CN216890096U - Deep desorption system for hydrochloric acid - Google Patents

Deep desorption system for hydrochloric acid Download PDF

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Publication number
CN216890096U
CN216890096U CN202220500955.3U CN202220500955U CN216890096U CN 216890096 U CN216890096 U CN 216890096U CN 202220500955 U CN202220500955 U CN 202220500955U CN 216890096 U CN216890096 U CN 216890096U
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tower
hydrochloric acid
hcl
calcium chloride
desorption
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杜树忠
曹卫东
艾海峰
周万礼
刘自松
杨宇静
乔云
武明
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Yunnan Nengtou Silicon Technology Development Co ltd
Yunnan Energy Investment Chemical Co ltd
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Yunnan Nengtou Silicon Technology Development Co ltd
Yunnan Energy Investment Chemical Co ltd
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Abstract

The utility model discloses a hydrochloric acid deep desorption system, which comprises a hydrochloric acid desorption system, an HCL purification system, a calcium chloride concentration system, a condensation collection system and a vacuum system, wherein an HCL redistribution tower is arranged at the exhaust tail end of the calcium chloride concentration system, a three-stage exhaust pipe is arranged at the top of the HCL redistribution tower, the end part of the three-stage exhaust pipe is connected with the condensation collection system, a three-stage liquid discharge pipe is arranged at the bottom of the HCL redistribution tower, a washing liquid circulation system communicated with the upper part of the HCL redistribution tower is arranged on the three-stage liquid discharge pipe, and the end part of the three-stage liquid discharge pipe is communicated with a feed inlet of the hydrochloric acid desorption system. The method has the advantages of reasonable process, small investment and simple operation, can wash and recover HCl carried by water vapor in the calcium chloride concentration process, thoroughly desorb, obviously reduce the content of HCL in condensed wastewater, reduce the subsequent wastewater treatment difficulty and save the system operation cost.

Description

Deep desorption system for hydrochloric acid
Technical Field
The utility model belongs to the technical field of organic silicon production processes, and particularly relates to a hydrochloric acid deep desorption system.
Background
In the production of organosilicon methyl chlorosilane, a large amount of hydrochloric acid as a byproduct is generated in the production links of chloromethane synthesis, dimethyl dichlorosilane hydrolysis, incineration, white carbon black and the like. The produced by-product hydrochloric acid has the characteristics of complex components, high HCL content, high desorption treatment difficulty and the like, the application range of the by-product hydrochloric acid is limited, the by-product hydrochloric acid is low in price and difficult to sell, and the produced dilute hydrochloric acid is difficult to sell even after the by-product hydrochloric acid is subjected to desorption treatment, so that the normal operation of a production device is severely restricted. The information records that the hydrochloric acid solution can form constant boiling solution under certain conditions, so that no matter dilute hydrochloric acid or concentrated hydrochloric acid can finally reach constant boiling state, but the highest azeotropic point of the hydrochloric acid is 109 ℃ under normal pressure, the mass fraction of hydrogen chloride is 20.24%, only about 20% of hydrochloric acid can be obtained by adopting distillation operation under normal pressure, and the conventional desorption of the hydrochloric acid is only suitable for hydrochloric acid with the mass fraction of more than 21%, so that the deep desorption process is an effective measure for desorption treatment of the existing byproduct hydrochloric acid. In the prior art, common hydrochloric acid deep desorption processes comprise a calcium chloride method and a sulfuric acid method, the calcium chloride method desorption process is mature, and the disassembly and the inspection are simpler when an organic matter blocks an analytical tower, so that the method is widely applied to byproduct hydrochloric acid; after the hydrochloric acid desorption impurities in the sulfuric acid method are dissolved in the sulfuric acid, the sulfuric acid needs to be periodically replaced by new sulfuric acid as an extracting agent (the mass content of the impurities is about 3%), and the treatment of the waste sulfuric acid is difficult. At present, companies mainly adopt a calcium chloride method to deeply desorb byproduct hydrochloric acid so as to realize effective recycling of chlorine resources, but in the use process of the existing calcium chloride method treatment process system, it is found that the concentration of byproduct hydrochloric acid discharged from different links in an organosilicon synthesis process is different, the HCL content in the byproduct hydrochloric acid is distributed in a range of 10-31% and is different, after the byproduct hydrochloric acid with different concentrations is desorbed by the calcium chloride method, the HCL content in desorbed condensation wastewater can be theoretically less than 1%, but generally can be less than 3% in actual production, and after the high-concentration condensation wastewater is discharged to a wastewater treatment process, the HCL content is relatively high, so that the treatment difficulty of the condensation wastewater is increased, and the treatment cost is increased. Therefore, the development of a hydrochloric acid deep desorption system with small equipment investment, simple operation and more thorough desorption effect is objectively needed.
Disclosure of Invention
The utility model aims to provide a hydrochloric acid deep desorption system which has the advantages of small equipment investment, simple operation and more thorough desorption effect.
The device comprises a hydrochloric acid desorption system, an HCL purification system, a calcium chloride concentration system, a condensation collection system and a vacuum system, wherein an HCL redistribution tower is arranged at the exhaust tail end of the calcium chloride concentration system, a three-stage exhaust pipe is arranged at the top of the HCL redistribution tower, the end part of the three-stage exhaust pipe is connected with the condensation collection system, a three-stage liquid discharge pipe is arranged at the bottom of the HCL redistribution tower, a washing liquid circulation system communicated with the upper part of the HCL redistribution tower is arranged on the three-stage liquid discharge pipe, and the end part of the three-stage liquid discharge pipe is communicated with a feed inlet of the hydrochloric acid desorption system.
Further, the condensation collection system comprises a condenser and an acidic wastewater tank, a top gas-phase outlet of the HCL redistribution tower is connected with the condenser, an upper gas-phase outlet of the condenser is connected with a vacuum system, and a liquid-phase outlet of the condenser is connected with the acidic wastewater tank.
Furthermore, the washing liquid circulation system comprises a circulation pump, a circulation pipe and a third liquid inlet pipe, wherein the third liquid inlet pipe is arranged at the upper part of the HCL redistribution tower, the circulation pipe is arranged between the third liquid inlet pipe and the third-stage liquid discharge pipe, and the circulation pump is arranged on the third-stage liquid discharge pipe.
Further, the HCL redistributing tower is a packed tower, and 1-3 sections of packing are installed at the upper section in the packed tower.
Further, hydrochloric acid desorption system includes hydrochloric acid desorption tower and first reboiler, HCL clean system includes second grade condenser and defroster, calcium chloride concentration system includes calcium chloride concentration tower and second reboiler, hydrochloric acid desorption tower middle part is provided with the mixed liquid entry of hydrochloric acid and calcium chloride, the bottom is connected with first reboiler, top gas phase export is connected with second grade condenser and defroster in proper order, bottom liquid phase pipe export is connected with calcium chloride concentration tower middle part, calcium chloride concentration tower bottom is connected with the second reboiler. Preferably, a liquid phase outlet at the bottom of the calcium chloride concentration tower is provided with a delivery pump, and an outlet of the delivery pump is connected with a mixed liquid inlet of the hydrochloric acid and the calcium chloride of the hydrochloric acid desorption tower.
Furthermore, the body of the HCL redistributing tower is made of a stainless steel lining PTFE material.
Furthermore, the outer walls of the hydrochloric acid desorption tower, the calcium chloride concentration tower and the washing tower are all provided with heat insulation layers.
According to the utility model, the HCL redistributing tower with a washing liquid circulating system is arranged at the rear end of the original desorption and concentration treatment, the HCL-containing superheated steam discharged from the calcium chloride concentrating tower is circularly washed, and the water vapor is not condensed in the washing process, so that the HCL content of the condensed water obtained by cooling the washed secondary steam after entering a subsequent condensation collecting system is extremely low. The method has the advantages of reasonable process, small investment and simple operation, can wash and recover HCl carried by water vapor in the calcium chloride concentration process, has thorough desorption, obviously reduces the content of HCL in the condensed wastewater while realizing effective desorption and recovery of HCl, reduces the subsequent wastewater treatment difficulty, saves the wastewater treatment cost, has better economic benefit and social benefit, and is easy to popularize and use.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention;
in the figure: 1-a first liquid inlet pipe, 2-a hydrochloric acid desorption tower, 3-a second liquid inlet pipe, 4-a first reboiler, 5-a first-stage exhaust pipe, 6-a second-stage condenser, 7-a demister, 8-a first-stage liquid discharge pipe, 9-a calcium chloride concentration tower, 10-a second reboiler, 11-a delivery pump, 12-a second-stage liquid discharge pipe, 13-a second-stage exhaust pipe, 14-a HCl redistribution tower, 15-a third liquid inlet pipe, 16-a third-stage exhaust pipe, 17-a condenser, 18-an acidic waste water tank, 19-a circulating pump, 20-a circulating pipe, 21-a third-stage liquid discharge pipe and 22-a vacuum system.
Detailed Description
The utility model is further described with reference to the accompanying drawings, but the utility model is not limited in any way, and any variations or modifications based on the teachings of the utility model are within the scope of the utility model.
As shown in figure 1, the utility model comprises a hydrochloric acid desorption system, an HCL purification system, a calcium chloride concentration system, a condensation collection system and a vacuum system 22, wherein an HCL redistribution tower 14 is arranged at the exhaust tail end of the calcium chloride concentration system, a three-stage exhaust pipe 16 is arranged at the top of the HCL redistribution tower 14, the end part of the three-stage exhaust pipe 16 is connected with the condensation collection system, a three-stage liquid discharge pipe 21 is arranged at the bottom of the HCL redistribution tower 14, a washing liquid circulating system communicated with the upper part of the HCL redistribution tower 14 is arranged on the three-stage liquid discharge pipe 21, the end part of the three-stage liquid discharge pipe 21 is communicated with a feed inlet of the hydrochloric acid desorption system, when in operation, HCL-containing vapor discharged from the top of the calcium chloride concentration system enters the HCL redistribution tower 14, the HCL-containing vapor is circularly washed by desalted water in the HCL redistribution tower 14, and the washed vapor enters the condensation collection system, the circulating washing liquid returns to the hydrochloric acid desorption system after being concentrated; the temperature of the top of the calcium chloride concentration system is 80-100 ℃, the vacuum degree is-40 to-60 Kpa, and the temperature and the pressure in the HCl redistribution tower 14 are consistent with the top of the calcium chloride concentration system.
Further, the condensation collection system comprises a condenser 17 and an acid wastewater tank 18, wherein a top gas-phase outlet of the HCL redistribution tower 14 is connected with the condenser 17, an upper gas-phase outlet of the condenser 17 is connected with a vacuum system 22, and a liquid-phase outlet of the condenser 17 is connected with the acid wastewater tank 18.
Further, the washing liquid circulating system includes a circulating pump 19, a circulating pipe 20 and a third liquid-feeding pipe 15, the third liquid-feeding pipe 15 is disposed at an upper portion of the HCL redistributing column 14, the circulating pipe 20 is disposed between the third liquid-feeding pipe 15 and a tertiary liquid-discharging pipe 21, and the circulating pump 19 is installed on the tertiary liquid-discharging pipe 21.
Further, the HCL redistributing tower 14 is a packed tower, and 1-3 sections of packing are installed at the upper section in the tower. The filler is made of anticorrosive materials such as ceramics, PP and the like, and is preferably theta 25PP pall ring random packing.
Further, hydrochloric acid desorption system includes hydrochloric acid desorption tower 2 and first reboiler 4, HCl clean system includes second grade condenser 6 and defroster 7, calcium chloride concentration system includes calcium chloride concentration tower 9 and second reboiler 10, 2 middle parts of hydrochloric acid desorption tower are provided with the mixed liquid entry of hydrochloric acid and calcium chloride, and the bottom is connected with first reboiler 4, and top gas phase export is connected with second grade condenser 6 and defroster 7 in proper order, and bottom liquid phase pipe export is connected with the 9 middle parts of calcium chloride concentration tower, and the 9 bottoms of calcium chloride concentration tower are connected with second reboiler 10. Preferably, a liquid phase outlet at the bottom of the calcium chloride concentration tower 9 is provided with a delivery pump 11, and a pump outlet of the delivery pump 11 is connected with a mixed liquid inlet of the hydrochloric acid and the calcium chloride of the hydrochloric acid desorption tower 2.
Furthermore, in order to prevent the HCL redistribution tower 14 from being corroded by HCL-containing steam and prolong the service life of the HCL-containing steam, the tower body of the HCL redistribution tower 14 is made of a stainless steel lining PTFE material.
In order to avoid heat loss in the hydrochloric acid desorption tower 2, the calcium chloride concentration tower 9 and the HCL redistribution tower 14 and ensure the stable operation of the system, the outer walls of the hydrochloric acid desorption tower 2, the calcium chloride concentration tower 9 and the HCL redistribution tower 14 are all provided with heat insulation layers.
The concrete process of the hydrochloric acid desorption system, the HCL purification system, the calcium chloride concentration system, the condensation collection system and the vacuum system 22 in the utility model is as follows: hydrochloric acid with different concentrations and calcium chloride solution concentrated by a calcium chloride concentration system are mixed and then enter a hydrochloric acid desorption system, namely hydrochloric acid with different concentrations entering from a first liquid inlet pipe 1 and calcium chloride solution entering from a second liquid inlet pipe 3 are mixed and then enter from a mixed solution inlet of hydrochloric acid and calcium chloride in the middle of a hydrochloric acid desorption tower 2, a first reboiler 4 adds steam into the hydrochloric acid desorption tower 2 to heat and desorb the mixed solution, HCL discharged from the top of the hydrochloric acid desorption tower 2 enters an HCL purification system through a first-stage exhaust pipe 5, the HCl purification system comprises a second-stage condenser 6 and a demister 7, HCL discharged from the top of the hydrochloric acid desorption tower 2 is subjected to two-stage deep cooling by the second-stage condenser 6 and drying by the demister 7 and is used for other processes, low-concentration calcium chloride solution discharged from the bottom of the hydrochloric acid desorption tower 2 enters the calcium chloride concentration system through a first-stage liquid discharge pipe 8, the calcium chloride concentration system comprises a calcium chloride concentration tower 9 and a second reboiler 10, namely, a low-concentration calcium chloride solution enters a calcium chloride concentration tower 9 through a primary liquid discharge pipe 8, a second reboiler 10 adds steam into the calcium chloride concentration tower 9 to heat and concentrate the low-concentration calcium chloride solution, when the mass fraction of the low-concentration calcium chloride solution is concentrated to 50%, the low-concentration calcium chloride solution returns to a hydrochloric acid desorption tower 2 through a secondary liquid discharge pipe 12 under the action of a delivery pump 11 to be continuously used, HCL-containing water vapor discharged from the top of the calcium chloride concentration tower 9 enters an HCL redistribution tower 14 through a secondary exhaust pipe 13, the HCL-containing water vapor is circularly washed in the HCl redistribution tower 14 by desalted water, the washed water vapor enters a condensation collection system, the condensation collection system comprises a condenser 17 and an acid waste water tank 18, the generated water vapor is discharged from a tertiary exhaust pipe 16 and condensed into condensed water through the condenser 17 to be discharged into the acid waste water tank 18, and the HCl redistribution tower 14 is provided with a washing liquid circulation system, the washing liquid circulating system comprises a circulating pump 19, a circulating pipe 20 and a third liquid inlet pipe 15, desalted water enters from the third liquid inlet pipe 15, circulating washing liquid returns to the HCl redistribution tower through the circulating pipe 20 under the action of the circulating pump 19 for recycling, and when the content of HCL in the circulating washing liquid in the HCL redistribution tower 14 reaches 10-17%, the circulating washing liquid returns to the hydrochloric acid desorption tower 2 of the hydrochloric acid desorption system through a three-level liquid discharge pipe 21 for desorption treatment. When the whole calcium chloride concentration system, the HCl redistribution tower 14 and the washing liquid circulating system run, the vacuum system 22 is used for vacuumizing and then the operation is carried out under negative pressure.
In the hydrochloric acid desorption by the calcium chloride method, the mass fraction of a calcium chloride solution in a calcium chloride concentration tower 9 is concentrated from 40% to 50%, the vacuum degree is controlled to be about-40 KPa to-60 KPa, the temperature of corresponding secondary saturated steam is 70 ℃ to 86 ℃, the boiling point of 40% to 50% of calcium chloride under the pressure is 115 ℃ to 125 ℃, in the actual operation, the outlet temperature at the top of the calcium chloride concentration tower 9 is generally controlled to be 80 ℃ to 100 ℃, the temperature of HCL-containing steam evaporated from the calcium chloride solution corresponds to the temperature of calcium chloride, and the superheated steam belongs to superheated steam under the pressure of-40 KPa to-60 KPa. The temperature and pressure in the HCl redistributing tower 14 are kept consistent with the top of the calcium chloride concentration system (namely the temperature is 80-100 ℃, and the pressure is-40 KPa to-60 KPa, so that the HCl in the HCl-containing steam is washed and absorbed in a circulating manner while the superheated steam is kept, the steam continuously enters a subsequent condensation collection system in a gaseous form, and is condensed into condensed water by a condenser 17 and then discharged into an acidic waste water tank 18.

Claims (8)

1. The utility model provides a hydrochloric acid degree of depth desorption system, includes hydrochloric acid desorption system, HCL clean system, calcium chloride concentrated system, condensation collecting system and vacuum system (22), its characterized in that: be provided with HCL redistributing tower (14) at the exhaust end of calcium chloride concentrated system, the top of HCL redistributing tower (14) is provided with tertiary blast pipe (16), and the end connection of tertiary blast pipe (16) has the condensation collection system, the bottom of HCL redistributing tower (14) is provided with tertiary fluid-discharge tube (21), is provided with the washing liquid circulation system with HCL redistributing tower (14) upper portion intercommunication on tertiary fluid-discharge tube (21), and the tip and the hydrochloric acid of tertiary fluid-discharge tube (21) are taken off the feed inlet of inhaling the system and are connected the intercommunication.
2. A hydrochloric acid deep desorption system according to claim 1, wherein the condensation collection system comprises a condenser (17) and an acid wastewater tank (18), the top gas phase outlet of the HCL redistribution tower (14) is connected with the condenser (17), the upper gas phase outlet of the condenser (17) is connected with a vacuum system (22), and the liquid phase outlet of the condenser (17) is connected with the acid wastewater tank (18).
3. The deep desorption system of hydrochloric acid according to claim 1, wherein the circulation system of the washing liquid comprises a circulation pump (19), a circulation pipe (20) and a third liquid inlet pipe (15), the third liquid inlet pipe (15) is arranged at the upper part of the HCL redistribution tower (14), the circulation pipe (20) is arranged between the third liquid inlet pipe (15) and the third liquid discharge pipe (21), and the circulation pump (19) is arranged on the third liquid discharge pipe (21).
4. The deep hydrochloric acid desorption system of claim 1, wherein the HCL redistribution tower (14) is a packed tower, and 1-3 sections of packing are arranged at the upper section in the tower.
5. The hydrochloric acid deep desorption system of claim 1, which comprises a hydrochloric acid desorption tower (2) and a first reboiler (4), the HCl purification system comprises a secondary condenser (6) and a demister (7), the calcium chloride concentration system comprises a calcium chloride concentration tower (9) and a second reboiler (10), the hydrochloric acid desorption tower (2) is provided with a mixed solution inlet of hydrochloric acid and calcium chloride in the middle, the bottom of the hydrochloric acid desorption tower is connected with the first reboiler (4), the top gas phase outlet of the hydrochloric acid desorption tower is connected with the secondary condenser (6) and the demister (7) in sequence, the bottom liquid phase pipe outlet of the hydrochloric acid desorption tower is connected with the middle of the reboiler (9), and the bottom of the calcium chloride concentration tower (9) is connected with the second reboiler (10).
6. The hydrochloric acid deep desorption system of claim 5, wherein a liquid phase outlet at the bottom of the calcium chloride concentration tower (9) is provided with a delivery pump (11), and a pump outlet of the delivery pump (11) is connected with a hydrochloric acid and calcium chloride mixed liquid inlet of the hydrochloric acid desorption tower (2).
7. The hydrochloric acid deep desorption system of claim 1, which is characterized in that: the body of the HCL redistributing tower (14) is made of a stainless steel lining PTFE material.
8. The hydrochloric acid deep desorption system of claim 5, which is characterized in that: and the outer walls of the hydrochloric acid desorption tower (2), the calcium chloride concentration tower (9) and the HCL redistribution tower (14) are all provided with heat insulation layers.
CN202220500955.3U 2022-03-09 2022-03-09 Deep desorption system for hydrochloric acid Active CN216890096U (en)

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