CN217367797U - Mixed acid separation system - Google Patents
Mixed acid separation system Download PDFInfo
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- CN217367797U CN217367797U CN202221344312.0U CN202221344312U CN217367797U CN 217367797 U CN217367797 U CN 217367797U CN 202221344312 U CN202221344312 U CN 202221344312U CN 217367797 U CN217367797 U CN 217367797U
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Abstract
The application provides a mixed acid separation system, through the combined action of a mixed acid storage tank, a film evaporator, a distillation still, a hydrochloric acid condenser, a sulfuric acid storage tank, a hydrochloric acid intermediate storage tank and a hydrochloric acid transfer pump, hydrochloric acid in the mixed acid is subjected to vaporization separation by using the film evaporator, is condensed and recovered to the hydrochloric acid intermediate storage tank by using the hydrochloric acid condenser, and is transferred to the hydrochloric acid condenser by using the hydrochloric acid transfer pump to circularly absorb hydrochloric acid gas again, so that the concentration of the recovered hydrochloric acid is improved; meanwhile, the sulfuric acid in the mixed acid is purified by secondary distillation in the distillation kettle, so that the purity of the sulfuric acid is improved, and the recovery efficiency of the mixed acid is also improved. By utilizing the mixed acid separation system, the sulfuric acid and the hydrochloric acid in the mixed acid are separated thoroughly, the hydrogen chloride in the system is absorbed thoroughly, and the concentration of the recovered hydrochloric acid is high, so that the acid content of the tail gas in the perchloromethylmercaptan production and the treatment load of a vacuum unit and a tail gas system can be reduced.
Description
Technical Field
The application relates to the technical field of mixed acid separation, in particular to a mixed acid separation system.
Background
The perchloromethylmercaptan is an important intermediate raw material of pesticide bactericides such as captan, folpet, hymexazol and the like, although the pesticide varieties are old, the pesticide varieties are sold by ten thousand tons in the international market every year, and the perchloromethylmercaptan is difficult to replace by modern new-variety agricultural bactericides. At present, the production methods of perchloromethylmercaptan (i.e. PMM) are few, carbon disulfide, dilute hydrochloric acid and chlorine are commonly used as raw materials to prepare the perchloromethylmercaptan through chlorination, and the technological process comprises the following steps:
chlorine is added into a chlorination reaction kettle, then carbon disulfide is added, and reaction is carried out under the action of water. In the reaction, 1 molecule of carbon disulfide and 5 molecules of chlorine gas are subjected to chlorination reaction to generate 1 molecule of perchloromethylmercaptan, 6 molecules of hydrogen chloride (the hydrogen chloride is dissolved in water to form hydrochloric acid) and 1 molecule of sulfuric acid. Therefore, a large amount of mixture of sulfuric acid and hydrochloric acid, i.e., mixed acid, is generated after the reaction is completed, and the yield of the mixed acid is huge, and if the mixed acid is not separated and recovered, serious problems of environmental pollution and resource waste are caused. The existing recovery method is to directly input the mixed acid into a distillation still, separate hydrochloric acid and sulfuric acid after vacuum pumping, pressure reduction, heating and concentration are carried out by using a vacuum unit, then directly purify the tail gas pumped out by the vacuum unit by using a tail gas system, and finally discharge the purified tail gas into the air. However, the concentration of the acid recovered in the mode is low, and the distilled hydrogen chloride is not completely absorbed, so that the acid content in the tail gas is high, and the processing load of a vacuum unit and a tail gas system is large.
SUMMERY OF THE UTILITY MODEL
The application provides a mixed acid separation system for when solving the above-mentioned mixed acid that produces in the current method separation perchloromethane mercaptan production process, retrieve that hydrochloric acid concentration is low and the chlorine hydride absorption is not thorough in the system and cause the acid content height in the tail gas, the big problem of vacuum unit and tail gas system treatment load.
The application provides a mixed acid separation system, includes: a mixed acid storage tank, a thin film evaporator, a hydrochloric acid condenser and a hydrochloric acid intermediate storage tank which are sequentially connected in series by a process pipeline;
the thin film evaporator comprises a thin film evaporator body, a mixed acid feeding port, a hydrochloric acid gas outlet and a liquid discharging port; the mixed acid feeding port is arranged at the top of the upper end enclosure of the film evaporator body; the hydrochloric acid gas outlet is arranged on one side surface of the upper end socket of the film evaporator body, which is far away from the mixed acid feeding port, and is connected with the hydrochloric acid condenser; the liquid outlet is arranged at the bottom of the thin film evaporator body and is connected with a distillation kettle;
the distillation kettle is respectively connected with a sulfuric acid storage tank and a hydrochloric acid condenser;
the hydrochloric acid intermediate storage tank is connected with a hydrochloric acid transfer pump; the hydrochloric acid transferring pump is connected with the hydrochloric acid condenser through a circulating pipeline and is used for pumping the hydrochloric acid in the hydrochloric acid intermediate storage tank into the hydrochloric acid condenser again.
Optionally, a steam preheater is arranged between the mixed acid storage tank and the thin film evaporator.
Optionally, a mixed acid transfer pump is arranged between the mixed acid storage tank and the steam preheater.
Optionally, the hydrochloric acid turnover storage tank is connected with the circulating pipeline through a hydrochloric acid turnover pipeline, and a three-way valve is arranged at the joint of the circulating pipeline and the hydrochloric acid turnover pipeline.
Optionally, the sulfuric acid storage tank is provided with a sulfuric acid level meter;
a sulphuric acid automatic control valve is arranged between the distillation still and the sulphuric acid storage tank and is connected with a sulphuric acid liquid level meter.
Optionally, the hydrochloric acid intermediate storage tank is provided with a hydrochloric acid liquid level meter;
a hydrochloric acid automatic control valve is arranged between the hydrochloric acid condenser and the hydrochloric acid intermediate storage tank, and the hydrochloric acid automatic control valve is connected with a hydrochloric acid liquid level meter.
Optionally, the distillation kettle comprises a distillation kettle barrel body, an exhaust port, a nitrogen port, a discharge port, a sampling port, an acid inlet, a stirring paddle, a jacket water inlet, a jacket water outlet, a sulfuric acid liquid outlet and a distillation kettle upper end enclosure;
the barrel body of the distillation kettle is connected with the upper end socket of the distillation kettle through a flange;
the exhaust port, the nitrogen port, the discharge port, the sampling port and the acid inlet are distributed at the top of the upper end enclosure of the distillation kettle;
the exhaust port is connected with a hydrochloric acid condenser;
the stirring paddle is arranged inside the barrel body of the distillation kettle;
the jacket covers the outer side of the distillation kettle barrel body, the jacket water inlet is arranged at the bottom of the jacket, and the jacket water outlet is arranged at one side of the jacket close to the distillation kettle upper end enclosure;
the sulfuric acid outlet is arranged at the bottom of the distillation kettle barrel body.
Optionally, the mixed acid material transfer pump is a magnetic pump lined with fluoroplastic.
In practical use, mixed acid formed by sulfuric acid and hydrochloric acid generated in the production of perchloromethylmercaptan is input into a mixed acid storage tank for storage, the mixed acid in the mixed acid storage tank is pumped into a thin film evaporator through a mixed acid transfer pump, the mixed acid enters the thin film evaporator body from a mixed acid feeding port at the top of the thin film evaporator body, under the action of gravity and airflow, the mixed acid forms a uniform film on a tower plate in the thin film evaporator body and flows from top to bottom, moisture in the mixed acid is heated and vaporized in the flowing process, and forms hydrochloric acid gas together with hydrogen chloride in the mixed acid, the hydrochloric acid gas is output from a hydrochloric acid gas outlet of the thin film evaporator and enters a hydrochloric acid condenser, water vapor in the hydrochloric acid gas is condensed into water, and meanwhile, the condensed water absorbs the hydrogen chloride in the hydrochloric acid gas to form hydrochloric acid which is input into a hydrochloric acid intermediate storage tank for temporary storage. The hydrochloric acid transferring pump pumps the hydrochloric acid in the hydrochloric acid intermediate storage tank into the hydrochloric acid condenser again to absorb hydrochloric acid gas, and the hydrochloric acid gas is circulated, so that the concentration of the hydrochloric acid in the hydrochloric acid intermediate storage tank is increased until the concentration of the hydrochloric acid in the hydrochloric acid intermediate storage tank reaches a preset concentration, such as 25-30%. The hydrochloric acid reaching the preset concentration in the hydrochloric acid intermediate storage tank can be transferred out for storage, or can be used for supplying hydrochloric acid to other workshops needing hydrochloric acid in a factory, such as a production workshop of perchloromethylmercaptan, or can be packaged into a product for sale.
According to the mixed acid separation system, through the combined action of the mixed acid storage tank, the film evaporator, the distillation still, the hydrochloric acid condenser, the sulfuric acid storage tank, the hydrochloric acid intermediate storage tank and the hydrochloric acid transfer pump, hydrochloric acid in the mixed acid is subjected to vaporization separation by using the film evaporator, is condensed and recovered to the hydrochloric acid intermediate storage tank by using the hydrochloric acid condenser, and is transferred to the hydrochloric acid condenser by using the hydrochloric acid transfer pump to circularly absorb hydrochloric acid gas again, so that the concentration of the recovered hydrochloric acid is improved; simultaneously, sulfuric acid in the mixed acid is purified by secondary distillation of a distillation still (for example, the purity of the available sulfuric acid is 85-90%), the purity of the sulfuric acid is improved, and the recovery efficiency of the mixed acid is also improved.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is a schematic diagram of a mixed acid separation system according to an embodiment of the present disclosure;
FIG. 2 is a schematic view of a mixed acid separation system according to another embodiment of the present disclosure;
FIG. 3 is a schematic view of a mixed acid separation system according to yet another embodiment of the present application;
fig. 4 is a schematic structural diagram of a distillation still according to an embodiment of the present disclosure.
Description of reference numerals:
1. a mixed acid storage tank;
2. a thin film evaporator;
201. a thin film evaporator body;
202. a mixed acid feeding port;
203. a hydrochloric acid gas outlet;
204. a liquid discharge port;
3. a distillation kettle;
301. a distillation still barrel;
302. an exhaust port;
303. a nitrogen port;
304. a discharge port;
305. a sampling port;
306. an acid inlet;
307. a stirring paddle;
308. a jacket;
309. a jacket water inlet;
310. a jacket water outlet;
311. a sulfuric acid outlet;
312. sealing the upper end of the distillation kettle;
31. a sulfuric acid self-control valve;
4. a hydrochloric acid condenser;
41. a hydrochloric acid automatic control valve;
5. a sulfuric acid storage tank;
51. a sulfuric acid level meter;
6. a hydrochloric acid intermediate storage tank;
61. a hydrochloric acid level meter;
7. a mixed acid transfer pump;
71. a three-way valve;
8. a hydrochloric acid turnover storage tank;
81. a hydrochloric acid transfer pipeline;
9. a hydrochloric acid transfer pump;
91. a circulating pipeline;
10. a steam preheater.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application are clearly and completely described below, and it is obvious that the described embodiments are a part of the embodiments of the present application, but not all of the embodiments. All other embodiments obtained by a person of ordinary skill in the art based on the embodiments in the present application without making any creative effort also belong to the protection scope of the present application.
As shown in fig. 1, the present application provides a mixed acid separation system comprising:
a mixed acid storage tank 1, a thin film evaporator 2, a hydrochloric acid condenser 4 and a hydrochloric acid intermediate storage tank 6 which are sequentially connected in series by a process pipeline;
the thin film evaporator 2 comprises a thin film evaporator body 201, a mixed acid feeding port 202, a hydrochloric acid gas outlet 203 and a liquid outlet 204; the mixed acid feeding port 202 is arranged at the top of the upper end enclosure of the thin film evaporator body 201; the hydrochloric acid gas outlet 203 is arranged on one side surface of the upper end socket of the film evaporator body 201 far away from the mixed acid feeding port 202 and is connected with the hydrochloric acid condenser 4; the liquid outlet 204 is arranged at the bottom of the thin film evaporator body 201 and is connected with the distillation kettle 3;
the distillation kettle 3 is respectively connected with a sulfuric acid storage tank 5 and a hydrochloric acid condenser 4;
the hydrochloric acid intermediate storage tank 6 is connected with a hydrochloric acid transferring pump 9; the hydrochloric acid transferring pump 9 is connected with the hydrochloric acid condenser 4 through a circulating pipeline 91 and is used for pumping the hydrochloric acid in the hydrochloric acid intermediate storage tank 6 into the hydrochloric acid condenser 4 again.
In the application, the mixed acid is generated in the production process of perchloromethylmercaptan, the production of the perchloromethylmercaptan is generated by the reaction of carbon disulfide and chlorine in the presence of hydrochloric acid, and the reaction formula is as follows:
CS 2 +5Cl 2 +4H 2 O→CCl 4 S+6HCl+H 2 SO 4 。
in the reaction, 1mol of carbon disulfide and 5mol of chlorine gas are subjected to chlorination reaction to generate 1mol of perchloromethylmercaptan, 6mol of hydrogen chloride (the hydrogen chloride is dissolved in water to form hydrochloric acid) and 1mol of sulfuric acid. Therefore, a large amount of mixed acid formed from sulfuric acid and hydrochloric acid is generated after the reaction is completed, and the mixed acid is output from the production section of perchloromethylmercaptan to the mixed acid storage tank 1 to be stored.
The film evaporator 2 is used for heating the mixed acid in the mixed acid storage tank 1 to evaporate hydrochloric acid in the mixed acid to generate hydrochloric acid gas, so that the hydrochloric acid is separated from the mixed acid, and the film evaporator 2 has the characteristics of high efficiency and energy saving. In order to improve the film evaporation effect, the operating pressure in the film evaporator 2 is negative pressure, such as-0.06 to-0.09 Mpa.
The distillation kettle 3 is used for carrying out secondary distillation on the sulfuric acid output from the thin film evaporator 2 (primary distillation purification is carried out in the thin film evaporator 2), and further evaporating hydrochloric acid mixed in the sulfuric acid, so as to purify the sulfuric acid, wherein the concentration of the purified sulfuric acid in the distillation kettle 3 is 85-90%. The hydrochloric acid gas evaporated from the distillation still 3 is sent to the hydrochloric acid condenser 4 to be condensed and recovered. In order to improve the distillation effect, the operation pressure in the distillation kettle 3 is negative pressure, such as-0.06 to-0.09 MPa.
The hydrochloric acid condenser 4 is used for condensing and recovering hydrochloric acid gas from the thin film evaporator 2 and the distillation still 3, and a cooling medium used by the hydrochloric acid condenser 4 is low-temperature frozen brine or low-temperature circulating water.
The sulfuric acid storage tank 5 is used for receiving and storing the purified and concentrated sulfuric acid from the distillation kettle 3, and the sulfuric acid in the sulfuric acid storage tank 5 can be transferred by using a corresponding acid pump or filled and sold.
The hydrochloric acid intermediate storage tank 6 is used for receiving and temporarily storing the cooled hydrochloric acid from the hydrochloric acid condenser 4.
Hydrochloric acid material transfer pump 9 is used for will storing in the hydrochloric acid in storage tank 6 in the middle of the hydrochloric acid, pump into hydrochloric acid condenser 4 again, absorbs hydrochloric acid gas and cools down as the absorption liquid to this concentration that promotes the hydrochloric acid in storage tank 6 in the middle of the hydrochloric acid until predetermined concentration, and the concentration of the hydrochloric acid that the system of this application obtained is 25 ~ 30%. The hydrochloric acid transferring pump 9 is arranged, so that the hydrogen chloride in the hydrochloric acid gas can be absorbed more thoroughly, the concentration of the hydrochloric acid is improved, and the hydrogen chloride in the system is also absorbed more thoroughly, so that the acid content of the tail gas and the processing load of a vacuum unit and a tail gas system are reduced.
According to the mixed acid separation system provided by the application, under the combined action of the mixed acid storage tank 1, the film evaporator 2, the distillation still 3, the hydrochloric acid condenser 4, the sulfuric acid storage tank 5, the hydrochloric acid intermediate storage tank and the hydrochloric acid transfer pump 9, mixed acid in the mixed acid storage tank 1 is input into the film evaporator body 201 through the mixed acid feeding port 202 of the film evaporator 2, hydrochloric acid in the mixed acid is vaporized and separated by the film evaporator 2, hydrochloric acid in the mixed acid is evaporated into hydrochloric acid gas, the hydrochloric acid gas is discharged into the hydrochloric acid condenser 4 from the hydrochloric acid gas outlet 203, the hydrochloric acid gas is condensed and recovered into the hydrochloric acid intermediate storage tank through the hydrochloric acid condenser 4, and the condensed and recovered hydrochloric acid is transferred into the hydrochloric acid condenser 4 by the hydrochloric acid transfer pump 9 to circularly absorb the hydrochloric acid gas again, so that the concentration of the recovered hydrochloric acid is improved; meanwhile, sulfuric acid in the mixed acid is input into the distillation still 3 from the liquid outlet 204 of the thin film evaporator 2, the distillation still 3 is used for secondary distillation and purification (for example, the purity of the available sulfuric acid is 85-90%), the purity of the sulfuric acid is improved, and the recovery efficiency of the mixed acid is also improved.
As shown in fig. 2, optionally, a steam preheater 10 is provided between the mixed acid storage tank 1 and the thin film evaporator 2.
In the present application, a steam preheater 10 is provided between the mixed acid storage tank 1 and the thin film evaporator 2, and the mixed acid from the mixed acid storage tank 1 is preheated and then the heated mixed acid is fed into the thin film evaporator 2, thereby reducing the heating load of the thin film evaporator 2. In actual use, the mixed acid enters a tube pass of the steam preheater 10, high-temperature steam (steam with the temperature of 120-130 ℃) enters a shell pass of the steam preheater to serve as a heating medium, the mixed acid in the tube pass is heated to a preset temperature, such as 80-90 ℃, and then the preheated mixed acid is input into the thin film evaporator 2, so that the heating load of the thin film evaporator 2 can be reduced, and the efficiency of the thin film evaporator 2 is improved.
Optionally, a mixed acid transfer pump 7 is arranged between the mixed acid storage tank 1 and the thin film evaporator 2.
In this application, mix sour commentaries on classics material pump 7's setting can promote the efficiency that mixes sour commentaries on classics material, saves the processing time.
As shown in fig. 2, optionally, the hydrochloric acid turnover tank 8 is connected to the circulation pipe 91 through a hydrochloric acid turnover pipe 81, and a three-way valve 71 is provided at the connection of the circulation pipe 91 and the hydrochloric acid turnover pipe 81.
In the application, the three-way valve 71 can control the flow direction of hydrochloric acid, when hydrochloric acid in the hydrochloric acid intermediate storage tank 6 needs to be used for circularly absorbing hydrochloric acid gas, the three-way valve 71 is communicated with the hydrochloric acid transferring pump 9 and the hydrochloric acid condenser 4 to block the hydrochloric acid transferring pipeline 81, and at the moment, the hydrochloric acid in the hydrochloric acid intermediate storage tank 6 flows to the hydrochloric acid condenser 4 through the hydrochloric acid transferring pump 9 and the three-way valve 71; if hydrochloric acid reaching the preset concentration in the hydrochloric acid intermediate storage tank 6 needs to be transferred into the hydrochloric acid turnover storage tank 8, the three-way valve 71 is communicated with the hydrochloric acid transfer pump 9 and the hydrochloric acid turnover storage tank 8, and the hydrochloric acid flows from the hydrochloric acid intermediate storage tank 6 to the hydrochloric acid turnover storage tank 8 through the three-way valve 71 via the hydrochloric acid transfer pump 9.
In another possible arrangement, a valve is provided on the recycle line 91 near the hydrochloric acid condenser 4, and another valve is provided on the hydrochloric acid transfer line 81 near the hydrochloric acid transfer tank 8, both valves being independently controllable, thereby achieving different flow directions of hydrochloric acid in the hydrochloric acid intermediate tank 6.
As shown in fig. 3, the sulfuric acid storage tank 5 is optionally provided with a sulfuric acid level meter 51;
a sulfuric acid automatic control valve 31 is arranged between the distillation still 3 and the sulfuric acid storage tank 5, and the sulfuric acid automatic control valve 31 is connected with a sulfuric acid liquid level meter 51.
Sulphuric acid level gauge 51 is used for monitoring liquid level height in the sulphuric acid storage tank 5 in this application, and give sulphuric acid automatic control valve 31 with data feedback, when the liquid level in the sulphuric acid storage tank 5 is higher than the default, sulphuric acid automatic control valve 31 closes, temporary stop is to sulphuric acid input in the sulphuric acid storage tank 5, treat the back of transfering the sulphuric acid in the sulphuric acid storage tank 5, liquid level height in the sulphuric acid storage tank 5 descends, when being less than the default, sulphuric acid level gauge 51 gives data feedback to sulphuric acid automatic control valve 31, sulphuric acid automatic control valve 31 is opened, continue to input sulphuric acid in the sulphuric acid storage tank 5. Through the connection of the sulfuric acid liquid level meter 51 and the sulfuric acid automatic control valve 31, the amount of the sulfuric acid input into the sulfuric acid storage tank 5 can be automatically controlled according to the liquid level height of the sulfuric acid in the sulfuric acid storage tank 5, and the mode has the characteristics of real time, automation and no need of manual operation.
As shown in fig. 3, optionally, the hydrochloric acid intermediate tank 6 is provided with a hydrochloric acid level meter 61;
a hydrochloric acid automatic control valve 41 is arranged between the hydrochloric acid condenser 4 and the hydrochloric acid intermediate storage tank 6, and the hydrochloric acid automatic control valve 41 is connected with a hydrochloric acid liquid level meter 61.
Similarly, the hydrochloric acid intermediate tank 6 is provided with a hydrochloric acid level meter 61; a hydrochloric acid automatic control valve 41 is arranged between the hydrochloric acid condenser 4 and the hydrochloric acid intermediate storage tank 6, and the hydrochloric acid automatic control valve 41 is connected with a hydrochloric acid liquid level meter 61. The action modes of the hydrochloric acid liquid level meter 61 and the hydrochloric acid automatic control valve 41 are similar to the action modes of the sulfuric acid liquid level meter 51 and the sulfuric acid automatic control valve 31, and are not described again.
As shown in fig. 4, optionally, the distillation kettle 3 comprises a distillation kettle barrel 301, an exhaust port 302, a nitrogen port 303, a discharge port 304, a sampling port 305, an acid inlet 306, a stirring paddle 307, a jacket 308, a jacket water inlet 309, a jacket water outlet 310, a sulfuric acid liquid outlet 311 and a distillation kettle upper head 312;
the distillation kettle barrel body 301 and the distillation kettle upper end enclosure 312 are connected through a flange;
the exhaust port 302, the nitrogen port 303, the discharge port 304, the sampling port 305 and the acid inlet 306 are distributed at the top of the distillation kettle upper head 312;
the exhaust port 302 is connected with the hydrochloric acid condenser 4;
the jacket 308 covers the outer side of the distillation kettle barrel body 301, the jacket water inlet 309 is arranged at the bottom of the jacket 308, and the jacket water outlet 310 is arranged at one side of the jacket 308 close to the distillation kettle upper end enclosure 312;
a sulfuric acid outlet 311 is arranged at the bottom of the distillation kettle barrel body 301.
In this application, the exhaust port 302 is connected to the hydrochloric acid condenser 4, and is used for discharging the hydrochloric acid gas mixed in the sulfuric acid to the hydrochloric acid condenser 4 for condensation and recovery in the distillation and concentration process.
The nitrogen port 303 is used for purging the distillation still 3 during routine maintenance, and the nitrogen port 303 is also used for evacuating and exhausting off-gas during distillation.
The discharge port 304 is used for discharging the pressure of the distillation kettle 3 when the pressure in the kettle is abnormally increased during operation, so that safety accidents are avoided.
A sampling port 305 for sampling and analyzing sulfuric acid in the distillation still 3.
The acid inlet 306 is connected to the bottom liquid outlet 204 of the thin film evaporator 2, and is used for introducing sulfuric acid in the thin film evaporator 2 into the distillation still 3.
The stirring paddle 307 is used for stirring the liquid in the distillation kettle 3 to make the liquid heated uniformly.
The jacket water inlet 309 is used for inputting a heating medium or a cooling medium; the jacket water outlet 310 is used for outputting a heating medium or a cooling medium.
The sulfuric acid outlet 311 is connected to the sulfuric acid storage tank 5, and is used for outputting the distilled and purified sulfuric acid to the sulfuric acid storage tank 5 for storage.
The still pot upper head 312 is used to seal the still pot 3, and may be a base for the arrangement of the above-described exhaust port 302, nitrogen port 303, discharge port 304, sampling port 305, and acid inlet port 306.
Optionally, the mixed acid rotary pump 7 is a magnetic pump lined with fluoroplastic.
In this application, because mix sour material pump 7's operational environment and be strong acid environment, ordinary pump can be corroded seriously and damage under this operational environment, chooses the inside lining fluoroplastics magnetic drive pump as mixing sour material pump of changeing for use, has acidproof corrosion resistant characteristics, can guarantee to mix sour material pump 7's normal work of changeing, is favorable to prolonging the life who mixes sour material pump 7 of changeing.
In the mixed acid separation system provided by the application, in practical use, mixed acid formed by sulfuric acid and hydrochloric acid generated in the production of perchloromethylmercaptan is input into the mixed acid storage tank 1 for storage, the mixed acid in the mixed acid storage tank 1 is pumped into the thin film evaporator 2 through the mixed acid transfer pump 7, the mixed acid enters the thin film evaporator body 201 from the mixed acid feeding port 202 at the top of the thin film evaporator 2, under the action of gravity and air flow, the mixed acid forms a uniform film on the tower plate in the thin film evaporator body 201 and flows from top to bottom, the water in the mixed acid is heated and vaporized in the flowing process, forming hydrochloric acid gas together with hydrogen chloride in the mixed acid, outputting the hydrochloric acid gas from a hydrochloric acid gas outlet 203 of the film evaporator 2, enabling the hydrochloric acid gas to enter a hydrochloric acid condenser 4, condensing water vapor in the hydrochloric acid gas into water, meanwhile, the condensed water absorbs the hydrogen chloride in the hydrochloric acid gas to form hydrochloric acid, and then the hydrochloric acid is input into a hydrochloric acid intermediate storage tank 6 for temporary storage. The hydrochloric acid in the hydrochloric acid intermediate storage tank 6 is pumped into the hydrochloric acid condenser 4 again by the hydrochloric acid transfer pump 9 to absorb hydrochloric acid gas, and the circulation is performed, so that the concentration of the hydrochloric acid in the hydrochloric acid intermediate storage tank 6 is improved, when the concentration of the hydrochloric acid in the hydrochloric acid intermediate storage tank 6 reaches a preset concentration (the concentration can be sampled and measured by an operator), for example, 25-30%, the hydrochloric acid in the hydrochloric acid intermediate storage tank 6 is transferred out by the hydrochloric acid transfer pump 9, the hydrochloric acid in the hydrochloric acid intermediate storage tank 6 can be transferred out for storage, or the hydrochloric acid transfer pump is used for supplying hydrochloric acid to other workshops needing hydrochloric acid in a factory, for example, a workshop of perchloromethylmercaptan, or the hydrochloric acid transfer pump is packaged into a product for sale.
In an implementation manner, the hydrochloric acid transferring pump 9 is connected with the hydrochloric acid transferring storage tank 8 and used for transferring the hydrochloric acid reaching the preset concentration in the hydrochloric acid intermediate storage tank 6 to the hydrochloric acid transferring storage tank 8 for centralized storage.
The unvaporized liquid in the thin film evaporator 2, which is sulfuric acid mixed with partial moisture and a small amount of hydrogen chloride in the present application, is output from a bottom liquid outlet 204 of the thin film evaporator 2 into the distillation still 3 for heating, the moisture and the hydrogen chloride mixed in the sulfuric acid are further distilled out (namely hydrochloric acid gas) in a distillation mode, the hydrochloric acid gas output from the distillation still 3 enters the hydrochloric acid condenser 4 for condensation to form hydrochloric acid, and the hydrochloric acid is collected into the hydrochloric acid intermediate storage tank 6 for temporary storage. The purified sulfuric acid in the distillation kettle 3 is input into a sulfuric acid storage tank 5 from the distillation kettle 3 for storage, so as to be used by other working sections in a factory or to be packaged into a product for sale.
In a realisable manner, the hydrochloric acid turnaround tank 8 is connected to the circulation conduit 91 by a hydrochloric acid turnaround conduit 81, and a three-way valve 71 is provided at the connection of the circulation conduit 91 and the hydrochloric acid turnaround conduit 81. The three-way valve 71 can control the flow direction of the hydrochloric acid, when the hydrochloric acid in the hydrochloric acid intermediate storage tank 6 needs to be used for circularly absorbing hydrochloric acid gas, the three-way valve 71 is communicated with the hydrochloric acid transfer pump 9 and the hydrochloric acid condenser to block the hydrochloric acid transfer pipeline 81, and at the moment, the hydrochloric acid in the hydrochloric acid intermediate storage tank 6 flows to the hydrochloric acid condenser 4 through the three-way valve 71 through the hydrochloric acid transfer pump 9.
If hydrochloric acid reaching the preset concentration in the hydrochloric acid intermediate storage tank 6 needs to be transferred into the hydrochloric acid turnover storage tank 8, the three-way valve 71 is communicated with the hydrochloric acid transfer pump 9 and the hydrochloric acid turnover storage tank 8, and the hydrochloric acid flows from the hydrochloric acid intermediate storage tank 6 to the hydrochloric acid turnover storage tank 8 through the three-way valve 71 via the hydrochloric acid transfer pump 9.
In another possible arrangement, a valve is arranged at one end of the circulating pipeline 91 close to the hydrochloric acid condenser 4, another valve is arranged at one end of the hydrochloric acid transfer pipeline 81 close to the hydrochloric acid transfer storage tank 8, and the two valves can be independently controlled, so that different flow directions of hydrochloric acid in the hydrochloric acid intermediate storage tank 6 are realized.
In an achievable mode, a steam preheater 10 is arranged between the mixed acid storage tank 1 and the thin film evaporator 2, the mixed acid from the mixed acid storage tank 1 is preheated, and the heated mixed acid is input into the thin film evaporator 2, so that the heating load of the thin film evaporator 2 is reduced.
In yet another possible implementation, the sulfuric acid storage tank 5 is provided with a sulfuric acid level meter 51; a sulfuric acid automatic control valve 31 is arranged between the distillation still 3 and the sulfuric acid storage tank 5, and the sulfuric acid automatic control valve 31 is connected with a sulfuric acid liquid level meter 51. The sulfuric acid liquid level meter 51 is used for monitoring the liquid level in the sulfuric acid storage tank 5 and feeding back data to the sulfuric acid automatic control valve 31, when the liquid level in the sulfuric acid storage tank 5 is higher than a preset value, the sulfuric acid automatic control valve 31 is closed, the sulfuric acid input into the sulfuric acid storage tank 5 is temporarily stopped, after the sulfuric acid in the sulfuric acid storage tank 5 is transferred out, the liquid level in the sulfuric acid storage tank 5 is reduced, when the liquid level is lower than the preset value, the sulfuric acid liquid level meter 51 feeds back the data to the sulfuric acid automatic control valve 31, the sulfuric acid automatic control valve 31 is opened, and the sulfuric acid continues to be input into the sulfuric acid storage tank 5. Through being connected of sulphuric acid level gauge 51 and sulphuric acid automatic control valve 31, can be according to the liquid level height of sulphuric acid in the sulphuric acid storage tank 5, the volume of the sulphuric acid in the automatic control input sulphuric acid storage tank 5, this kind of mode has real-time, automatic, need not manual operation's characteristics.
Similarly, the hydrochloric acid intermediate tank 6 is provided with a hydrochloric acid level meter 61; a hydrochloric acid automatic control valve 41 is arranged between the hydrochloric acid condenser 4 and the hydrochloric acid intermediate storage tank 6, and the hydrochloric acid automatic control valve 41 is connected with a hydrochloric acid liquid level meter 61.
The action modes of the hydrochloric acid liquid level meter 61 and the hydrochloric acid automatic control valve 41 are similar to the action modes of the sulfuric acid liquid level meter 51 and the sulfuric acid automatic control valve 31, and are not described again.
It should be noted that, under the guidance of the present invention, those skilled in the art can also make partial modifications to the above system. For example, a pump, a pressure sensor, a flow meter, a temperature sensor, and the like are arranged between different units or devices and equipment on a conveying pipeline inside the system, different valves are also arranged at the same time, such as a pressure relief valve, a pressure regulating valve, a safety valve, and the like which are used for regulating and stabilizing the pressure of the whole system, and the opening degree of the valves can be regulated to regulate the material flow in the pipeline, and the like.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present application, and not for limiting the same; although the present application has been described in detail with reference to the foregoing embodiments, it will be understood by those skilled in the art; the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present application.
Claims (8)
1. A mixed acid separation system is characterized by comprising a mixed acid storage tank (1), a film evaporator (2), a hydrochloric acid condenser (4) and a hydrochloric acid intermediate storage tank (6) which are sequentially connected in series through process pipelines;
the thin film evaporator (2) comprises a thin film evaporator body (201), a mixed acid feed port (202), a hydrochloric acid gas outlet (203) and a liquid discharge port (204); the mixed acid feeding port (202) is arranged at the top of an upper end enclosure of the thin film evaporator body (201); the hydrochloric acid gas outlet (203) is arranged on one side surface of an upper end enclosure of the thin film evaporator body (201) far away from the mixed acid feed port (202), and is connected with the hydrochloric acid condenser (4); the liquid outlet (204) is arranged at the bottom of the thin film evaporator body (201) and is connected with a distillation kettle (3);
the distillation kettle (3) is respectively connected with a sulfuric acid storage tank (5) and the hydrochloric acid condenser (4);
the hydrochloric acid intermediate storage tank (6) is connected with a hydrochloric acid transferring pump (9); the hydrochloric acid transferring pump (9) is connected with the hydrochloric acid condenser (4) through a circulating pipeline (91) and is used for pumping the hydrochloric acid in the hydrochloric acid intermediate storage tank (6) into the hydrochloric acid condenser (4) again.
2. The mixed acid separation system according to claim 1, characterized in that a steam preheater (10) is provided between the mixed acid storage tank (1) and the thin film evaporator (2).
3. The mixed acid separation system according to claim 2, characterized in that a mixed acid transfer pump (7) is arranged between the mixed acid storage tank (1) and the steam preheater (10).
4. The mixed acid separation system according to any one of claims 1-3, characterized in that the system further comprises a hydrochloric acid turnover storage tank (8), the hydrochloric acid turnover storage tank (8) is connected with the circulation pipeline (91) through a hydrochloric acid turnover pipeline (81), and a three-way valve (71) is arranged at the connection of the circulation pipeline (91) and the hydrochloric acid turnover pipeline (81).
5. The mixed acid separation system according to claim 4, wherein the sulfuric acid storage tank (5) is provided with a sulfuric acid level meter (51);
a sulfuric acid automatic control valve (31) is arranged between the distillation kettle (3) and the sulfuric acid storage tank (5), and the sulfuric acid automatic control valve (31) is connected with the sulfuric acid liquid level meter (51).
6. The mixed acid separation system according to claim 4, wherein the hydrochloric acid intermediate storage tank (6) is provided with a hydrochloric acid level meter (61);
a hydrochloric acid automatic control valve (41) is arranged between the hydrochloric acid condenser (4) and the hydrochloric acid intermediate storage tank (6), and the hydrochloric acid automatic control valve (41) is connected with the hydrochloric acid liquid level meter (61).
7. The mixed acid separation system according to claim 1, wherein the distillation kettle (3) comprises a distillation kettle barrel (301), an exhaust port (302), a nitrogen port (303), a discharge port (304), a sampling port (305), an acid inlet (306), a stirring paddle (307), a jacket (308), a jacket water inlet (309), a jacket water outlet (310), a sulfuric acid liquid outlet (311) and a distillation kettle upper end enclosure (312);
the distillation kettle barrel body (301) is connected with the distillation kettle upper end enclosure (312) through a flange;
the exhaust port (302), the nitrogen port (303), the discharge port (304), the sampling port (305) and the acid inlet (306) are distributed at the top of the distillation still upper head (312);
the exhaust port (302) is connected with the hydrochloric acid condenser (4);
the stirring paddle (307) is arranged inside the distillation kettle barrel body (301);
the jacket (308) covers the outer side of the distillation kettle barrel body (301), the jacket water inlet (309) is arranged at the bottom of the jacket (308), and the jacket water outlet (310) is arranged on one side of the jacket (308) close to the distillation kettle upper end enclosure (312);
the sulfuric acid outlet (311) is arranged at the bottom of the distillation kettle barrel body (301).
8. The mixed acid separation system according to claim 3, wherein the mixed acid transfer pump (7) is a fluoroplastic lined magnetic pump.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202221344312.0U CN217367797U (en) | 2022-05-31 | 2022-05-31 | Mixed acid separation system |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202221344312.0U CN217367797U (en) | 2022-05-31 | 2022-05-31 | Mixed acid separation system |
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| CN217367797U true CN217367797U (en) | 2022-09-06 |
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| CN202221344312.0U Active CN217367797U (en) | 2022-05-31 | 2022-05-31 | Mixed acid separation system |
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| CN (1) | CN217367797U (en) |
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