Allyloxyamine sulfate production system
By optimizing the allyloxyamine sulfate production system, the problems of long production cycle and safety risks were solved, and efficient and safe allyloxyamine sulfate production was achieved. The product yield and purity reached high standards and were suitable for industrial application.
Patent Information
- Application Number
- CN202422139117.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-02
- Publication Date
- 2025-10-03
- Estimated Expiration
- 2034-09-02
AI Technical Summary
The existing allyloxyamine sulfate production process has a long production cycle and safety risks, especially the distillation operation of dichloromethane, which poses safety hazards.
A production system was designed, including a sulfuric acid high-level tank, a hydrolysis kettle, a centrifuge, a condenser, and a dryer. By optimizing the process and equipment connections, the hydrolysis, centrifugation, and drying of sulfuric acid and allylamide were achieved, dichloromethane extraction was avoided, and gravity and condenser reflux were used to shorten the production cycle and improve safety.
The production cycle is shortened by 61%, the use of dichloromethane is avoided, and the safety risk is reduced. The product yield is 90% and the purity is 98%, which is suitable for industrial production.
Smart Images
Figure CN223404892U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of chemical equipment, in particular to an allyloxyamine sulfate production system. Background Art
[0002] Clethodim is a new post-emergence herbicide for dryland fields used to control grass weeds such as barnyard grass, wild oats, crabgrass, foxtail grass, goosegrass, foxtail grass, bluegrass, and hard grass. It is suitable for broad-leaved fields such as soybeans, rapeseed, cotton, and peanuts, and has a broad market. In the production of clethodim, allyloxyamine sulfate is an important raw material and has a large market demand. Currently, in the existing technology, the synthesis of allyloxyamine sulfate generally involves adding hydrochloric acid to allylamide to hydrolyze it into a salt, then neutralizing it with liquid caustic soda, extracting it with dichloromethane, and then evaporating the dichloromethane to obtain the allyloxyamine sulfate product. This production method not only has a long production cycle (typically 18 hours), but also poses certain safety risks during the distillation of dichloromethane. Therefore, this application proposes an allyloxyamine sulfate production system with a short production cycle and high production safety. Utility Model Content
[0003] In order to make up for the deficiencies of the prior art, the utility model provides an allyloxyamine sulfate production system.
[0004] The utility model is achieved through the following technical solutions:
[0005] An allyloxyamine sulfate production system comprises a sulfuric acid header tank, a hydrolysis kettle, and a centrifuge, which are fixedly connected in sequence via pipelines. Valves are fixedly provided on the pipelines connecting the sulfuric acid header tank and the hydrolysis kettle, as well as on the pipelines connecting the hydrolysis kettle and the centrifuge. The hydrolysis kettle is also fixedly connected to a condenser I via an air inlet pipe and a reflux pipe, respectively. One discharge port of the centrifuge is fixedly connected to a dryer via a spiral feeder. The lower ends of the sulfuric acid header tank and the condenser I are both higher than the upper end of the hydrolysis kettle, and the lower end of the hydrolysis kettle is higher than the upper end of the centrifuge.
[0006] Preferably, the discharge port of the dryer is fixedly connected to the bagging machine through a pipeline.
[0007] Preferably, the lower end of the dryer is higher than the upper end of the bagging machine.
[0008] Preferably, another discharge port of the centrifuge is fixedly connected to a centrifuge mother liquor receiving tank via a pipeline, and the upper end of the centrifuge mother liquor receiving tank is lower than the lower end of the centrifuge.
[0009] Preferably, the upper end of the dryer is also fixedly connected to the condenser II through a pipeline, and the lower end of the condenser II is fixedly connected to the methanol receiving tank through a pipeline; the upper end of the methanol receiving tank is lower than the lower end of the condenser II.
[0010] Compared with the prior art, the beneficial technical effects of this application are:
[0011] The allyloxyamine sulfate production system described in the present application has a production cycle of 7 hours for producing allyloxyamine sulfate products, which is 61% lower than the production cycle of allyloxyamine sulfate products in the prior art (generally 18 hours). Moreover, the allyloxyamine sulfate production system described in the present application does not require dichloromethane extraction when producing the allyloxyamine sulfate product, so there is naturally no need to evaporate dichloromethane, thereby effectively avoiding the safety risks caused by evaporating dichloromethane in the prior art. Therefore, the present application has higher production safety. Therefore, the allyloxyamine sulfate production system described in the present application is very suitable for industrial production. BRIEF DESCRIPTION OF THE DRAWINGS
[0012] Figure 1 This is a schematic diagram of the allyloxyamine sulfate production system of the present application;
[0013] In the figure: sulfuric acid high-level tank 1, condenser I 2, hydrolysis kettle 3, centrifuge 4, dryer 5, bagging machine 6, manual valve 7, screw feeder 8, centrifuge mother liquor receiving tank 9, condenser II 10, methanol receiving tank 11. DETAILED DESCRIPTION
[0014] like Figure 1 As shown, an allyloxyamine sulfate production system includes a sulfuric acid high-level tank 1, a hydrolysis kettle 3 and a centrifuge 4 fixedly connected in sequence by pipelines. Manual valves 7 are fixedly provided on the pipelines connecting the sulfuric acid high-level tank 1 and the hydrolysis kettle 3 and on the pipelines connecting the hydrolysis kettle 3 and the centrifuge 4. The hydrolysis kettle 3 is also fixedly connected to the condenser I 2 through an air inlet pipe and a reflux pipe respectively. One discharge port of the centrifuge 4 is fixedly connected to the dryer 5 through a screw feeder 8. The discharge port of the dryer 5 is fixedly connected to the bagging machine 6 through a pipeline. The other discharge port of the centrifuge 4 is fixedly connected to the centrifuge nut through a pipeline. liquid receiving tank 9; the upper end of the dryer 5 is also fixedly connected to the condenser II 10 through a pipe, and the lower end of the condenser II 10 is also fixedly connected to the methanol receiving tank 11 through a pipe, and the dryer 5, condenser II 10 and methanol receiving tank 11 are connected; in the present application, the lower ends of the sulfuric acid high-level tank 1 and the condenser I 2 are higher than the upper end of the hydrolysis kettle 3, the lower end of the hydrolysis kettle 3 is higher than the upper end of the centrifuge 4, the lower end of the centrifuge 4 is higher than the upper end of the centrifuge mother liquor receiving tank 9, the lower end of the dryer 5 is higher than the upper end of the bagging machine 6, and the lower end of the condenser II 10 is higher than the upper end of the methanol receiving tank 11.
[0015] The working principle of the present application is as follows: 487kg of sulfuric acid is added to the sulfuric acid high-level tank 1 through the feeding port of the high-level tank 1, 725kg of methanol and 725kg of allylamide are respectively added to the hydrolysis kettle 3 through the two feeding ports of the hydrolysis kettle 3, and then, the stirring device provided in the hydrolysis kettle 3 is controlled to stir, and then the manual valve 7 provided on the pipeline between the sulfuric acid high-level tank 1 and the hydrolysis kettle 3 is opened, so that the sulfuric acid in the sulfuric acid high-level tank 1 is added dropwise to the hydrolysis kettle 3 under the condition that methanol and allylamide are stirred and mixed, after the sulfuric acid is added dropwise, the temperature in the hydrolysis kettle 3 is raised to 60°C, and the reflux reaction is carried out for 2 hours. During the reflux reaction, the methanol vapor is condensed through the condenser Ⅰ2, and the condensed methanol liquid is refluxed into the hydrolysis kettle 3 under the action of gravity. After the reflux reaction is carried out for 2 hours, the reaction is terminated, and then the material in the hydrolysis kettle 3 is cooled to 5 ℃, and then open the manual valve 7 provided on the pipeline between the hydrolysis kettle 3 and the centrifuge 4, and the material in the hydrolysis kettle 3 flows into the centrifuge 4 under the action of gravity for centrifugation to obtain a centrifuge mother liquor and an allyloxyamine sulfate wet product, wherein the allyloxyamine sulfate wet product enters the screw feeder 8 through one discharge port of the centrifuge 4, and the centrifuge mother liquor enters the centrifuge mother liquor receiving tank 9 through another discharge port of the centrifuge 4, and then, the screw feeder 8 is started, and the allyloxyamine sulfate wet product is transported to the dryer 5 under the action of the screw feeder 8 for drying to obtain an allyloxyamine sulfate product, and the methanol vapor generated during the drying process is condensed through the condenser II 10, and the methanol liquid formed after condensation flows into the methanol receiving tank 11 for recovery under the action of gravity, and the allyloxyamine sulfate product in the dryer 5 enters the bagging machine 6 for bagging under the action of gravity. Through testing, it can be seen that the yield of the allyloxyamine sulfate product prepared by the allyloxyamine sulfate production system described in the present application is 90% and the purity is 98%.
Claims
1. An allyloxyamine sulfate production system, characterized in that: The invention comprises a high-level sulfuric acid tank, a hydrolysis kettle and a centrifuge which are fixedly connected in sequence through pipelines. Valves are fixedly provided on the pipelines connecting the high-level sulfuric acid tank and the hydrolysis kettle, as well as on the pipelines connecting the hydrolysis kettle and the centrifuge. The hydrolysis kettle is also fixedly connected to a condenser I through an air inlet pipe and a reflux pipe respectively. The discharge port of the centrifuge is fixedly connected to a dryer through a spiral feeder. The lower ends of the high-level sulfuric acid tank and the condenser I are both higher than the upper end of the hydrolysis kettle, and the lower end of the hydrolysis kettle is higher than the upper end of the centrifuge.
2. The allyloxyamine sulfate production system according to claim 1, wherein: The discharge port of the drying machine is fixedly connected to the bagging machine through a pipeline.
3. The allyloxyamine sulfate production system according to claim 2, wherein: The lower end of the drying machine is higher than the upper end of the bagging machine.
4. The allyloxyamine sulfate production system according to claim 1, wherein: Another discharge port of the centrifuge is fixedly connected to a centrifuge mother liquor receiving tank through a pipeline, and the upper end of the centrifuge mother liquor receiving tank is lower than the lower end of the centrifuge.
5. The allyloxyamine sulfate production system according to claim 1, wherein: The upper end of the dryer is also fixedly connected to the condenser II through a pipeline, and the lower end of the condenser II is fixedly connected to the methanol receiving tank through a pipeline; the upper end of the methanol receiving tank is lower than the lower end of the condenser II.