Dibromo-oxime intermediate production system
By designing a continuous production system for the production of dibromophoroxime intermediates, the problem of local excess of bromine and potassium bicarbonate in the prior art is solved, and the production effect of high purity and high yield is achieved.
Patent Information
- Application Number
- CN202421998539.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-08-19
- Publication Date
- 2025-05-27
- Estimated Expiration
- 2034-08-19
AI Technical Summary
In the prior art, when producing dibromophoroxime intermediates, it is necessary to add bromine and potassium bicarbonate aqueous solutions at the same time, resulting in a local excess of bromine and potassium bicarbonate, thereby reducing the purity of the dibromophoroxime intermediate.
A dibromophoric oxime intermediate production system is designed. By setting up a bromine storage tank, a potassium bicarbonate aqueous solution storage tank, a mixer, a tube reactor and a dibromophoric oxime receiving tank, and controlling it through valves and adjusting the feed pump, it ensures that the bromine and potassium bicarbonate aqueous solution are mixed in the mixer and then enter the tube reactor with the oxime-based acetic acid aqueous solution for reaction, achieving continuous production.
The problem of local excess of bromine and potassium bicarbonate is effectively avoided, and the purity and yield of dibromophora intermediates are improved, with the purity increased to 95% and the yield increased to 80%.
Smart Images
Figure CN222901032U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of chemical equipment, in particular to a production system for a dibromooxime intermediate. Background Art
[0002] Pyroxasulfone is an isoxazole herbicide. Pyroxasulfone has a broad market, mainly because pyroxasulfone can effectively control gramineous weeds such as Setaria, Digitaria, and Echinochloa, as well as broad-leaved weeds such as Amaranthus, Datura, Solanum, and Abutilon, and the application crops of pyroxasulfone are relatively extensive, such as crops like corn, cotton, peanut, wheat, sunflower, etc. During the production process of pyroxasulfone, dibromooxime is an important intermediate. Due to the broad market of pyroxasulfone, the market demand for this intermediate, dibromooxime, is also relatively large. Currently, the purity of the produced dibromooxime intermediate is generally 70%. This is mainly because in the prior art, different feeding devices are required to simultaneously drop bromine and an aqueous potassium bicarbonate solution when producing dibromooxime, and there will inevitably be a problem of local excess of bromine and potassium bicarbonate during the dropping process. The local excess of bromine and potassium bicarbonate will result in more impurities in the prepared dibromooxime intermediate, thereby leading to a low purity of the prepared dibromooxime intermediate. For this reason, this application proposes a novel continuous production system for dibromooxime intermediate. Summary of the Invention
[0003] The utility model aims to make up for the deficiencies of the prior art and provides a production system for a dibromooxime intermediate.
[0004] The utility model is realized through the following technical solutions:
[0005] A production system for a dibromooxime intermediate includes a bromine storage tank and an aqueous potassium bicarbonate solution storage tank. The bromine storage tank and the aqueous potassium bicarbonate solution storage tank are respectively fixedly connected to a mixer through pipelines. The mixer and an aqueous oximinoacetic acid solution storage tank are respectively fixedly connected to a tubular reactor through pipelines. The tubular reactor is fixedly connected to a dibromooxime receiving tank through a pipeline; valves I, II, III, IV, and V are respectively fixedly provided on the pipelines connecting the aqueous oximinoacetic acid solution storage tank and the tubular reactor, the pipeline connecting the bromine storage tank and the mixer, the pipeline connecting the aqueous potassium bicarbonate solution storage tank and the mixer, the pipeline connecting the mixer and the tubular reactor, and the pipeline connecting the tubular reactor and the dibromooxime receiving tank; under normal conditions, valves I, II, III, IV, and V are all in a closed state.
[0006] Preferably, the feed port of the mixer connected to the bromine storage tank through a pipeline is lower than the discharge port of the bromine storage tank.
[0007] Preferably, the feed port of the mixer connected to the aqueous potassium bicarbonate solution storage tank through a pipeline is lower than the discharge port of the aqueous potassium bicarbonate solution storage tank.
[0008] Preferably, the feed inlet of the tubular reactor connected to the mixer through a pipeline is lower than the discharge outlet of the mixer.
[0009] Preferably, the feed inlet of the tubular reactor connected to the aqueous solution storage tank of oxime acetic acid is lower than the discharge outlet of the aqueous solution storage tank of oxime acetic acid.
[0010] Preferably, the discharge outlet of the tubular reactor is higher than the feed inlet of the dibromooxime receiving tank.
[0011] Preferably, a bromine feed pump is fixedly connected to the pipeline connecting the bromine storage tank and the mixer; a potassium bicarbonate feed pump is fixedly connected to the pipeline connecting the potassium bicarbonate aqueous solution storage tank and the mixer; an oxime acetic acid feed pump is fixedly connected to the pipeline connecting the aqueous solution storage tank of oxime acetic acid and the tubular reactor.
[0012] Preferably, the dibromooxime receiving tank is fixedly connected with a venting device. In this application, the venting device is used to treat the volatile gas volatilized from the dibromooxime receiving tank.
[0013] Preferably, the venting device includes a falling film absorber, a falling film absorption tank and a tail gas absorption tower; wherein, the upper end surface of the dibromooxime receiving tank is fixedly connected to the falling film absorber through a pipeline, and the lower part of the side surface of the falling film absorber is fixedly connected to the tail gas absorption tower through a pipeline.
[0014] Compared with the prior art, the beneficial technical effects of this application are:
[0015] The dibromooxime intermediate production system described in this application does not require the simultaneous dropping of bromine and aqueous potassium bicarbonate solution. Therefore, it can effectively avoid the problem of low purity of dibromooxime intermediate caused by local excess of bromine and potassium bicarbonate due to the dropping of bromine and aqueous potassium bicarbonate solution. The dibromooxime intermediate production system described in this application can realize the continuous production of dibromooxime intermediate. Specifically, through the setting of the connection relationship and position relationship of the aqueous glyoxylic acid solution storage tank, bromine storage tank, aqueous potassium bicarbonate solution storage tank, mixer, tubular reactor, dibromooxime receiving tank, aqueous glyoxylic acid feed pump, bromine feed pump, and aqueous potassium bicarbonate feed pump, etc., this application can control the feeding speeds of the aqueous glyoxylic acid solution, bromine, and aqueous potassium bicarbonate solution, and make them reach the point where bromine and aqueous potassium bicarbonate solution can be simultaneously input into the mixer for mixing, and the mixed material after mixing can enter the tubular reactor simultaneously with the aqueous glyoxylic acid solution for reaction to synthesize dibromooxime intermediate. Obviously, this application realizes the purpose of continuous production of dibromooxime intermediate by regulating the feeding speeds of the aqueous glyoxylic acid solution, bromine, and aqueous potassium bicarbonate solution. Moreover, the yield and purity of the dibromooxime intermediate prepared by the dibromooxime intermediate production system described in this application have been improved compared with the dibromooxime intermediate produced in the prior art (the purity of dibromooxime produced in the prior art is generally 80% and the yield is generally 70%). Specifically, the yield of the dibromooxime intermediate prepared by the dibromooxime intermediate production system described in this application is as high as 80% and the purity is as high as 95%. BRIEF DESCRIPTION OF THE DRAWINGS
[0016] Figure 1 is a schematic diagram of a dibromooxime intermediate production system of this application;
[0017] In the figure: 1, aqueous glyoxylic acid solution storage tank; 2, bromine storage tank; 3, aqueous potassium bicarbonate solution storage tank; 4, mixer; 5, tubular reactor; 6, dibromooxime receiving tank; 7, aqueous glyoxylic acid feed pump; 8, bromine feed pump; 9, aqueous potassium bicarbonate feed pump; 10, valve I; 11, valve II; 12, valve III; 13, valve IV; 14, valve V; 15, falling film absorber; 16, falling film absorption tank; 17, tail gas absorption tower. DETAILED DESCRIPTION OF THE EMBODIMENTS
[0018] As Figure 1 shown, a dibromooxime intermediate production system includes a bromine storage tank 2 and an aqueous potassium bicarbonate solution storage tank 3, and both the bromine storage tank 2 and the aqueous potassium bicarbonate solution storage tank 3 are provided with feed inlets;
[0019] The discharge port of the bromine storage tank 2 is fixedly connected to an inlet of the mixer 4 through a pipeline. The above-mentioned inlet of the mixer 4 is lower than the discharge port of the bromine storage tank 2. A valve II 11 is also fixedly installed on the pipeline connecting the discharge port of the bromine storage tank 2 and the above-mentioned inlet of the mixer 4;
[0020] The discharge port of the potassium bicarbonate aqueous solution storage tank 3 is fixedly connected to another inlet of the mixer 4 through a pipeline. The above-mentioned another inlet of the mixer 4 is lower than the discharge port of the potassium bicarbonate aqueous solution storage tank 3. A valve III 12 is also fixedly installed on the pipeline connecting the discharge port of the potassium bicarbonate aqueous solution storage tank 3 and the above-mentioned another inlet of the mixer 4;
[0021] The discharge port of the mixer 4 and the discharge port of the oximinoacetic acid aqueous solution storage tank 1 are respectively fixedly connected to two inlets of the tubular reactor 5 through pipelines. Among them, a valve I 10 is also fixedly connected to the pipeline connecting the discharge port of the oximinoacetic acid aqueous solution storage tank 1 and one of the inlets of the tubular reactor 5. A valve IV 13 is also fixedly connected to the pipeline connecting the discharge port of the mixer 4 and one of the inlets of the tubular reactor 5; In this application, the oximinoacetic acid aqueous solution storage tank 1 is also provided with an inlet. Moreover, the inlet of the tubular reactor 5 connected to the mixer 4 through the pipeline is lower than the discharge port of the mixer 4, and the inlet of the tubular reactor 5 connected to the oximinoacetic acid aqueous solution storage tank 1 through the pipeline is lower than the discharge port of the oximinoacetic acid aqueous solution storage tank 1;
[0022] The discharge port of the tubular reactor 5 is fixedly connected to the inlet of the dibromooxime receiving tank 6 through a pipeline. A valve V 14 is also fixedly connected to the pipeline connecting the discharge port of the tubular reactor 5 and the inlet of the dibromooxime receiving tank 6. The discharge port of the tubular reactor 5 is higher than the inlet of the dibromooxime receiving tank 6;
[0023] In this application, under normal conditions, the valve I 10, the valve II 11, the valve III 12, the valve IV 13 and the valve V 14 are all in a closed state; Moreover, in this embodiment, the inner diameter sizes of all pipelines are the same.
[0024] In addition, a bromine feed pump 8 is also fixedly connected to the pipeline connecting the bromine storage tank 2 and the mixer 4 in this application. A potassium bicarbonate feed pump 9 is also fixedly connected to the pipeline connecting the potassium bicarbonate aqueous solution storage tank 3 and the mixer 4. An oximinoacetic acid feed pump 7 is also fixedly connected to the pipeline connecting the oximinoacetic acid aqueous solution storage tank 1 and the tubular reactor 5; Among them, the valve I 10 is located between the oximinoacetic acid aqueous solution storage tank and the oximinoacetic acid feed pump 7, the valve II 11 is located between the bromine storage tank 2 and the bromine feed pump 8, and the valve III 12 is located between the potassium bicarbonate aqueous solution storage tank 3 and the potassium bicarbonate feed pump 9.
[0025] In addition, a venting device is fixedly connected to the dibromooxime receiving tank in this application. The venting device includes a falling film absorber 15, a falling film absorption tank 16, and a tail gas absorption tower 17. The upper end surface of the dibromooxime receiving tank 6 is fixedly connected to the falling film absorber 15 through a pipeline, and the lower part of the side surface of the falling film absorber 15 is fixedly connected to the tail gas absorption tower 17 through a pipeline.
[0026] The working principle of the dibromooxime intermediate production system in this application is as follows: Add 3560 kg of an aqueous solution of oximinoacetic acid with a mass percentage of 10% into the oximinoacetic acid aqueous solution storage tank 1, add 1000 kg of bromine into the bromine storage tank 2, and add 8760 kg of an aqueous solution of potassium bicarbonate with a mass percentage of 10% into the potassium bicarbonate aqueous solution storage tank 3. Then, open valves Ⅰ 10, valves Ⅱ 11, valves Ⅲ 12, valves Ⅳ 13, and valves Ⅴ 14, and start the oximinoacetic acid feed pump 7, the bromine feed pump 8, and the potassium bicarbonate feed pump 9. Bromine and the aqueous solution of potassium bicarbonate are simultaneously pumped into the mixer 4 for mixing to obtain a mixed material liquid. Among them, the mixing process of bromine and the aqueous solution of potassium bicarbonate is completed from entering the mixer 4 to leaving the mixer 4, and valve Ⅳ 13 is not closed during this process. The mixed material liquid and the aqueous solution of oximinoacetic acid are simultaneously transported to the tubular reactor 5, and the reaction is completed from entering the tubular reactor 5 to flowing out of the tubular reactor 5 to obtain the dibromooxime intermediate. Among them, the time for the mixed material liquid and the aqueous solution of oximinoacetic acid to flow into the tubular reactor 5 to flow out of the tubular reactor 5 is 1 min, and the reaction temperature set in the tubular reactor 5 is 20 - 25 °C. The generated dibromooxime intermediate will flow into the dibromooxime receiving tank 6 through a pipeline for storage. In this embodiment, the inner diameter sizes of all pipelines are the same. After starting the oximinoacetic acid feed pump 7, the bromine feed pump 8, and the potassium bicarbonate feed pump 9, the flow rate of the aqueous solution of oximinoacetic acid in the pipeline: the flow rate of bromine: the flow rate of the aqueous solution of potassium bicarbonate: the flow rate of the mixed material liquid = 1:0.28:2.46:2.74.
[0027] The volatile gas 17 volatilized from the dibromooxime receiving tank 6 in this embodiment will enter the falling film absorber 15. Under the condensation effect of the falling film absorber 15, the high-boiling substances in the volatile gas will condense into a liquid phase and enter the falling film absorption tank 16 under the action of gravity. The low-boiling substances in the volatile gas that are not condensed into a liquid phase and still remain in the gas phase will enter the tail gas absorption tower 17 for tail gas treatment. Therefore, the dibromooxime intermediate production system described in this application also has better environmental protection effects. Tests on the dibromooxime intermediate prepared by using the dibromooxime intermediate production system in this application show that the purity of the dibromooxime intermediate is as high as 95%, and the yield of the dibromooxime intermediate is as high as 80%.
Claims
1. A dibromooxime intermediate production system, characterized in that: The invention comprises a bromine storage tank and a potassium bicarbonate aqueous solution storage tank, wherein the bromine storage tank and the potassium bicarbonate aqueous solution storage tank are fixedly connected to a mixer through pipelines, the mixer and the oxime acetic acid aqueous solution storage tank are fixedly connected to a tubular reactor through pipelines, and the tubular reactor is fixedly connected to a dibromooxime receiving tank through pipelines; valves I, II, III, IV and V are fixedly arranged on the pipeline connecting the oxime acetic acid aqueous solution storage tank and the tubular reactor, the pipeline connecting the bromine storage tank and the mixer, the pipeline connecting the potassium bicarbonate aqueous solution storage tank and the mixer, the pipeline connecting the mixer and the tubular reactor, and the pipeline connecting the tubular reactor and the dibromooxime receiving tank; under normal conditions, valves I, II, III, IV and V are all in a closed state.
2. A dibromooxime intermediate production system according to claim 1, characterized in that: The feed inlet of the mixer connected to the bromine storage tank through a pipeline is lower than the discharge outlet of the bromine storage tank.
3. A dibromooxime intermediate production system according to claim 1, characterized in that: The feed inlet of the mixer connected to the potassium bicarbonate aqueous solution storage tank through a pipeline is lower than the discharge port of the potassium bicarbonate aqueous solution storage tank.
4. A dibromooxime intermediate production system according to claim 1, characterized in that: The feed inlet of the tubular reactor to which the mixer is connected by a pipeline is lower than the discharge outlet of the mixer.
5. A dibromooxime intermediate production system according to claim 1, characterized in that: The feed inlet of the tubular reactor connected to the oximinoacetic acid aqueous solution storage tank through a pipeline is lower than the discharge outlet of the oximinoacetic acid aqueous solution storage tank.
6. A dibromooxime intermediate production system according to claim 1, characterized in that: The discharge port of the tubular reactor is higher than the feed port of the dibromooxime receiving tank.
7. A dibromooxime intermediate production system according to claim 1, characterized in that: A bromine feed pump is fixedly connected to the pipeline connecting the bromine storage tank and the mixer; a potassium bicarbonate feed pump is fixedly connected to the pipeline connecting the potassium bicarbonate aqueous solution storage tank and the mixer; and a oxime acetic acid feed pump is fixedly connected to the pipeline connecting the oxime acetic acid aqueous solution storage tank and the tubular reactor.
8. A dibromooxime intermediate production system according to claim 1, characterized in that: The dibromooxime receiving tank is fixedly connected with a venting device.
9. A dibromooxime intermediate production system according to claim 8, characterized in that: The venting device comprises a falling film absorber, a falling film absorption tank and a tail gas absorption tower; wherein the upper end surface of the dibromooxime receiving tank is fixedly connected to the falling film absorber through a pipeline, and the lower side of the falling film absorber is fixedly connected to the tail gas absorption tower through a pipeline.