Device for improving hydrogen chloride removal efficiency
By designing an alkali bottle and a gas distributor in the acetylene hydrochlorination microreactor fixed-bed device, the contact time of hydrogen chloride in the alkali solution is extended, which solves the problem of low hydrogen chloride removal efficiency in vinyl chloride product gas, and improves the accuracy of chromatographic analysis and the service life of the chromatographic column.
Patent Information
- Application Number
- CN202422672190.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-04
- Publication Date
- 2025-11-04
- Estimated Expiration
- 2034-11-04
AI Technical Summary
In existing technologies, trace amounts of hydrogen chloride entrained in the vinyl chloride product gas generated by the hydrochlorination of acetylene are difficult to remove effectively, resulting in reduced column efficiency and poor analytical performance.
Design a device comprising an alkali bottle and a gas distributor. By extending the contact time of the product gas in the alkali solution, the alkali solution absorbs hydrogen chloride. The gas distributor is designed with a ring or tree structure to increase the gas-liquid contact area and residence time.
The removal efficiency of hydrogen chloride reached 99.9%, ensuring the accuracy of chromatographic analysis and the service life of the chromatographic column.
Smart Images
Figure CN223505085U_ABST
Abstract
Description
Technical Field
[0001] This utility model belongs to the field of acetylene hydrochlorination microreactor product gas treatment technology, specifically relating to a device for improving hydrogen chloride removal efficiency in a fixed bed of acetylene hydrochlorination microreactor. Background Technology
[0002] The acetylene hydrochlorination microreactor fixed-bed reactor is a key experimental device for evaluating catalyst performance in the laboratory. During the reaction of acetylene and hydrogen chloride with the catalyst to produce vinyl chloride, trace amounts of hydrogen chloride are carried into the subsequent gas chromatography analysis. Acidic gases such as hydrogen chloride are not easily volatilized and accumulate at the column tip, causing excessive column runoff, tailing of active components, and reduced column efficiency and resolution. Furthermore, acidic gases entering the chromatograph can damage the deactivation surface of the fused silica tubing, leading to deterioration of peak shapes and affecting analytical results. The traditional method for removing hydrogen chloride from the product gas is to perform alkaline washing and dehydration before chromatographic analysis. This method suffers from short contact time between hydrogen chloride and alkaline solution, resulting in low removal efficiency. To address the problem of trace amounts of hydrogen chloride carried by vinyl chloride produced in the acetylene hydrochlorination reaction, this invention proposes a device to minimize the amount of hydrogen chloride in the product gas before it enters the gas chromatograph. Utility Model Content
[0003] This invention proposes a device to improve the removal efficiency of hydrogen chloride, which effectively solves the problem of low hydrogen chloride removal efficiency in traditional product gas treatment systems and is beneficial to the accuracy of data during continuous chromatographic analysis.
[0004] The device for improving hydrogen chloride removal efficiency described in this utility model, such as... Figure 2 As shown, it consists of an alkali bottle 3 and a gas distributor 4 located inside the alkali bottle 3; the alkali bottle 3 is sealed with a rubber stopper 2, and two round holes are provided on the rubber stopper 2, an inlet pipe 1 is inserted into one round hole, and an exhaust pipe 5 is inserted into the other round hole; the alkali bottle 3 contains 60-80% volume of alkali solution.
[0005] Furthermore, the gas distributor 4 has a ring structure. Figure 2 ) or tree structure ( Figure 3 The materials of the exhaust pipe 1 and the exhaust pipe 5 can be glass, stainless steel, copper, aluminum, plastic, ceramic, etc. The material of the intake pipe 1 is the same as that of the gas distributor 4. The material of the exhaust pipe 5 can be glass, stainless steel, copper, aluminum, plastic, ceramic, etc. The inner diameter of the intake pipe 1 is 6-8mm and the inner diameter of the exhaust pipe 5 is 6-8mm.
[0006] Furthermore, the alkali bottle 3 is a wide-mouth bottle, conical bottle, narrow-mouth bottle, etc., with a volume of 500-1000mL. The inlet of the gas inlet pipe 1 is located outside the alkali bottle 3 and is connected to the product gas outlet of the acetylene hydrochlorination micro-reactor fixed bed device. The outlet of the gas inlet pipe 1 is located 1-3cm below the alkali liquid surface inside the alkali bottle 3 and is connected to the gas distributor 4. The inlet of the exhaust pipe 5 is located 1-3cm above the alkali liquid surface inside the alkali bottle 3. The upper and lower surfaces of the gas distributor 4 are provided with distribution holes 6. The product gas in the gas inlet pipe 1 is discharged into the alkali liquid through the distribution holes 6. The hydrogen chloride in the product gas reacts with the alkali liquid and is absorbed. The remaining vinyl chloride gas escapes from the alkali liquid and is discharged from the alkali bottle 3 through the exhaust pipe 5. The portions of the inlet pipe 1 and the outlet pipe 5 located outside the alkali bottle 3 bend outwards at a position 8-15 mm above the rubber stopper 2; the outlet of the outlet pipe 5 is located outside the alkali bottle 3 and is open to the atmosphere, used to balance the gas pressure of the alkali bottle 3 or to take samples of the dried vinyl chloride gas for chromatographic analysis.
[0007] Furthermore, such as Figure 3 As shown, both the gas distributor 4 and the inlet pipe 1 are made of glass and are vertically connected by glass adhesive. The outer diameter of the annular gas distributor 4 is 16-30 mm, and the inner diameter is 10-22 mm. Five to 13 distribution holes 6 are provided on the upper and lower surfaces of the gas distributor 4, each with a diameter of 2-3 mm. The three adjacent distribution holes 6 on the upper and lower surfaces are staggered. This arrangement ensures that no two distribution holes 6 on the upper and lower surfaces are on the same straight line perpendicular to the bottom surface of the alkali bottle 3, increasing the residence time of the product gas in the alkali solution and thus more effectively removing hydrogen chloride gas.
[0008] Furthermore, such as Figure 4As shown, the tree-like gas distributor 4 consists of a central axis pipe and guide vanes. The plane formed by the central axis pipe and guide vanes is parallel to the bottom plane of the alkali bottle 3. The central axis pipe is perpendicularly connected to the inlet pipe 1 and has the same diameter (both inner and outer diameters are equal). The guide vanes are hollow pipes, symmetrically installed on both sides of the central axis pipe, with 6 to 18 guide vanes on each side. The outer edge of the guide vanes on the same side is spaced from the inner wall of the alkali bottle 3 and arranged in an arc shape with the same shape as the inner wall of the alkali bottle 3. The inner diameter of the guide vanes is smaller than that of the inlet pipe 1 and the... The inner diameter of the central axis pipeline and the angle (i.e., the inner inclination angle) between the guide vane and the central axis pipeline are 90 degrees. 15 to 20 distribution holes 6 are provided on the upper and lower surfaces of the central axis pipeline, and 2 to 10 distribution holes 6 are provided on the upper and lower surfaces of each guide vane. The diameter of the distribution holes 6 is 2 to 3 mm. Any two distribution holes 6 on the upper and lower surfaces of the central axis pipeline and the guide vane are not on the same straight line perpendicular to the bottom surface of the alkali bottle 3. This arrangement can increase the residence time of the product gas in the alkali solution, thereby more fully removing hydrogen chloride gas.
[0009] Furthermore, the alkaline solution in the alkaline solution bottle 3 can be a saturated sodium hydroxide solution, a saturated ammonia solution, or a saturated sodium bicarbonate solution.
[0010] Compared with the prior art, the advantages of this utility model are: by extending the contact time of the product gas in the alkaline solution, the removal effect of acidic gases such as hydrogen chloride in the product gas is enhanced, ensuring that gases such as hydrogen chloride in the product gas can be completely removed. Attached Figure Description
[0011] To more clearly illustrate the embodiments of this utility model, the drawings used in the description of the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0012] Figure 1 : A schematic diagram of the structure of the acetylene hydrochlorination microreactor fixed bed device using the apparatus described in this utility model;
[0013] Figure 2 : This is a schematic diagram of the structure of the device described in this utility model;
[0014] Figure 3 : This is a schematic diagram of the ring structure distributor described in this utility model;
[0015] Figure 4 : This is a schematic diagram of the tree-like structure distributor described in this utility model;
[0016] The names of each part are: 1. Inlet pipe, 2. Rubber stopper, 3. Alkali bottle, 4. Gas distributor, 5. Exhaust pipe, 6. Distribution hole. Detailed Implementation
[0017] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.
[0018] Example 1
[0019] like Figure 1 The diagram shows the structure of a micro-reactor fixed-bed device for acetylene hydrochlorination, used in the process of carrying out the acetylene hydrochlorination reaction. It mainly includes an acetylene hydrochlorination reaction system, a product gas treatment system, and a product gas delivery and analysis system. The acetylene hydrochlorination reaction system includes a reactor and feed lines for N2, C2H2, and HCl, as well as pressure gauges. The product gas treatment system includes an alkali bottle and a product gas pretreatment feed valve. The product gas delivery and analysis system consists of a delivery pipe, a dryer, and a gas chromatograph.
[0020] As shown in Figure 2 and Figure 3 As shown, this utility model discloses a device for improving hydrogen chloride removal efficiency. The outlet of the inlet pipe 1 is connected to a gas distributor 4, which is located in the alkali solution in the alkali solution bottle 3. The gas distributor 4 is a ring-shaped distributor made of glass, with an outer diameter of 16mm and an inner diameter of 10mm. The diameter of the distribution holes 6 is 2mm. There are 13 distribution holes 6 on each of the upper and lower surfaces of the distributor 4, with three adjacent distribution holes 6 on the upper and lower surfaces arranged in a staggered manner. The alkali solution bottle 3 is a 500mL narrow-mouth bottle, and 40... A 0 mL, 2 mol / L saturated sodium hydroxide solution is used as the absorbent, and the bottle mouth is sealed with a rubber stopper 2. Two round holes are made on the rubber stopper 2. An inlet pipe 1 is inserted into one round hole, and an exhaust pipe 5 is inserted into the other round hole. The length of the exhaust pipe 5 in the alkali bottle 3 is less than the length of the inlet pipe 1. The outlet of the inlet pipe 1 is directly inserted 2 cm below the surface of the alkali solution and connected to the gas distributor 4. The inlet of the exhaust pipe 5 is located 2 cm above the surface of the alkali solution. The inlet pipe 1 and the exhaust pipe 5 located outside the alkali bottle 3 are bent 10 mm above the rubber stopper.
[0021] In the acetylene hydrochlorination reaction, HCl and C2H2 are introduced into the reactor (containing a gold-based non-mercury catalyst) at a molar ratio of 1.1:1 (N2 is used at a rate of 15 mL / min; nitrogen is used as a protective gas to replace air in the pipeline and to purge impurities such as water vapor volatilized from the catalyst during the drying process, preventing catalyst deactivation under air conditions). The acetylene hydrochlorination reaction produces vinyl chloride product gas. This product gas enters the alkali solution bottle 3 through inlet pipe 1. A product gas pretreatment feed valve is installed on inlet pipe 1 between the reactor and the alkali solution bottle 3. This pretreatment feed valve is a glass ball valve used to regulate the pressure of the product gas entering the alkali solution bottle 3. The alkali solution bottle 3 is secured to inlet pipe 1 and exhaust pipe 5 by a rubber stopper 2. The product gas enters the gas distributor 4 through inlet pipe 1, distributing the product gas evenly within the alkali solution. The alkali bottle 3 contains a 2 mol / L saturated sodium hydroxide solution, with the solution level reaching 80% of the bottle body, ensuring that the alkali solution completely submerges the gas distributor 4. A product gas pretreatment discharge valve is installed on the exhaust pipe 5 outside the alkali bottle 3. After the product gas is washed with alkali to remove hydrogen chloride, it enters the dryer through the exhaust pipe 5. The product gas pretreatment discharge valve is a glass ball valve used to regulate the pressure of the product gas entering the dryer and the gas chromatograph, maintaining the pressure between 0.5 and 0.8 MPa. The product gas dryer is filled with silica gel to completely remove any moisture entrained in the product gas after water washing. The product gas dried by the product gas dryer is then sent to the gas chromatograph for analysis via a rubber tube. Using the device described in this invention, the removal efficiency of hydrogen chloride can reach 99.9%.
[0022] All aspects not detailed in this utility model are conventional technical means known to those skilled in the art. The above description is only a preferred embodiment of this utility model and is not intended to limit this utility model. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this utility model should be included within the protection scope of this utility model.
Claims
1. An apparatus for improving hydrogen chloride removal efficiency, characterized in that: It consists of an alkali bottle (3) and a gas distributor (4) located inside the alkali bottle (3); the alkali bottle (3) is sealed with a rubber stopper (2), and two round holes are provided on the rubber stopper (2). An inlet pipe (1) is inserted into one round hole, and an exhaust pipe (5) is inserted into the other round hole; the alkali bottle (3) contains 60-80% alkali solution by volume; the inlet of the inlet pipe (1) is located outside the alkali bottle (3) and is connected to the product gas outlet of the acetylene hydrochlorination micro-reaction fixed bed device; the outlet of the inlet pipe (1) is located inside the alkali bottle (3). The gas distributor (4) is connected below the surface of the alkaline solution in the bottle (3); the inlet of the exhaust pipe (5) is located above the surface of the alkaline solution in the bottle (3), and the outlet of the exhaust pipe (5) is located outside the bottle (3) and connected to the atmosphere; the upper and lower surfaces of the gas distributor (4) are provided with distribution holes (6); the product gas in the inlet pipe (1) is discharged into the alkaline solution through the distribution holes (6), the hydrogen chloride in the product gas reacts with the alkaline solution and is absorbed, and the remaining vinyl chloride gas escapes from the alkaline solution and is discharged from the alkaline solution bottle (3) through the exhaust pipe (5).
2. The apparatus for improving hydrogen chloride removal efficiency as described in claim 1, characterized in that: The alkali bottle (3) is a wide-mouth bottle, conical bottle or narrow-mouth bottle with a volume of 500-1000mL; the part of the air inlet pipe (1) and the exhaust pipe (5) located outside the alkali bottle (3) bends outward at a position 8-15mm above the rubber stopper (2); the outlet of the air inlet pipe (1) is located 1-3cm below the alkali liquid surface inside the alkali bottle (3), and the inlet of the exhaust pipe (5) is located 1-3cm above the alkali liquid surface inside the alkali bottle (3).
3. The apparatus for improving hydrogen chloride removal efficiency as described in claim 1, characterized in that: The gas distributor (4) has a ring structure or a tree structure, and its material is glass, stainless steel, copper, aluminum, plastic or ceramic. The material of the intake pipe (1) is the same as that of the gas distributor (4). The material of the exhaust pipe (5) is glass, stainless steel, copper, aluminum, plastic or ceramic. The inner diameter of the intake pipe (1) is 6-8 mm, and the inner diameter of the exhaust pipe (5) is 6-8 mm.
4. The apparatus for improving hydrogen chloride removal efficiency as described in claim 3, characterized in that: The outer diameter of the annular gas distributor (4) is 16-30 mm and the inner diameter is 10-22 mm. The annular gas distributor (4) is vertically connected to the inlet pipe (1). 5-13 distribution holes (6) are provided on the upper and lower surfaces of the gas distributor (4), and the diameter of each distribution hole (6) is 2-3 mm. The three adjacent distribution holes (6) on the upper and lower surfaces of the gas distributor (4) are arranged in a staggered manner.
5. The apparatus for improving hydrogen chloride removal efficiency as described in claim 3, characterized in that: The tree-like gas distributor (4) consists of a central axis pipe and guide vanes. The plane formed by the central axis pipe and guide vanes is parallel to the bottom plane of the alkali bottle (3). The central axis pipe is perpendicularly connected to the inlet pipe (1) and has the same inner and outer diameters. The guide vanes are hollow pipes, and the guide vanes are symmetrically installed on both sides of the central axis pipe, with 6 to 18 guide vanes on each side. The outer edge of the guide vanes on the same side is spaced from the inner wall of the alkali bottle (3) and is arc-shaped with the same shape as the inner wall of the alkali bottle (3). Arrangement; the inner diameter of the guide vane is smaller than the inner diameter of the inlet pipe (1) and the central axis pipe, and the angle between the guide vane and the central axis pipe is 90 degrees; 15 to 20 distribution holes (6) are provided on the upper and lower surfaces of the central axis pipe, and 2 to 10 distribution holes (6) are provided on the upper and lower surfaces of each guide vane, and the diameter of the distribution holes (6) is 2 to 3 mm; any two distribution holes (6) on the upper and lower surfaces of the central axis pipe and the guide vane are not on the same straight line perpendicular to the bottom surface of the alkali bottle (3).