CN111569808A - Energy integrated utilization bulk drug reaction purification system and process method thereof - Google Patents
Energy integrated utilization bulk drug reaction purification system and process method thereof Download PDFInfo
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Abstract
The invention discloses a bulk drug reaction purification system for energy integrated utilization, which is characterized in that a normal-temperature glycol is added in the traditional bulk drug reaction purification system, and the heat to be absorbed by gasifying and heating process material flow liquid ammonia is matched with the normal-temperature glycol to generate low-temperature glycol required by a crystallization kettle; high-grade heat released by liquefaction of the gaseous solvent is absorbed by circulating water to generate hot water with a lower temperature, and the hot water is supplied to a second reaction kettle for use; the low-temperature glycol at the outlet of the crystallization kettle has lower temperature than the low-temperature water, and has higher grade as a refrigerant, so the low-temperature glycol can replace the low-temperature water. The purification system of the invention effectively reduces the use amount of low-temperature glycol, hot water and low-temperature water, further utilizes the residual energy and also reduces the consumption of public works. The invention also discloses a raw material medicine reaction purification process method for energy integrated utilization, which has low energy consumption, saves energy, reduces emission, protects the environment and reduces the cost.
Description
Technical Field
The invention relates to the technical field of production of raw material medicines, in particular to a raw material medicine reaction purification system for energy integrated utilization and a process method thereof.
Background
The production of pharmaceutical and chemical industry consumes a lot of energy, and the current society is facing a severe examination of energy shortage. With the development of social economy, people increasingly demand fine chemicals such as medical products, and how to effectively reduce energy consumption in production is an urgent problem to be solved.
The method for producing itraconazole bulk drug disclosed in chinese patent CN201710717004.5 adopts three step temperatures of the same heat exchange medium to control the temperature change of the liquid in each reactor, and adopts a buffer transition and temperature change mode when the temperature gradient changes greatly during the switching process of the reactor material, so as to avoid the influence of the temperature shock and the uneven heat transfer of the reaction liquid and the rigid fission influence of the equipment caused by the phase change of the heat exchange medium in the jacket or the shock heat stimulation. The utility consumption is reduced by 14.3%. However, this patent achieves the purpose of temperature control of the reaction vessel by switching the three temperature steps of high, medium and low (140 ℃, 20 ℃ and-10 ℃), and although the use of a medium of a suitable temperature can avoid a part of energy waste, the reduction of utility consumption is limited due to the lack of effective energy exchange between the media of different temperature gradients.
Most of the raw material medicines are produced in an intermittent operation process, and the intermittent process has the characteristics of small batch, multiple varieties, high added value, complex synthesis steps, fast product updating and the like, so that the intermittent process has particularity in the aspect of energy utilization. The dependence of each logistics on time is strong, the process parameters are complex, and mathematical description is difficult; the energy consumption changes along with time, and the energy consumption is intermittent, wherein direct energy recovery and indirect energy recovery are considered, and an intermediate storage is arranged. These characteristics make it difficult to find a simple and feasible batch process energy comprehensive optimization method, and the existing batch process energy comprehensive optimization model is complicated. With the increasingly tense and sustainable development of energy situation, the comprehensive optimization of energy in the intermittent process is more and more emphasized.
Wangma and the like (an energy comprehensive optimization strategy [ J ] of an intermittent chemical process, computer and applied chemistry, 2009) provides a simple and feasible method suitable for intermittent process energy comprehensive optimization based on a three-link model of energy consumption analysis in a continuous process according to related constraint relations of an intermittent process recovery link and an energy utilization link, and performs analysis and energy comprehensive integrated optimization on a polyester resin production process. However, methods based on pinch analysis have resulted from improvements to continuous process pinch techniques. Due to the characteristics of the batch process and its complexity and time variability, the method has certain limitations in the application of the energy comprehensive optimization of the batch process.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a raw material medicine reaction purification system for energy integrated utilization and a process method thereof, aiming at the difference of energy grades in public works used by all equipment, residual energy is integrated and utilized, so that the waste of the residual energy and the harm of emission to the environment are reduced, the using amount of a public work medium is effectively reduced, the energy is saved, the emission is reduced, the environment is protected, and the cost is reduced.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides a bulk drug reaction purification system for energy integrated utilization, which comprises a first reaction kettle, a second reaction kettle, a distillation kettle and a crystallization kettle which are connected in sequence; the bottom and the top of the outer interlayer space of the first reaction kettle are respectively provided with a normal-temperature ethylene glycol inlet and a low-temperature ethylene glycol outlet; the bottom and the top of the outer interlayer space of the second reaction kettle are respectively provided with a hot water inlet and a low-temperature water outlet; the bottom and the top of the interlayer space outside the crystallization kettle are respectively provided with a low-temperature ethylene glycol inlet and a secondary low-temperature ethylene glycol outlet;
the normal-temperature ethylene glycol inlet is connected with the bottom of the ethylene glycol storage tank, and the low-temperature ethylene glycol outlet is connected with the low-temperature ethylene glycol inlet; the hot water inlet is connected with a shell pass circulating water outlet of the condenser; the secondary low-temperature ethylene glycol outlet is connected with a shell pass secondary low-temperature ethylene glycol inlet arranged at the bottom of the cooler, and a shell pass normal-temperature ethylene glycol outlet arranged at the top of the cooler is connected with the top of the ethylene glycol storage tank; a solvent steam outlet at the top of the distillation kettle is sequentially connected with the condenser and the tube side of the cooler;
the connections are all pipeline connections.
Further, the outer interlayer space of the distillation kettle is heated in a mode of introducing steam.
Furthermore, a shell pass circulating water inlet of the condenser is connected with external cooling water.
Further, the low-temperature water of the second reaction kettle is returned to a public engineering center through the low-temperature water outlet.
The second aspect of the invention provides a process method for the reaction and purification of bulk drugs with integrated utilization of energy, which comprises the following steps:
s1: putting reactants into the first reaction kettle, reacting at-35 ℃ until the reaction is finished, introducing normal-temperature ethylene glycol from the normal-temperature ethylene glycol inlet to raise the temperature in the first reaction kettle to-20 ℃, simultaneously introducing low-temperature ethylene glycol discharged from the low-temperature ethylene glycol outlet into an interlayer space outside the crystallization kettle through a pipeline, and then sending a reaction product after temperature rise to the second reaction kettle;
s2: the second reaction kettle is heated by hot water discharged from a shell pass circulating water outlet of the condenser, a reaction product obtained in the step S1 is subjected to secondary reaction, and the reaction product is sent to the distillation kettle after the reaction is finished;
s3: distilling the distillation kettle to completely evaporate the solvent in the distillation kettle, condensing circulating water at 32 ℃ in the condenser in sequence through a pipeline, cooling the circulating water at 7 ℃ in the cooler to 25 ℃, and finally entering a collecting tank;
s4: the distillation residues in the distillation kettle are fed into the crystallization kettle, the low-temperature ethylene glycol at minus 15 ℃ entering from the low-temperature ethylene glycol inlet is cooled, and the subsequent working section is carried out after the crystallization is finished; meanwhile, the secondary low-temperature glycol sent out from the secondary low-temperature glycol outlet enters the shell side of the cooler.
Further, in step S1, the substance to be charged into the first reaction vessel further includes liquid ammonia at-35 ℃.
Further, in step S2, the temperature of the hot water is 85 ℃.
Further, in step S3, the distillation still employs steam heating distillation at 143 ℃.
Further, in step S4, the subsequent section is a separation section.
By adopting the technical scheme, compared with the prior art, the invention has the following technical effects:
compared with the traditional bulk drug reaction purification system, the purification system provided by the invention adds a stream of normal-temperature ethylene glycol, and the heat to be absorbed by gasifying and heating process stream liquid ammonia is matched with the normal-temperature ethylene glycol to generate low-temperature ethylene glycol required by a crystallization kettle; high-grade heat released by liquefaction of the gaseous solvent is absorbed by circulating water to generate hot water with a lower temperature, and the hot water is supplied to a second reaction kettle (R02); the low-temperature glycol at the outlet of the crystallization kettle has lower temperature than the low-temperature water, and has higher grade as a refrigerant, so that the low-temperature glycol can replace the low-temperature water; the purification system effectively reduces the use amount of low-temperature glycol, hot water and low-temperature water, further utilizes the residual energy and also reduces the consumption of public works.
Drawings
FIG. 1 is a flow diagram of a conventional bulk drug reaction purification system;
FIG. 2 is a flow chart of the bulk drug reaction purification system for integrated energy utilization according to the present invention;
wherein the reference numerals are:
a first reaction vessel 1; a second reaction kettle 2; a distillation kettle 3; a crystallization kettle 4; a condenser 5; a cooler 6; a glycol storage tank 7; a solvent vapor outlet 8; a normal temperature ethylene glycol inlet 9; a low temperature ethylene glycol outlet 10; a hot water inlet 11; a low temperature water outlet 12; a low temperature ethylene glycol inlet 13; a secondary low temperature ethylene glycol outlet 14; a second low temperature ethylene glycol inlet 15; a normal temperature ethylene glycol outlet 16; a circulating water outlet 17; a circulating water inlet 18.
Detailed Description
As shown in fig. 2, the invention provides a bulk drug reaction purification system with integrated energy utilization, which comprises a first reaction kettle 1, a second reaction kettle 2, a distillation kettle 3 and a crystallization kettle 4 which are connected in sequence; the bottom and the top of the outer interlayer space of the first reaction kettle 1 are respectively provided with a normal-temperature ethylene glycol inlet 9 and a low-temperature ethylene glycol outlet 10; the bottom and the top of the outer interlayer space of the second reaction kettle 2 are respectively provided with a hot water inlet 11 and a low-temperature water outlet 12; the bottom and the top of the interlayer space outside the crystallization kettle 4 are respectively provided with a low-temperature ethylene glycol inlet 13 and a secondary low-temperature ethylene glycol outlet 14;
a normal-temperature ethylene glycol inlet 9 is connected with the bottom of the ethylene glycol storage tank 7, and a low-temperature ethylene glycol outlet 10 is connected with a low-temperature ethylene glycol inlet 13; the hot water inlet 11 is connected with a shell pass circulating water outlet 17 of the condenser 5; a secondary low-temperature ethylene glycol outlet 14 is connected with a shell pass secondary low-temperature ethylene glycol inlet 15 arranged at the bottom of the cooler 6, and a shell pass normal-temperature ethylene glycol outlet 16 arranged at the top of the cooler 6 is connected with the top of the ethylene glycol storage tank 7; a solvent steam outlet 8 at the top of the distillation kettle 3 is sequentially connected with a condenser 5 and a tube pass of a cooler 6;
the connections are all pipeline connections.
Further, the outer interlayer space of the distillation kettle 3 is heated in a mode of introducing steam; a shell pass circulating water inlet 18 of the condenser 5 is connected with external cooling water; the low temperature water of the second reaction vessel 2 is returned to the utility center through its low temperature water outlet 12.
The raw material medicine reaction purification process method adopting the system comprises the following steps:
s1: putting reactants and liquid ammonia at the temperature of minus 35 ℃ into a first reaction kettle 1, reacting at the temperature of minus 35 ℃ until the reaction is finished, introducing normal-temperature ethylene glycol from a normal-temperature ethylene glycol inlet 9 to increase the temperature in the first reaction kettle 1 to minus 20 ℃, simultaneously introducing low-temperature ethylene glycol discharged from a low-temperature ethylene glycol outlet 10 into an interlayer space outside a crystallization kettle 4 through a pipeline, and then sending a reaction product after temperature rise to a second reaction kettle 2;
s2: hot water at 85 ℃ is discharged from a shell pass circulating water outlet 17 of the condenser 5 to heat the second reaction kettle 2, a reaction product obtained in S1 is subjected to secondary reaction, and the reaction product is sent to the distillation kettle 3 after the reaction is finished;
s3: heating and distilling the distillation kettle 3 by adopting steam at 143 ℃ to completely distill out the solvent in the kettle, condensing the circulating water at 32 ℃ in a condenser 5 and cooling the circulating water at 7 ℃ in a cooler 6 to 25 ℃ through a pipeline in sequence, and finally feeding the circulating water into a collection tank;
s4: the distillation residues in the distillation kettle 3 are sent into a crystallization kettle 4, the ethylene glycol with the temperature of-15 ℃ is cooled through a low-temperature ethylene glycol inlet 13, and the ethylene glycol enters a subsequent separation working section after the crystallization is finished; meanwhile, the second low-temperature glycol sent out from the second low-temperature glycol outlet 14 enters the shell side of the cooler 6.
The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
Comparative example
As shown in fig. 1, the comparative example provides a traditional bulk drug reaction purification system, which comprises a first reaction kettle 1, a second reaction kettle 2, a distillation kettle 3 and a crystallization kettle 4 which are connected in sequence; a solvent steam outlet 8 at the top of the distillation kettle 3 is sequentially connected with a condenser 5 and a tube pass of a cooler 6; the water inlets of the condenser 5 and the cooler 6 are both externally connected with a water source, and the water outlets are both emptied.
The raw material medicine reaction purification process method adopting the traditional system comprises the following steps: s1: putting reactants into a first reaction kettle 1(R01), introducing liquid ammonia at-35 ℃ for cooling, reacting the reactants at-35 ℃ until the reaction is finished, discharging the gasified liquid ammonia gas, and conveying reaction products to a second reaction kettle 2(R02) when the temperature in the reaction kettle is raised to be higher than-20 ℃; s2: heating the reaction product in R02 with hot water at 85 deg.C for secondary reaction, and transferring to distillation still (R03) after the reaction; s3: heating and distilling with steam at 143 deg.C to completely distill out solvent in distillation kettle (R03), sequentially condensing with circulating water at 32 deg.C in condenser 5(E01) and cooling with low temperature water at 7 deg.C in cooler 6(E02) to 25 deg.C via pipeline, and finally feeding into collection tank; s3: the distillation residue enters a crystallization kettle 4(R04) for crystallization, the system is cooled by glycol at the low temperature of 15 ℃ below zero, and the subsequent separation stage is carried out after the crystallization is finished.
In the process of the reaction and purification of the bulk drugs, strict requirements are imposed on the temperature, all equipment needs public works, and all related public works are supplied by a factory in a unified way. The specific consumption is shown in Table 1.
TABLE 1 consumption of utilities in conventional Process
The above process requires the public works of heating medium and cooling medium, and the target temperature of each medium is different, and the medium gasification heat absorption is also involved. Therefore, by integrally utilizing the residual energy, the consumption of the public works can be reduced by matching the use hot spot with the release hot spot.
The reusable energy is calculated according to the energy calculation formula (1), and the calculation result is shown in table 2.
Q＝m×CP×(T1-T2)+m×r -----(1)
Q: total amount of energy kJ
m: mass kg of substance
CP: constant pressure hot melt kJ/kg. deg.C
T1: original temperature C
T2: target temperature C
r: heat of vaporization kJ/kg
TABLE 2 conventional Process energy reuse
From table 2 it can be seen that for a cooling utility, the vaporization of liquid ammonia absorbs a lot of heat, and the low temperature ethylene glycol (-15 ℃) grade is higher relative to another cooling utility, while the low temperature ethylene glycol outlet temperature for cooling R04 is 0 ℃, and the grade is also higher relative to the low temperature water (7 ℃), so that this energy can be reused theoretically. Similarly, the energy grade of the solvent (120 ℃ C. and 100 ℃ C. respectively) in E01 and E02 is higher than that of the heating public engineering hot water (85 ℃ C.) used in R02, so that the effective energy can be further utilized by heat exchange.
Example 1
In this embodiment: and (3) adding an ethylene glycol storage tank for cold in the process material flow liquid ammonia, and storing a certain amount of normal-temperature ethylene glycol as an intermediate medium for exchanging heat required by gasification and temperature rise of the liquid ammonia in the R01. In the heat exchange process, the flow rate of the circulating water in E01 is controlled to increase the outlet temperature of the circulating water to 85 ℃, and the circulating water is distributed to R02 for use, so that the use of hot water in the public works is reduced. The low-temperature ethylene glycol used by R04 is recycled to the outlet and directly distributed to E02 for use instead of low-temperature water. And adjusting the production time of each device to enable the energy matching devices to produce simultaneously. The method comprises the following specific steps:
s1: putting reactants and liquid ammonia at the temperature of minus 35 ℃ into a first reaction kettle 1, reacting at the temperature of minus 35 ℃ until the reaction is finished, introducing normal-temperature ethylene glycol from a normal-temperature ethylene glycol inlet 9 to increase the temperature in the first reaction kettle 1 to minus 20 ℃, simultaneously introducing low-temperature ethylene glycol discharged from a low-temperature ethylene glycol outlet 10 into an interlayer space outside a crystallization kettle 4 through a pipeline, and then sending a reaction product after temperature rise to a second reaction kettle 2;
s2: hot water at 85 ℃ is discharged from a shell pass circulating water outlet 17 of the condenser 5 to heat the second reaction kettle 2, a reaction product obtained in S1 is subjected to secondary reaction, and the reaction product is sent to the distillation kettle 3 after the reaction is finished;
s3: heating and distilling the distillation kettle 3 by adopting steam at 143 ℃ to completely distill out the solvent in the kettle, condensing the circulating water at 32 ℃ in a condenser 5 and cooling the circulating water at 7 ℃ in a cooler 6 to 25 ℃ through a pipeline in sequence, and finally feeding the circulating water into a collection tank;
s4: the distillation residues in the distillation kettle 3 are sent into a crystallization kettle 4, the ethylene glycol with the temperature of-15 ℃ is cooled through a low-temperature ethylene glycol inlet 13, and the ethylene glycol enters a subsequent separation working section after the crystallization is finished; meanwhile, the second low-temperature glycol sent out from the second low-temperature glycol outlet 14 enters the shell side of the cooler 6.
The remaining high grade energy listed in the proportional table 2 is re-used in the form of regenerative utilities. The regenerated low-temperature ethylene glycol is calculated according to the heat balance formulas (2) and (3), and the mass of hot water is shown in a table 3:
Q＝m1×CP1×(T1-T2)/ti1＝m2×CP2×(t1-t2)/ti2——(2)
Qi＝Q×tii——(3)
q: total amount of energy kJ per unit time
Qi: total amount of energy kJ
m1、m2: mass kg of substance
CP1、CP2: constant pressure hot melt kJ/kg. deg.C
T1、t1: original temperature C
T2、t2: target temperature C
ti1、ti2: reaction time min
TABLE 3 New Utility project with heat exchange generation
Distributing the public works obtained by energy exchange to required equipment, replacing low-temperature water with low-temperature ethylene glycol recycled, and calculating the saving ratio of each public work according to a formula (4), wherein the saving ratio is specifically shown in table 4.
I＝(m/m0)×(ti0/ti)×100％ ——(4)
I: saving ratio
m: newly created utility mass kg
m0: original public work mass kg
ti: reaction time min for the creation of a new utility
ti0: reaction time min of the matching apparatus
TABLE 4 Utility savings after Process adjustments
By redistribution of public works, the energy of 1095100kJ can be reused theoretically, the low-temperature glycol is saved by 7262.50kg and 36.50%, the hot water is saved by 590.45kg and 8.70%, and the low-temperature water is saved by 66000kg and 100%.
The invention adds a stream of normal temperature ethylene glycol to match the heat absorbed by the gasification and heating of the process stream liquid ammonia to generate the low temperature ethylene glycol required by the crystallization kettle. The high-grade heat released by the liquefaction of the gaseous solvent is absorbed by the circulating water to generate hot water with a lower temperature, and the hot water is supplied to the reaction kettle 2 (R02). The low-temperature glycol at the outlet of the crystallization kettle (R04) has lower temperature than the low-temperature water, and has higher grade as a refrigerant, so the low-temperature glycol can replace the low-temperature water. Through the adjustment, the use amount of the low-temperature glycol, the hot water and the low-temperature water is effectively reduced. Not only is surplus energy utilized even further, but utility consumption is also reduced.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (9)
1. A bulk drug reaction purification system for energy integrated utilization is characterized by comprising a first reaction kettle (1), a second reaction kettle (2), a distillation kettle (3) and a crystallization kettle (4) which are connected in sequence; the bottom and the top of the outer interlayer space of the first reaction kettle (1) are respectively provided with a normal-temperature ethylene glycol inlet (9) and a low-temperature ethylene glycol outlet (10); the bottom and the top of the outer interlayer space of the second reaction kettle (2) are respectively provided with a hot water inlet (11) and a low-temperature water outlet (12); the bottom and the top of the interlayer space outside the crystallization kettle (4) are respectively provided with a low-temperature ethylene glycol inlet (13) and a secondary low-temperature ethylene glycol outlet (14);
the normal-temperature ethylene glycol inlet (9) is connected with the bottom of the ethylene glycol storage tank (7), and the low-temperature ethylene glycol outlet (10) is connected with the low-temperature ethylene glycol inlet (13); the hot water inlet (11) is connected with a shell pass circulating water outlet (17) of the condenser (5); the secondary low-temperature ethylene glycol outlet (14) is connected with a shell-side secondary low-temperature ethylene glycol inlet (15) arranged at the bottom of the cooler (6), and a shell-side normal-temperature ethylene glycol outlet (16) arranged at the top of the cooler (6) is connected with the top of the ethylene glycol storage tank (7); a solvent steam outlet (8) at the top of the distillation kettle (3) is sequentially connected with the condenser (5) and the tube pass of the cooler (6);
the connections are all pipeline connections.
2. The bulk drug reaction and purification system with integrated energy utilization of claim 1, wherein the outer interlayer space of the distillation still (3) is heated by introducing steam.
3. The bulk drug reaction and purification system for integrated energy utilization according to claim 1, wherein a shell-side circulating water inlet (18) of the condenser (5) is connected with external cooling water.
4. The bulk drug reaction and purification system for energy integrated utilization according to claim 1, wherein the low-temperature water in the second reaction kettle (2) is returned to a public engineering center through the low-temperature water outlet (12).
5. A bulk drug reaction purification process method adopting the system of any one of claims 1-4, characterized by comprising the following steps:
s1: putting reactants into the first reaction kettle (1), reacting at-35 ℃ until the reaction is finished, introducing normal-temperature ethylene glycol from the normal-temperature ethylene glycol inlet (9), raising the temperature in the first reaction kettle (1) to-20 ℃, simultaneously introducing low-temperature ethylene glycol discharged from the low-temperature ethylene glycol outlet (10) into an interlayer space outside the crystallization kettle (4) through a pipeline, and then sending a reaction product after temperature rise to the second reaction kettle (2);
s2: the second reaction kettle (2) is heated by hot water discharged from a shell pass circulating water outlet (17) of the condenser (5), a reaction product obtained from S1 is subjected to secondary reaction, and the reaction product is sent to the distillation kettle (3) after the reaction is finished;
s3: distilling the distillation kettle (3) to completely evaporate the solvent in the kettle, condensing circulating water at 32 ℃ in the condenser (5) in sequence through a pipeline, cooling the circulating water at 7 ℃ in the cooler (6) to 25 ℃, and finally feeding the circulating water into a collecting tank;
s4: the distillation residues in the distillation kettle (3) are sent into the crystallization kettle (4), the ethylene glycol with the temperature of-15 ℃ entering from the low-temperature ethylene glycol inlet (13) is cooled, and the ethylene glycol enters a subsequent working section after crystallization is finished; meanwhile, the secondary low-temperature glycol sent out from the secondary low-temperature glycol outlet (14) enters the shell side of the cooler (6).
6. The process according to claim 5, wherein in step S1, the material charged into the first reaction vessel (1) further comprises liquid ammonia at-35 ℃.
7. The process of claim 5, wherein in step S2, the temperature of the hot water is 85 ℃.
8. The process of claim 5, wherein in step S3, the distillation still (3) is heated and distilled by steam at 143 ℃.
9. A process according to claim 5, characterized in that in step S4, said subsequent station is a separation station.
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| CN107321277A (en) * | 2017-08-05 | 2017-11-07 | 德莱创节能科技（苏州）有限公司 | A kind of synthetic latex resource recovering system |
| WO2020041535A1 (en) * | 2018-08-22 | 2020-02-27 | Johnson Ip Holding, Llc | Exhaust gas energy recovery converter |
| CN110433758A (en) * | 2019-08-23 | 2019-11-12 | 安徽广信农化股份有限公司 | A kind of hexazinone crystallization reactor |
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