Chemical fluorosulfonic acid preparation and tail gas recovery system

Abstract

The utility model discloses a fluorosulfonic acid preparation and tail gas recovery system for chemical industry belongs to organic chemical production technical field, solved the reaction temperature difficult control, byproduct hydrogen chloride cannot be absorbed thoroughly, environmental pollution serious etc.

Description

Technical Field

[0001] This utility model belongs to the field of organic chemical production technology, specifically relating to a chemical fluorosulfonic acid preparation and tail gas recovery system. Background Technology

[0002] Fluorosulfonic acid, as an important chemical raw material, is widely used in organic synthesis, pharmaceutical manufacturing, pesticide production, and fine chemicals. Its unique chemical properties make it a key catalyst and reagent in many reactions. However, traditional fluorosulfonic acid preparation processes have many problems, limiting its wider application and development. In traditional processes, fluorosulfonic acid is usually synthesized by reacting anhydrous hydrogen fluoride (HF) with chlorosulfonic acid (ClSO3H).

[0003] This process involves two highly corrosive and toxic chemicals, and the alternating endothermic and exothermic reactions make precise temperature control difficult. This unstable temperature condition increases operational complexity and increases the risk of explosions or burns, posing a serious threat to operator safety. Furthermore, hydrogen chloride (HCl), a byproduct of fluorosulfonic acid production, is often not completely absorbed. Untreated hydrogen chloride emissions into the environment cause severe air pollution, corrode surrounding buildings and equipment, and negatively impact human health. Long-term exposure to high concentrations of hydrogen chloride can lead to respiratory illnesses and other health problems; therefore, effectively treating these exhaust gases is a pressing issue. Utility Model Content

[0004] This invention provides a system for preparing chemical-grade fluorosulfonic acid and recovering its tail gas, in order to solve the problems mentioned in the background art.

[0005] Therefore, the present invention adopts the following technical solution: A chemical fluorosulfonic acid preparation and tail gas recovery system includes a raw material storage tank, a reaction vessel, a reflux tower, a falling film absorber, a water washing tower, an alkali washing tower, and related valves, instruments, and equipment.

[0006] The raw material storage tanks include an anhydrous hydrogen fluoride storage tank and an anhydrous chlorosulfonic acid storage tank, both constructed of corrosion-resistant metal and meeting relevant pressure vessel requirements. The bottom of the anhydrous hydrogen fluoride storage tank is connected to a hydrogen fluoride metering pump via pipeline, with a flow meter and regulating valve installed on the pipeline. The bottom of the anhydrous chlorosulfonic acid storage tank is equipped with a chlorosulfonic acid metering pump, with a flow meter and regulating valve installed on the pipeline.

[0007] The reactor is made of corrosion-resistant material and meets the relevant requirements for pressure vessels. It is equipped with a cooling coil that leads to a circulating water pipeline. A regulating valve is installed on the circulating water inlet pipeline. A thermometer is installed on the top of the reactor and interlocked with the PLC controller. The reaction is carried out by setting the flow rate and the reactor temperature is controlled by the circulating water regulating valve.

[0008] A reflux tower is installed at the top of the reactor, and a condenser is installed at the top of the reflux tower. The condenser is cooled by circulating water, and packing (PP Pall rings) is installed at the bottom. The reaction gas phase is sent to the reflux tower for separation through the gas phase pipe, and hydrogen chloride enters the falling film absorber through the gas phase pipe.

[0009] The falling film absorber absorbs hydrogen chloride by adding primary water, and a regulating valve is installed on the primary water delivery pipeline. The absorbed hydrogen chloride is converted into hydrochloric acid, which flows through a pipeline to an acid circulation tank. A level gauge is installed at the bottom of the acid circulation tank, and an absorption circulation pump is installed at the bottom of the acid circulation tank, forming its own circulation with the falling film absorber through pipelines.

[0010] Unabsorbed gas phase from the falling film absorber enters the water washing tower through a pipeline. The water washing tower is constructed with a PTFE-lined rigid frame and a packing section in the middle. The gas phase flows out from the top of the water washing tower. A primary water makeup pipeline with a regulating valve is installed in the bottom of the water washing tower. A level gauge is installed in the bottom of the water washing tower. The bottom of the bottom is connected to a water washing pump via a pipeline, which is then connected to the top of the water washing tower, and a regulating valve controls the flow rate.

[0011] Unabsorbed gas phase from the water washing tower is sent to the alkali washing tower via pipeline. The alkali washing tower is made of PTFE-lined steel with a packing section in the middle. The gas phase enters the alkali washing tower through the pipeline and flows out from the top. An alkali pipeline is installed in the bottom of the alkali washing tower, and a regulating valve is installed on the pipeline. A level gauge is installed in the bottom of the alkali washing tower. The bottom of the bottom is connected to the alkali washing pump through a pipeline, which is connected to the top of the alkali washing tower through a pipeline, and a regulating valve is installed to control the flow rate.

[0012] The beneficial effects of this utility model are as follows: This invention provides a highly efficient, safe, and environmentally friendly process for the preparation of fluorosulfonic acid and the recovery of tail gas. It solves the problems of difficult-to-control reaction temperature, incomplete absorption of byproduct hydrogen chloride, and serious environmental pollution in the prior art, thereby improving production efficiency, reducing environmental pollution, and ensuring production safety. Attached Figure Description

[0013] Figure 1 This is a diagram showing the structural connections of the equipment according to this utility model; In the diagram, 1-anhydrous hydrogen fluoride storage tank, 2-anhydrous chlorosulfonic acid storage tank, 3-reaction vessel, 4-reflux tower, 5-falling film absorber, 6-acid circulation tank, 7-water washing tower, 8-alkali washing tower, 9-waste alkali tank, 10-hydrochloric acid tank, 11-PLC control. Detailed Implementation

[0014] The present invention will be further described below with reference to the accompanying drawings and specific embodiments: It also includes: hydrogen fluoride metering pump B1, chlorosulfonic acid metering pump B2, absorption circulation pump B3, water washing circulation pump B4, alkali washing circulation pump B5, regulating valve T1, regulating valve T2, regulating valve T3, regulating valve T4, regulating valve T5, regulating valve T6, regulating valve T7, regulating valve T8, regulating valve T9, regulating valve T10, regulating valve T11, circulating water inlet X1, circulating water outlet X2, flow meter F1, flow meter F2, level gauge L1, level gauge L2, level gauge L3, vapor phase pipe Q1, vapor phase pipe Q2, vapor phase pipe Q3, vapor phase pipe Q4, vent pipe Q5, thermometer T, cooling coil G, primary water W, acid pipe S1, acid pipe S2, acid pipe S3, acid pipe S4, acid pipe S5, acid pipe S6, alkali pipe J, alkali pipe J1, alkali pipe J2, alkali pipe J3.

[0015] like Figure 1 As shown, anhydrous hydrogen fluoride storage tank 1 and anhydrous chlorosulfonic acid storage tank 2 are respectively added to reaction vessel 3 through metering pumps B1 / B2. Flow meters F1 / F2 and regulating valves T1 / T2 are installed on the pipelines to facilitate the setting and addition of the amount added.

[0016] The reactor 3 is equipped with a cooling coil G that is connected to a circulating water pipe X1. A regulating valve T3 is installed on the circulating water outlet pipe X2. A thermometer T is installed on the top of the reactor 3. The thermometer T is interlocked with the PLC controller 11. The reaction is carried out by setting the flow rate. The temperature of the reactor is controlled by the circulating water regulating valve. The fluorosulfonic acid produced after the reaction is completed is stored in the reactor for later use.

[0017] A reflux tower 4 is installed at the top of the reactor 3 to separate reactants and by-products. A condenser is installed at the top of the reflux tower 4, and the condenser is cooled by circulating water. Packing material (PP Pall rings) is installed at the bottom. The reaction gas phase passes through gas phase Q1 into the reflux tower 4 for separation, and hydrogen chloride enters the falling film absorber 5 through gas phase pipeline Q2.

[0018] The falling film absorber 5 absorbs hydrogen chloride by adding primary water W, and a regulating valve T4 is installed on the primary water delivery pipeline. The absorbed hydrogen chloride generates hydrochloric acid, which flows to the acid circulation tank 6 through pipeline S1, and a level gauge L1 is installed at the bottom.

[0019] An absorption circulation pump B3 is installed at the bottom of the acid circulation tank 6. It forms a self-circulating absorption of the by-product hydrogen chloride through the falling film absorber 5 via the pipeline S2. When the hydrochloric acid concentration in the acid circulation tank reaches 32%, the regulating valve T11 on the pipeline S3 is opened to transport the acid to the hydrochloric acid tank 9.

[0020] Unabsorbed gas phase from falling film absorber 5 enters water washing tower 7 through pipeline Q3. The water washing tower is made of PTFE-lined steel with a packing section in the middle. The gas phase flows out from the top of water washing tower 7 through pipeline Q3. A primary water replenishment pipeline is installed in the bottom of the water washing tower, and a regulating valve T5 is installed on the pipeline. A level gauge L2 is installed in the bottom of water washing tower 7. The bottom of the bottom is connected to water washing pump B4 through pipeline S4, and connected to the top of water washing tower through pipeline S5. A regulating valve T8 is installed to control the flow rate. It absorbs by-product hydrogen chloride through its own circulation. When the acid concentration in water washing tower 7 reaches 32%, the regulating valve T10 on pipeline S6 is opened to transport hydrochloric acid to hydrochloric acid tank 10.

[0021] Unabsorbed gaseous phase from water washing tower 7 is sent to alkaline washing tower 8 via pipeline Q4. Alkaline washing tower 8 is made of PTFE-lined steel with a packing section in the middle. The gaseous phase enters alkaline washing tower 8 through pipeline Q4 and flows out from the top. Alkaline washing tower 8 has an alkali pipeline J at its bottom, with a regulating valve T9 installed on pipeline J. A level gauge L3 is installed at the bottom of alkaline washing tower 8. The bottom of the bottom is connected to alkaline washing pump B5 via pipeline J1, and to the top of alkaline washing tower 8 via pipeline J2, with a regulating valve T7 controlling the flow rate. When the acid concentration in alkaline washing tower 8 is less than 1%, the regulating valve T8 on pipeline J3 is opened to transport waste alkali to waste alkali tank 10, and the unabsorbed gaseous phase from alkaline washing tower 8 is discharged through pipeline Q5.

Claims

1. A system for preparing and recovering fluorosulfonic acid for chemical use, characterized in that, Includes raw material storage tank, reaction vessel (3), reflux tower (4), falling film absorber (5), water washing tower (7), alkali washing tower (8) and related valves and instruments; The raw material storage tanks include an anhydrous hydrogen fluoride storage tank (1) and an anhydrous chlorosulfonic acid storage tank (2). The bottom of the anhydrous hydrogen fluoride storage tank (1) is connected to a hydrogen fluoride metering pump B1 via a pipeline. A flow meter F1 and a regulating valve T1 are installed on the pipeline. The bottom of the anhydrous chlorosulfonic acid storage tank (2) is connected to a chlorosulfonic acid metering pump B2 via a pipeline. A flow meter F2 and a regulating valve T2 are installed on the pipeline. The hydrogen fluoride metering pump B1 and the chlorosulfonic acid metering pump B2 are respectively connected to the reaction vessel (3). The reactor (3) is equipped with a cooling coil G connected to a circulating water pipe. A reflux tower (4) is installed at the top of the reactor (3). A condenser is installed at the top of the reflux tower (4). The condenser is cooled by circulating water. The gas phase pipe Q1 connected to the top of the reactor (3) is sent to the reflux tower (4) for separation. The gas phase pipe Q2 connected to the top of the reflux tower (4) enters the falling film absorber (5). The falling film absorber (5) absorbs water by adding primary water W. The bottom of the falling film absorber (5) is connected to the acid circulation tank (6) via the acid pipe S1. The bottom of the acid circulation tank (6) is equipped with a level gauge L1 and an absorption circulation pump B3. The falling film absorber (5) forms its own circulation through the acid pipe S2. The lower part of the falling film absorber (5) is connected to the gas phase pipe Q3 and enters the top of the water washing tower (7). The bottom of the water washing tower (7) is equipped with a primary water supply pipe; the bottom of the water washing tower (7) is equipped with a level gauge L2. The bottom of the tower is connected to the water washing circulation pump B4 through the acid pipe S4 and connected to the top of the water washing tower (7) through the acid pipe S5. The top of the water washing tower (7) is connected to the gas phase pipe Q4 and sent to the top of the alkali washing tower (8). The bottom of the alkali washing tower (8) is equipped with an alkali pipe J, and a regulating valve T9 is installed on the alkali pipe J. The bottom of the alkali washing tower (8) is equipped with a level gauge L3. The bottom of the bottom of the tower is connected to the alkali washing circulation pump B5 through the alkali pipe J1, and connected to the top of the alkali washing tower (8) through the alkali pipe J2.

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