CN219848217U - Dilute sulfuric acid continuous purifying treatment device - Google Patents

Dilute sulfuric acid continuous purifying treatment device Download PDF

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Publication number
CN219848217U
CN219848217U CN202321322739.5U CN202321322739U CN219848217U CN 219848217 U CN219848217 U CN 219848217U CN 202321322739 U CN202321322739 U CN 202321322739U CN 219848217 U CN219848217 U CN 219848217U
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sulfuric acid
tower
dilute sulfuric
steam
tower body
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CN202321322739.5U
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韩景岩
徐建生
陈伟
韩志涛
张晓林
王春生
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Henan Hdf Chemical Co ltd
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Henan Hdf Chemical Co ltd
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Abstract

The utility model discloses a dilute sulfuric acid continuous purification treatment device, which comprises a stripping tower consisting of a tower kettle and a tower body, wherein the middle part of the tower body is provided with a 1/2-height filling area, the upper and lower parts of the filling area are provided with polytetrafluoroethylene grid plates, the filling is polytetrafluoroethylene pall rings, the upper end of the tower body is provided with a steam outlet, the steam outlet is externally connected with a condenser, the condenser is connected with a condensate recovery tank and a vacuum buffer tank, the upper part of the tower body is provided with a feed inlet, the feed inlet is internally connected with a liquid distributor, the feed inlet is externally connected with a feed pipeline through a feed pump, the tower kettle is provided with a thermometer A and a vacuum meter, the bottom of the tower kettle is provided with a discharge pipeline, the discharge pipeline is connected with a dilute sulfuric acid storage tank through a extraction pump, the discharge pipeline is provided with a discharge control valve and a discharge flowmeter, the upper end of the tower kettle is provided with a steam pipeline which is internally connected with a gas disperser, the steam pipeline is externally connected with a hot water tank, and the water temperature is maintained at 80+/-2 ℃; the utility model has the advantages of good purification treatment effect, high purification treatment efficiency, safety, reliability and high recycling rate.

Description

Dilute sulfuric acid continuous purifying treatment device
Technical Field
The utility model belongs to the technical field of chemical purification recovery treatment equipment, relates to a dilute sulfuric acid continuous purification treatment device, and in particular relates to a dilute sulfuric acid continuous purification treatment device after methyl chloride is dried.
Background
The current domestic method for producing glyphosate is mainly an alkyl ester method, and dimethyl phosphite is one of the raw materials for producing glyphosate by the alkyl ester method. In the process of producing dimethyl phosphite, a large amount of byproduct chloromethane is generated, and the chloromethane is required to be purified and dried when being recycled, so that the requirements of industrial production can be met. The byproduct chloromethane contains more impurities such as moisture, methanol, methylal and the like, wherein the large moisture content is a main problem of chloromethane recovery.
The most common mode of the prior dry impurity-removing chloromethane is to adopt concentrated sulfuric acid, after chloromethane gas passes through the concentrated sulfuric acid, the concentrated sulfuric acid absorbs water and gradually becomes dilute sulfuric acid, meanwhile, some raw materials and products such as methanol, methylal and the like enter the concentrated sulfuric acid, along with the higher content of organic matters in the sulfuric acid, the COD value is about 600000mg/L, the liquid level even reaches the flammability degree, if the concentrated sulfuric acid is formed by direct heating and concentration treatment, the concentrated sulfuric acid has oxidability, and the concentrated sulfuric acid contains combustible gas such as methanol, methylal and the like, has higher on-site treatment danger coefficient, causes serious potential safety hazard to the production site, is difficult to treat and is difficult to recycle, so that the purification treatment device for the dilute sulfuric acid formed after the dry impurity-removing chloromethane is provided.
For example, the Chinese patent application No. CN213951039U discloses a purifying treatment device for dilute sulfuric acid, which is characterized in that high-temperature steam is introduced into a reaction kettle, the dilute sulfuric acid in the reaction kettle is heated and evaporated, water in the dilute sulfuric acid is evaporated, the evaporated water steam takes away organic matters in the dilute sulfuric acid, then the water steam containing the organic matters is condensed and recycled, the purifying treatment effect is good, the treatment cost is low, and the problems of inflammability, explosiveness and unsafety and difficult material recycling existing in the existing direct heating and concentrating treatment method are solved; however, in actual use, the problems of unsatisfactory purification treatment effect and low purification treatment efficiency are found; in order to solve the problems, it is necessary to develop a continuous purification treatment device for dilute sulfuric acid.
Disclosure of Invention
The utility model aims to overcome the defects of the prior art and provide the dilute sulfuric acid continuous purifying treatment device which has the advantages of good purifying treatment effect, high purifying treatment efficiency, safety, reliability and high resource recycling rate.
The purpose of the utility model is realized in the following way: the utility model provides a dilute sulfuric acid continuous purification treatment device, includes the stripper that comprises tower cauldron and tower body, the tower body middle part is equipped with the packing district, the height in packing district is the half of tower body height, be equipped with the grid tray of polytetrafluoroethylene material about the packing district, the packing in packing district is tetrafluoropall ring, the tower body upper end is equipped with the steam outlet, the external condenser of steam outlet, the condenser is connected with condensate recovery tank and vacuum buffer tank, tower body upper portion is close to steam outlet department is equipped with the feed inlet, the feed inlet inscription equal altitude is located the liquid distributor in tower body upper portion center, feed inlet department installs feed control valve, feed check valve and feed flowmeter, the feed inlet passes through the external feed pipeline of feed pump, thermometer A and vacuum gauge are installed to the tower cauldron bottom, the discharge pipeline is equipped with the discharge pipeline through adopting the pump to connect dilute sulfuric acid holding vessel, install ejection of compact control valve and ejection of compact flowmeter on the discharge pipeline, the tower cauldron upper end is equipped with condensate recovery tank and vacuum buffer tank, the steam pipeline inscription equal altitude just is located the liquid distributor in tower body upper portion center, feed control valve, steam inlet temperature control valve and steam meter are installed to the steam tank on the water heater, the steam tank is installed to the steam tank is located in 2.
Preferably, the condenser is a graphite tubular condenser, the steam outlet is connected with the condenser through a steam outlet control valve, the condenser is connected with a vacuum buffer tank through a vacuum control valve A, the vacuum buffer tank is externally connected with a vacuum device through a vacuum control valve B, and the condensate recovery tank is externally connected with a rectification recovery system through a condensate control valve.
Preferably, the hot water tank is heated by a jacket, and the hot water tank is externally connected with a water supplementing pipeline through a water inlet control valve.
Preferably, the gas disperser is of porous structure.
Preferably, a liquid level meter B is arranged on the dilute sulfuric acid storage tank.
Due to the adoption of the technical scheme, the utility model has the beneficial effects that: the utility model adopts a stripping tower consisting of a tower kettle and a tower body to replace the existing reaction kettle, a filling area with the height of one half is arranged in the tower body, the filling area consists of grid plates with the upper part and the lower part being made of polytetrafluoroethylene materials and filling materials with the middle part being made of tetrafluoropall ring materials, and the contact area between steam and dilute sulfuric acid flowing through the filling area is large in the process of rising from the lower part of the filling area, so that the purification treatment effect is good and the purification treatment efficiency is high; the utility model adopts the omnibearing feeding of the liquid distributor, can lead the dilute sulfuric acid to uniformly flow through the filling area in a large area, is convenient for the steam to fully contact and mix with the dilute sulfuric acid, takes away organic matters in the dilute sulfuric acid, and further improves the purifying treatment effect; the utility model adopts the one-way valve to control the input of raw material dilute sulfuric acid and steam, can prevent backflow and suck-back in the process of purifying dilute sulfuric acid, and is safe and reliable while smoothly completing the purifying treatment work; the utility model takes away the organic matters by adopting the steam with the temperature of about 80 ℃, can avoid carbonization of the organic matters caused by the steam with the excessive temperature, and the blackening of the dilute sulfuric acid can influence the recycling of the dilute sulfuric acid after the purification treatment; in general, the utility model has the advantages of good purification treatment effect, high purification treatment efficiency, safety, reliability and high resource recycling rate.
Drawings
Fig. 1 is a schematic diagram of the overall composition structure of the present utility model.
In the figure: 1. the stripping tower 101, the tower body 102, the tower kettle 2, the packing area 3, the liquid distributor 4, the steam outlet 5, the feed inlet 6, the feed flowmeter 7, the feed check valve 8, the feed control valve 9, the feed pipeline 10, the feed pump 11, the liquid level meter B12, the dilute sulfuric acid storage tank 13, the extraction pump 14, the discharge control valve 15, the discharge pipeline 16, the gas distributor 17, the discharge flowmeter 18, the thermometer A19, the vacuum gauge 20, the steam pipeline 21, the steam inlet check valve 22, the steam inlet flowmeter 23, the steam inlet control valve 24, the water supplementing control valve 25, the water supplementing pipeline 26, the thermometer B27, the liquid level meter A28, the hot water tank 29, the rectification recovery system 30, the condensate control valve 31, the condensate recovery tank 32, the condenser 33, the steam outlet control valve 34, the vacuum control valve A35, the vacuum control valve B36, the vacuum device 37 and the vacuum buffer tank.
Detailed Description
The technical scheme of the utility model is further specifically described below with reference to the accompanying drawings.
As shown in figure 1, the utility model aims to mainly solve the problem of dilute sulfuric acid purification treatment after chloromethane drying, and to purify and recycle sulfuric acid, reduce resource waste and avoid the problem of safety and environmental protection.
The device mainly comprises a hot water tank 28, a stripping tower 1, a feed pump 10, a extraction pump 13, a condenser 32, a condensate recovery tank 31 and a vacuum buffer tank 37.
The stripping tower 1 is characterized in that the main body of the stripping tower 1 is divided into a tower kettle 102 and a tower body 101, the tower body 101 and the tower kettle 102 are internally treated by lining fluorine, and the tower kettle 102 is connected with the lower part of the tower body 101 by using a flange.
The tower kettle 102 is provided with a thermometer A18 and a vacuum gauge 19.
The height of the packing region 2 in the tower body 101 is 1/2,1/2 of the height of the tower body 101 is high, the residence time of sulfuric acid in the packing can be prolonged, the sulfuric acid is fully contacted by steam, organic matters are removed more thoroughly, the packing position is in the middle of the tower body 101, grid plates are arranged on the upper portion and the lower portion of the packing region 2, the material is polytetrafluoroethylene material, the packing is of a tetrafluoropall ring type, the tetrafluoropall ring is convenient for the sulfuric acid to fully contact with the steam, meanwhile, the tetrafluoropall ring has strong acid and alkali corrosion resistance, is difficult to be corroded, and is basically not influenced by the sulfuric acid after long-term use.
The outer layer of the hot water tank 28 is a jacket, water in the tank can be heated, the water temperature is maintained to be 80+/-2 ℃, a stable steam source is provided for the stripping tower 1, when the liquid temperature in the tower kettle 102 is higher, the sulfuric acid in the packing area 2 of the tower body 101 is higher, organic matters are carbonized and the sulfuric acid is blackened, so that the water temperature is maintained to be about 80 ℃, the tank body of the hot water tank 28 is reasonably provided with a thermometer B26 and a liquid level meter A27, and a steam inlet control valve 23, a steam inlet one-way valve 21 and a steam inlet flowmeter 22 are arranged on a steam pipeline 20 before steam enters the stripping tower 1.
The steam pipeline 20 of hot water jar 28 get into tower cauldron 102 bottom, terminal connection gas disperser 16, gas disperser 16 is porous structure, further is convenient for steam and sulphuric acid fully contact, carries out secondary purification to sulphuric acid, more that the organic matter was taken away, purifying treatment effect is better, steam gets into tower body 101 behind tower cauldron 102, heats tower body 101, fully contacts with dilute sulphuric acid, carries out purifying treatment to dilute sulphuric acid, steam outlet 4 is located the tower body 101 top, is connected with condenser 32 through the pipeline.
The device is characterized in that a feed inlet 5 for dilute sulfuric acid to be purified is arranged above the filler zone 2 and below the steam outlet 4, the dilute sulfuric acid to be purified enters the tower body 101 from the feed inlet 5, steam contacts with the dilute sulfuric acid through the filler, heat is released at the same time, organic matters in the dilute sulfuric acid are carried out of the tower body 101, condensation recovery is carried out after the organic matters are output from the steam outlet 4, and the dilute sulfuric acid after the purification enters the tower kettle 102.
The feeding pump 10 outputs dilute sulfuric acid to be purified to the feeding port 5 of the tower body 101 through the feeding pipeline 9, the feeding port 5 is connected with the liquid distributor 3 in the tower body 101, the feeding pipeline 9 is provided with the feeding control switch 8, the feeding flowmeter 6 and the feeding one-way valve 7, the feeding control switch 8, the feeding flowmeter 6 and the feeding one-way valve 7 are made of polytetrafluoroethylene materials, and the feeding pipeline 9 is made of polytetrafluoroethylene or fluorine-lined materials.
The extraction pump 13 extracts the dilute sulfuric acid which is located in the tower kettle 102 and is subjected to purification treatment, one end of the discharge pipeline 15 is located at the bottom of the tower kettle 102, the dilute sulfuric acid storage tank 12 is driven in through the extraction pump 13, the liquid level meter B11 is installed on the dilute sulfuric acid storage tank 12 and is used for displaying the height of stored sulfuric acid, the purified dilute sulfuric acid is timely turned out, the discharge pipeline 15 is provided with the discharge control switch 14 and the discharge flowmeter 17, the discharge control switch 14 and the discharge flowmeter 17 are made of polytetrafluoroethylene materials, and the discharge pipeline 15 is made of polytetrafluoroethylene materials or fluorine-lined materials.
The condenser 32 is used for cooling the steam fully contacted with the dilute sulfuric acid, and the steam carrying the organic matters enters the condenser 32 through a steam outlet 4 and is cooled into liquid in the condenser.
The condenser 32 adopts a tubular condenser, the pipeline is respectively connected with the condensate recovery tank 31 and the vacuum buffer tank 37, the condenser 32 is made of graphite, the corrosion is reduced, and the cost is saved.
The condensate recovery tank 31 is used for collecting condensate, and separating methanol, methylal and the like from the condensate through the rectification system 29, so that the condensate can be continuously recycled, and the resource waste is reduced.
The vacuum buffer tank 37 provides a stable negative pressure condition for the whole device, ensures the vacuum stability of the whole device and is connected with the vacuum device 36 through a pipeline.
After the installation, the utility model can be put into use, dilute sulfuric acid to be purified is continuously input into the tower body 101 through the feeding pump 10 and the feeding pipeline 9, is uniformly dispersed by the liquid distributor 3 and then is sprayed on the filler, the dilute sulfuric acid flows through the filler area 2, steam is fully contacted with the sulfuric acid through the filler, and simultaneously releases heat, organic matters in the sulfuric acid are brought out of the tower body 101 from the steam outlet 4, enter the condenser 32 for condensation recovery, condensate is recovered and enters the condensate recovery tank 31, the sulfuric acid after being purified by the steam enters the tower kettle 102, and the sulfuric acid in the tower kettle 102 is the sulfuric acid after being purified.
The utility model adopts the stripping tower 1, has good treatment effect and high treatment efficiency, and simultaneously the stripping tower 1 and the pipeline thereof adopt polytetrafluoroethylene materials or fluorine-lined materials for treatment, thereby being corrosion-resistant and reducing the maintenance consumption of equipment and pipelines.
The utility model is carried out under the condition of micro negative pressure, and is used for continuously feeding and continuously extracting, thereby realizing the continuous treatment of dilute sulfuric acid, reducing links of intermediate feeding and discharging and reducing dangerous operation.
The steam pipeline 20 and the feeding pipeline 9 for dilute sulfuric acid to be purified are both provided with one-way valves, so that backflow and suck-back can be prevented in the process of purifying dilute sulfuric acid.
The novel dilute sulfuric acid treatment device can continuously treat dilute sulfuric acid, the COD value of the dilute sulfuric acid can be reduced to below 1000mg/L from about 600000mg/L, the purified sulfuric acid can be concentrated again, the concentrated sulfuric acid can be continuously used in production, the risk coefficient is greatly reduced, and the treatment cost is reduced.
The foregoing description of the preferred embodiments of the utility model is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the utility model.

Claims (5)

1. The utility model provides a dilute sulfuric acid continuous purification treatment device, includes the stripper that comprises tower cauldron and tower body, its characterized in that: the middle part of the tower body is provided with a filling area, the height of the filling area is half of the height of the tower body, grid plates made of polytetrafluoroethylene are arranged on the upper part and the lower part of the filling area, the filling of the filling area is tetrafluoropall rings, the upper end of the tower body is provided with a steam outlet, the steam outlet is externally connected with a condenser, the condenser is connected with a condensate recovery tank and a vacuum buffer tank, the upper part of the tower body is provided with a feed inlet close to the steam outlet, the feed inlet is internally connected with a liquid distributor which is equal in height and is positioned in the center of the upper part of the tower body, the feed inlet is provided with a feed control valve, a feed one-way valve and a feed flowmeter, the utility model discloses a steam turbine, including tower cauldron, dilute sulphuric acid holding vessel, feed inlet, discharge pump, steam pipe, thermometer A and vacuum gauge are installed to the feed inlet, thermometer A and vacuum gauge are installed to the tower cauldron, the tower cauldron bottom is equipped with the discharge pipeline, the discharge pipeline passes through the discharge pump and connects dilute sulphuric acid holding vessel, install ejection of compact control valve and ejection of compact flowmeter on the discharge pipeline, the tower cauldron upper end is equipped with steam pipe, the steam pipe inscription is located the gas disperser of tower cauldron bottom, the external hot water tank of steam pipe, install level gauge A and thermometer B on the hot water tank, install admission control valve, admission check valve and admission flowmeter on the steam pipe.
2. The continuous purification treatment apparatus for dilute sulfuric acid according to claim 1, wherein: the condenser is a graphite tubular condenser, the steam outlet is connected with the condenser through a steam outlet control valve, the condenser is connected with a vacuum buffer tank through a vacuum control valve A, the vacuum buffer tank is externally connected with a vacuum device through a vacuum control valve B, and the condensate recovery tank is externally connected with a rectification recovery system through a condensate control valve.
3. The continuous purification treatment apparatus for dilute sulfuric acid according to claim 1, wherein: the hot water tank is heated by a jacket, and is externally connected with a water supplementing pipeline through a water inlet control valve.
4. The continuous purification treatment apparatus for dilute sulfuric acid according to claim 1, wherein: the gas disperser is of a porous structure.
5. The continuous purification treatment apparatus for dilute sulfuric acid according to claim 1, wherein: and a liquid level meter B is arranged on the dilute sulfuric acid storage tank.
CN202321322739.5U 2023-05-29 2023-05-29 Dilute sulfuric acid continuous purifying treatment device Active CN219848217U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202321322739.5U CN219848217U (en) 2023-05-29 2023-05-29 Dilute sulfuric acid continuous purifying treatment device

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202321322739.5U CN219848217U (en) 2023-05-29 2023-05-29 Dilute sulfuric acid continuous purifying treatment device

Publications (1)

Publication Number Publication Date
CN219848217U true CN219848217U (en) 2023-10-20

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Family Applications (1)

Application Number Title Priority Date Filing Date
CN202321322739.5U Active CN219848217U (en) 2023-05-29 2023-05-29 Dilute sulfuric acid continuous purifying treatment device

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CN (1) CN219848217U (en)

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