Chloroacetic acid production device for glycine processing
By introducing automated detection equipment and gas distributors into the chloroacetic acid production unit, the problems of misjudgment of the reaction endpoint and inaccurate catalyst addition were solved, achieving efficient control of the chlorination reaction and improving the product quality of glycine.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- HENAN HDF CHEM CO LTD
- Filing Date
- 2025-05-27
- Publication Date
- 2026-05-05
AI Technical Summary
Existing chloroacetic acid production facilities have misjudgments in determining the reaction endpoint, leading to side reactions, making it difficult to recover and reuse the catalyst, affecting the quality of glycine products, and causing the catalyst to be added inaccurately, resulting in excessive sulfate content.
A production apparatus including a chlorination reactor and a proportioning reactor was designed. It is equipped with automated detection equipment such as a radar level gauge, an online component analyzer, an online thermometer, and an online hydrometer. Combined with remote data transmission from a DCS computer, it realizes real-time monitoring and control of the reaction. The uniformity and accuracy of the reaction are ensured by a gas distributor and a catalyst metering tank.
It improves the accuracy of the chlorination reaction endpoint, reduces the occurrence of side reactions, ensures the precise addition of catalyst, improves the product quality of glycine, and reduces analytical errors and material waste.
Smart Images
Figure CN224194707U_ABST
Abstract
Description
Technical Field
[0001] This utility model belongs to the field of chemical technology, specifically relating to a chloroacetic acid production apparatus for processing aminoacetic acid. Background Technology
[0002] Glycine, also known as glycine or glucoside, is a white monoclinic or hexagonal crystal, or a white crystalline powder. It is odorless, has a characteristic sweet taste, is easily soluble in water, slightly soluble in methanol and ethanol, and almost insoluble in acetone and ether. Glycine is mainly used for the decarbonization of fertilizers, in pharmaceuticals and pesticides, and is one of the raw materials for the synthesis of glyphosate via the alkyl ester method. It can also be used as a raw material and preservative in cosmetics, and has a relatively broad market and application prospects. Currently, the main method for synthesizing glycine in China is the chloroacetic acid amination method, using hexamethylenetetramine aqueous solution as a catalyst, synthesized in an aqueous or alcoholic phase at room temperature and pressure, followed by alcohol precipitation, centrifugation, purification, and drying to obtain the product glycine. In the production of chloroacetic acid, sulfur is often used as a catalyst, with acetic acid and chlorine as raw materials reacting in a chlorination reactor. After the reaction, a certain amount of water is added to the product to prevent crystallization, and then it is transferred to an ammonia plant as a raw material. In the chloroacetic acid production process, the current method of determining the reaction endpoint is usually based on the change in the specific gravity of the materials. This method has limitations and is prone to misjudgment, ultimately leading to side reactions and affecting product quality. Furthermore, the catalyst (sulfur powder) used in the preparation of chloroacetic acid is often drawn into the reactor under negative pressure, which makes proportion control difficult. As the reaction proceeds, sulfur is difficult to recover and reuse, and it also enters the byproduct hydrogen chloride, causing the sulfate content in the prepared hydrochloric acid to exceed the standard, rendering it unusable as a raw material for production applications. This also significantly impacts the byproducts. Therefore, to change the catalyst and its addition method, accurately determine the chlorination reaction endpoint, improve product quality, and solve the production problem of chlorinated liquid for glycine processing, it is necessary to develop a new chloroacetic acid production unit for glycine processing. Utility Model Content
[0003] The purpose of this invention is to overcome the shortcomings of the prior art and provide a chloroacetic acid production device for processing glycine with a reasonable structural design and good performance.
[0004] The purpose of this utility model is achieved as follows: A chloroacetic acid production device for processing glycine includes a chlorination reactor and a proportioning reactor. The chlorination reactor is cylindrical in shape, with an inner jacket on its outer wall. A level gauge (a) is vertically connected to the side end. A discharge pipe is located in the middle of the lower surface. From left to right, the upper surface is equipped with a radar level gauge, a chlorine inlet pipe, an online component analyzer, an online thermometer, an online hydrometer, a condenser, a catalyst injection pipe, and an acetic acid inlet pipe. A cooling water inlet pipe is connected to the lower left end of the jacket, and a cooling water outlet pipe is connected to the upper right end. One end of the chlorine inlet pipe is located at the bottom inside the chlorination reactor and connected to an annular gas distributor. The other end is located outside the chlorination reactor and connected to a digital flow meter. A condenser is connected to the condenser, and the upper end of the condenser is equipped with... It has an outlet, which is connected to an absorption tower. The lower end is connected to a reflux pipe, and the reflux pipe is connected to a condenser pipe. The catalyst injection pipe is connected to a catalyst metering tank, and the upper end of the catalyst metering tank is equipped with a catalyst replenishment pipeline. There are multiple mixing kettles, which are respectively set on the lower side of the chlorination kettle. Each kettle includes a kettle body and a stirring shaft. The side end of the kettle body is vertically connected to a level gauge b. The middle of the lower surface is provided with a discharge pipe. The right side of the upper surface is connected to a water replenishment pipe. The left side of the upper surface is provided with an inlet pipe and an online moisture measuring device. The inlet pipe is connected to the discharge pipe. The stirring shaft rotates vertically and passes through the center of the upper surface of the kettle body. The upper end of the stirring shaft is located outside the kettle body and is connected to a stirring motor. The lower end is located inside the kettle body and is connected to a frame-type stirring paddle.
[0005] Furthermore, an observation port is provided on the right side of the upper surface of the chlorination reactor, and a transparent explosion-proof glass is fixedly installed inside the observation port, with an explosion-proof searchlight installed above it.
[0006] Furthermore, the chlorination vessel is externally fitted with an insulation layer.
[0007] Furthermore, the stirring motor is a variable frequency motor, and it is equipped with a protective net.
[0008] Furthermore, control valves are installed on the cooling water inlet pipe, the cooling water outlet pipe, the chlorine gas inlet pipe, the condenser pipe, the catalyst injection pipe, the acetic acid inlet pipe, the outlet pipe, the water replenishment pipe, and the liquid inlet pipe. The control valves can be adjusted on-site or remotely.
[0009] Furthermore, the radar level gauge, the online component analyzer, the online thermometer, the online hydrometer, and the online moisture measuring device are all externally connected to a DCS computer for remote transmission of detection data.
[0010] The beneficial effects of this utility model are as follows: By setting up a radar level gauge, an online component analyzer, an online thermometer, an online hydrometer, and an online moisture measuring device, and by connecting the above devices and instruments to an external DCS computer for remote transmission of detection data, this utility model can understand the reaction situation in the chlorination reactor through automated detection and analysis, and make timely adjustments and controls, improve the judgment of the chlorination reaction endpoint, reduce the occurrence of side reactions, and reduce the need for human intervention in sampling and analysis, thereby reducing analytical errors and increasing the quality of chloroacetic acid used in the processing of glycine.
[0011] By setting up a gas distributor, the uniformity of chlorine gas injected into the chlorination reactor can be increased, thereby ensuring more thorough contact between gas and liquid, a more complete reaction, and reducing material waste and loss. By setting up a catalyst metering tank, the amount of catalyst added can be precisely controlled, thus accurately controlling the chlorination reaction and reducing the introduction of impurities and the occurrence of side reactions. By setting up a level gauge and a radar level meter, the detection results can be easily compared, thereby avoiding the problem of misjudgment of the level due to false level readings. In summary, this utility model has the advantages of reasonable structural design and good performance. Attached Figure Description
[0012] Figure 1 This is a schematic diagram of the structure of this utility model.
[0013] In the diagram: 1. Chlorination vessel; 11. Level gauge a; 12. Discharge pipe; 13. Radar level gauge; 14. Online component analyzer; 15. Online thermometer; 16. Online hydrometer; 17. Cooling water inlet pipe; 18. Cooling water outlet pipe; 19. Observation port; 2. Mixing vessel; 21. Vessel body; 22. Stirring shaft; 23. Level gauge b; 24. Discharge pipe; 25. Water replenishment pipe; 26. Liquid inlet pipe; 27. Online moisture measuring device; 28. Stirring motor; 29. Frame-type stirring paddle; 3. Chlorine gas inlet pipe; 4. Condenser pipe; 5. Catalyst filling pipe; 6. Acetic acid inlet pipe; 7. Gas distributor; 8. Condenser; 81. Discharge port; 82. Reflux pipe; 9. Catalyst metering tank. Detailed Implementation
[0014] The present invention will be further described below with reference to the accompanying drawings.
[0015] Example: Figure 1As shown, a chloroacetic acid production apparatus for processing glycine includes a chlorination reactor 1 and a proportioning reactor 2. The chlorination reactor 1 is cylindrical in shape, with an internal jacket on its outer wall. A level gauge a11 is vertically connected to the side end. A discharge pipe 12 is located in the middle of the lower surface. The upper surface, from left to right, is equipped with a radar level gauge 13, a chlorine inlet pipe 3, an online component analyzer 14, an online thermometer 15, an online hydrometer 16, a condenser 4, a catalyst injection pipe 5, and an acetic acid inlet pipe 6. A cooling water inlet pipe 17 is connected to the lower left end of the jacket, and a... The cooling water outlet pipe 18; one end of the chlorine gas inlet pipe 3 is located at the bottom of the chlorination reactor 1 and connected to an annular gas distributor 7; the other end is located outside the chlorination reactor 1 and connected to a digital gas flow meter; the condenser pipe 4 is connected to a condenser 8, and the upper end of the condenser 8 is provided with an outlet 81, which is connected to an absorption tower; the lower end is connected to a return pipe 82, and the return pipe 82 is interconnected with the condenser pipe 4; the catalyst injection pipe 5 is connected to a catalyst metering tank 9, and the upper end of the catalyst metering tank 9 is provided with a catalyst replenishment pipeline.
[0016] Multiple mixing vessels 2 are respectively located on the lower side of the chlorination vessel 1. Each vessel includes a vessel body 21 and a stirring shaft 22. A liquid level gauge b23 is vertically connected to the side end of the vessel body 21. A discharge pipe 24 is provided in the middle of the lower surface. A water supply pipe 25 is connected to the right side of the upper surface. An inlet pipe 26 and an online moisture measuring device 27 are provided on the left side of the upper surface. The inlet pipe 26 is connected to the discharge pipe 12. The stirring shaft 22 is vertically rotatably inserted through the center of the upper surface of the vessel body 21. The upper end of the stirring shaft 22 is located outside the vessel body 21 and is externally connected to a stirring motor 28. The lower end is located inside the vessel body 21 and is connected to a frame-type stirring paddle 29.
[0017] An observation port 19 is provided on the right side of the upper surface of the chlorination reactor 1. A transparent explosion-proof glass is fixedly installed inside the observation port 19, and an explosion-proof searchlight is installed above it. The observation port 19 allows for easy observation of the reaction inside the chlorination reactor 1. An insulation layer is fixedly fitted onto the outside of the chlorination reactor 1, providing insulation and protection. The stirring motor 28 is a variable frequency motor, and a protective net is fitted onto its exterior to prevent foreign objects from entering the stirring motor 28 and affecting its normal operation. The cooling water inlet pipe... 17. Control valves are installed on the cooling water outlet pipe 18, the chlorine inlet pipe 3, the condenser pipe 4, the catalyst injection pipe 5, the acetic acid inlet pipe 6, the discharge pipe 12, the water replenishment pipe 25, and the liquid inlet pipe 26. The control valves can be adjusted on-site and remotely. The radar level gauge 13, the online component analyzer 14, the online thermometer 15, the online hydrometer 16, and the online moisture measuring device 27 are all connected to a DCS computer for remote transmission of detection data.
[0018] In use, this invention first introduces chlorine and acetic acid, the raw materials for chloroacetic acid production, into the chlorination reactor 1 via chlorine inlet pipe 3 and acetic acid inlet pipe 6, respectively. During this process, the gas distributor 7 increases the uniformity of the chlorine gas injected into the chlorination reactor 1, resulting in more thorough gas-liquid contact, a more complete reaction, and reduced material waste. Next, liquid acetic anhydride catalyst is quantitatively added into the chlorination reactor 1 via catalyst metering tank 9 and catalyst injection pipe 5. The catalyst metering tank 9 allows for precise control of the amount of liquid acetic anhydride catalyst added, thereby accurately controlling the chlorination reaction and reducing the introduction of impurities. The process involves detecting and analyzing the gas-liquid mixture inside the chlorination reactor 1, including the introduction of side reactions. Subsequently, the system uses a radar level gauge 13, an online component analyzer 14, an online thermometer 15, and an online hydrometer 16 to automatically detect and analyze the mixture. The radar level gauge 13 measures the liquid level inside the chlorination reactor 1 and compares it with the data from the level gauge a11 to avoid false readings. The online component analyzer 14 analyzes the composition of the material inside the chlorination reactor 1 to understand the chlorination reaction process, track the reaction progress and endpoint, and facilitate timely adjustments and control. The online thermometer 15 measures the temperature inside the chlorination reactor 1 and transmits the measured data. The data is transmitted to the DCS computer for analysis. Simultaneously, the temperature inside the chlorination reactor 1 is regulated and controlled via remote adjustment of the control valves of the cooling water inlet pipe 17 and cooling water outlet pipe 18, using a jacketed cooling system. An online hydrometer 16 measures the specific gravity of the materials inside the chlorination reactor 1, monitoring changes in specific gravity as a basis for determining the reaction endpoint. Furthermore, the condenser 8 and condenser pipe 4 are used to condense and filter the gases produced during the chlorination reaction. Finally, the crude chlorinated liquid produced after the chlorination reaction is completed can be injected into the reactor body 21 of the proportioning reactor 2 via the discharge pipe 12 and the inlet pipe 26. After completing the above operations, the stirring motor 28 is turned on, and water is added to the inside of the vessel 21 through the water supply pipe 25. At this time, the stirring motor 28 is turned on, which drives the stirring shaft 22 and the frame stirring paddle 29 to rotate, thereby achieving uniform mixing of crude chlorination solution and water through the frame stirring paddle 29. In addition, during this process, the moisture content of the material in the vessel 21 can be measured by the online moisture measuring device 27 to prevent the addition of too much or too little water, thereby accurately controlling the amount of water added. Finally, after the crude chlorination solution and water are mixed according to the ratio, the resulting chloroacetic acid solution can be discharged through the discharge pipe 24 and enter the subsequent production process.This invention employs this structure to understand the reaction situation within the chlorination reactor 1 through automated detection and analysis, enabling timely adjustments and control. This improves the accuracy of determining the chlorination reaction endpoint and reduces the occurrence of side reactions. It effectively solves problems such as difficulty in determining the chlorination reaction endpoint in the glycine chlorination process, difficulty in controlling the amount of catalyst added, and low automation in analysis and detection. This increases the quality of chloroacetic acid used in glycine processing. Overall, this invention has the advantages of a reasonable structural design and good performance.
[0019] The above embodiments are only used to illustrate the technical solution of this utility model and are not intended to limit it. Although the utility model has been described in detail with reference to the above embodiments, those skilled in the art should understand that modifications or equivalent substitutions can still be made to the specific implementation of this utility model without departing from the spirit and scope of this utility model. Any modifications or equivalent substitutions should be covered within the scope of the claims of this utility model.
Claims
1. A chloroacetic acid production apparatus for processing glycine, comprising a chlorination reactor (1) and a proportioning reactor (2), characterized in that: The chlorination reactor (1) is cylindrical in shape, with an inner jacket on its outer wall. A level gauge a (11) is vertically connected to the side end. A discharge pipe (12) is located in the middle of the lower surface. The upper surface is equipped with a radar level gauge (13), a chlorine feed pipe (3), an online component analyzer (14), an online thermometer (15), an online hydrometer (16), a condenser (4), a catalyst injection pipe (5), and an acetic acid feed pipe (6) from left to right. The lower left end of the jacket is connected to a cooling water inlet pipe (17), and the upper right end is connected to a cooling water outlet pipe (18). The chlorine feed pipe (3) One end is located at the bottom of the chlorination vessel (1) and connected to an annular gas distributor (7), and the other end is located outside the chlorination vessel (1) and connected to a gas digital flow meter. The condenser (4) is connected to a condenser (8), and the upper end of the condenser (8) is provided with an outlet (81), which is connected to an absorption tower. The lower end is connected to a return pipe (82), and the return pipe (82) is connected to the condenser (4). The catalyst injection pipe (5) is connected to a catalyst metering tank (9), and the upper end of the catalyst metering tank (9) is provided with a catalyst replenishment pipeline. There are multiple mixing tanks (2), which are respectively set below the side of the chlorination tank (1). Each tank includes a tank body (21) and a stirring shaft (22). A liquid level gauge b (23) is vertically connected to the side end of the tank body (21). A discharge pipe (24) is provided in the middle of the lower surface. A water supply pipe (25) is connected to the right side of the upper surface. An inlet pipe (26) and an online moisture measuring device (27) are provided on the left side of the upper surface. The inlet pipe (26) is connected to the outlet pipe (12). The stirring shaft (22) is vertically rotated and passes through the center of the upper surface of the tank body (21). The upper end of the stirring shaft (22) is located outside the tank body (21) and is connected to a stirring motor (28). The lower end is located inside the tank body (21) and is connected to a frame-type stirring paddle (29).
2. The chloroacetic acid production apparatus for processing glycine as described in claim 1, characterized in that: An observation port (19) is provided on the right side of the upper surface of the chlorination vessel (1). A transparent explosion-proof glass is fixedly installed inside the observation port (19), and an explosion-proof searchlight is installed above it.
3. The chloroacetic acid production apparatus for processing glycine as described in claim 1, characterized in that: The chlorination vessel (1) is externally fitted with an insulation layer.
4. The chloroacetic acid production apparatus for processing glycine as described in claim 1, characterized in that: The stirring motor (28) is a variable frequency motor, and a protective net is installed on its exterior.
5. The chloroacetic acid production apparatus for processing glycine as described in claim 1, characterized in that: Control valves are installed on the cooling water inlet pipe (17), the cooling water outlet pipe (18), the chlorine gas inlet pipe (3), the condenser pipe (4), the catalyst injection pipe (5), the acetic acid inlet pipe (6), the outlet pipe (12), the water replenishment pipe (25), and the liquid inlet pipe (26). The control valves can be adjusted on-site or remotely.
6. The chloroacetic acid production apparatus for processing glycine as described in claim 1, characterized in that: The radar level gauge (13), the online component analyzer (14), the online thermometer (15), the online hydrometer (16), and the online moisture measuring device (27) are all connected to an external DCS computer for remote transmission of detection data.