, the mixed solution enters a cooler C, the mixed solution is cooled to 8-12 ℃ from 23-27 ℃ by low-temperature water, and finally the mixed solution of 6-APA, ammonium chloride, phenylacetic acid and the like enters a discharge tank.
2. The process for removing alcohol esters from 6-APA mother liquor according to claim 1, wherein said pure water is H2O。
3. The method for removing alcohol ester in 6-APA mother liquor according to claim 1, wherein the 6-APA mother liquor comprises 4-5% by mass of butanol, 0.1-1.0% by mass of butyl acetate, 0.01-0.10% by mass of ammonium chloride, 85-95% by mass of phenylacetic acid and 0.1-0.5% by mass of 6-APA.
4. The process for removing alcohol esters from 6-APA mother liquor as claimed in claim 1, wherein the rectification system is under negative pressure in the range of 40 x 103-50×103Pa。
5. A device for removing alcohol ester in 6-APA mother liquor is characterized by comprising a mother liquor tank, a feed pump, a heat exchanger A, a preheater C, a preheater A, reduced pressure distillation equipment, a rectifying tower, a heat exchanger B, a vacuum condenser, a buffer tank and a vacuum pump which are sequentially connected through pipelines;
wherein the pure water pipeline is connected with a preheater B, the preheater B is connected with a heater, and the heater is connected with the bottom of the rectifying tower; the liquid outlet end of the tower kettle of the rectifying tower is connected with a preheater C, and the preheater C is also sequentially connected with a cooler B, a discharge pump, the cooler C and a discharge tank; the preheater C is also connected with the feed inlet of the rectifying tower sequentially through the preheater A and the reduced pressure distillation equipment; the top of the rectifying tower is connected with a heat exchanger A, and the heat exchanger A is also connected with a heat exchanger B and a preheater C respectively; a discharge port at the top end of the heat exchanger B is connected with a butanol-removing wastewater system through the intermediate tank, the cooler A and the phase splitting tank in sequence; a discharge port at the bottom end of the heat exchanger B is also connected with a vacuum condenser, the vacuum condenser is also connected with a buffer tank, and the vacuum condenser and the buffer tank are also respectively connected with an intermediate tank; the mother liquor tank is connected with the heat exchanger A;
the rectifying tower is divided into an upper part and a lower part, the upper layer is a plate tower, the range of tower plates is 5-7, and the distance between plates is 40-60 cm; the lower layer is a packed tower, the packed tower is provided with 2-4 packing layers, the height of each packing layer is 1-4 m, and the packing is the same;
the mother liquor feeding position is the first plate from the last of the plate tower;
the buffer tank is also connected with a vacuum pump.
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