A method for solidifying 2-chloro-5-chloromethylthiazole kettle residue
By cooling the reactor and adding a hydroxyl compound to solidify the 2-chloro-5-chloromethylthiazole reactor residue, the problem of reactor residue treatment is solved, swelling is prevented, and environmental pollution is reduced.
Patent Information
- Application Number
- CN202311831152.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-12-28
- Publication Date
- 2026-02-10
- Estimated Expiration
- 2043-12-28
AI Technical Summary
In existing technologies, 2-chloro-5-chloromethylthiazole residues are difficult to handle, and they tend to expand at room temperature, increasing floor space requirements and polluting the environment.
The 2-chloro-5-chloromethylthiazole residue remaining after distillation is placed in a reaction vessel, the temperature is lowered and a hydroxyl compound such as methanol, ethanol or formic acid is added, and the reaction is allowed to stand until it solidifies, and then it is taken out and stored.
It effectively prevents the expansion of reactor residue, reduces environmental pollution, and achieves solidification of reactor residue.
Smart Images
Figure CN117815613B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of 2-chloro-5-chloromethylthiazole technology, specifically relating to a method for solidifying 2-chloro-5-chloromethylthiazole residue in an autoclave. Background Technology
[0002] 2-Chloro-5-chloromethylthiazole is an important intermediate in the synthesis of pesticides such as thiamethoxam, thiamethoxam, and dinotefuran. Currently, thiamethoxam, as a second-generation neonicotinoid insecticide, is highly effective and low-toxicity, exhibiting stomach poison, contact, and systemic activity against pests. It effectively inhibits and blocks the central nervous system of insects, ultimately paralyzing and killing them. In the production of thiamethoxam, 2-chloro-5-chloromethylthiazole is distilled with other solvents in a distillation apparatus. However, the distillation apparatus retains 2-chloro-5-chloromethylthiazole residue, which is difficult to handle and swells at room temperature, increasing the footprint and polluting the environment. Summary of the Invention
[0003] This invention provides a method for curing 2-chloro-5-chloromethylthiazole residue in an autoclave, in order to solve the technical problem that 2-chloro-5-chloromethylthiazole residue is difficult to handle in the prior art.
[0004] To achieve the above objectives, the technical solution adopted by the present invention is: to provide a method for the curing of 2-chloro-5-chloromethylthiazole residue in an autoclave, comprising:
[0005] S1: Place the 2-chloro-5-chloromethylthiazole residue from the distillation apparatus into the reaction vessel, and lower the temperature of the 2-chloro-5-chloromethylthiazole residue;
[0006] S2: Maintain the reactor temperature and add hydroxyl compounds to the reactor;
[0007] S3: Let stand and wait for the hydroxyl compound to react with the 2-chloro-5-chloromethylthiazole residue in the reactor and gradually solidify;
[0008] S4: Remove the completely solidified 2-chloro-5-chloromethylthiazole residue from the reactor and store it.
[0009] In one possible implementation, the residual temperature of the 2-chloro-5-chloromethylthiazole reactor in step S1 is reduced to 80°C-90°C.
[0010] In one possible implementation, the temperature inside the reactor is maintained at no less than 70°C in step S2.
[0011] In one possible implementation, the amount of the added hydroxyl compound is 3%-10% of the residue content of the 2-chloro-5-chloromethylthiazole.
[0012] In one possible implementation, the 2-chloro-5-chloromethylthiazole residue and the hydroxyl compound are continuously stirred during the addition of the hydroxyl compound.
[0013] In one possible implementation, the hydroxyl compound is added to the reaction vessel at a constant rate over a period of 30-40 minutes.
[0014] In one possible implementation, the resting and waiting time in step S3 is 50-70 minutes.
[0015] In one possible implementation, the hydroxyl compound is methanol, ethanol, or formic acid.
[0016] In one possible implementation, in step S4, the temperature of the 2-chloro-5-chloromethylthiazole residue is reduced to below 50°C, and the solidified 2-chloro-5-chloromethylthiazole residue is removed, crushed, and bagged.
[0017] In one possible implementation, the reactor is equipped with a screw conveyor for removing the solidified 2-chloro-5-chloromethylthiazole reactor residue.
[0018] The beneficial effects of the method for solidifying 2-chloro-5-chloromethylthiazole residue provided by this invention are as follows: Compared with the prior art, the method for solidifying 2-chloro-5-chloromethylthiazole residue of this invention involves first transferring the 2-chloro-5-chloromethylthiazole residue formed in the distillation apparatus after distillation of 2-chloro-5-chloromethylthiazole and other solvents to a reaction vessel; secondly, lowering the temperature of the 2-chloro-5-chloromethylthiazole residue while maintaining the temperature of the reaction vessel; and then adding hydroxylating agents to the reaction vessel. The 2-chloro-5-chloromethylthiazole residue is left to stand and allow the hydroxyl compound to react with the residue, gradually solidifying it. Finally, the completely solidified residue is removed and stored. This method lowers the temperature of the 2-chloro-5-chloromethylthiazole residue and allows the addition of the hydroxyl compound to react with it, solidifying the residue and effectively preventing its expansion, which could lead to environmental pollution. Attached Figure Description
[0019] To more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0020] Figure 1 The flowchart for the solidification of 2-chloro-5-chloromethylthiazole residue provided in the embodiments of the present invention is shown. Detailed Implementation
[0021] To make the technical problems, solutions, and beneficial effects of this invention clearer, the invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the invention.
[0022] It should be noted that when a component is referred to as being "fixed to" or "set on" another component, it can be directly on or indirectly on that other component. When a component is referred to as being "connected to" another component, it can be directly connected to or indirectly connected to that other component.
[0023] It should be understood that the terms "length", "width", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on the present invention.
[0024] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of this invention, "a plurality of" means two or more, unless otherwise explicitly specified.
[0025] Please see Figure 1 The method for solidifying 2-chloro-5-chloromethylthiazole residue in an autoclave, provided by the present invention, will now be described. A method for solidifying 2-chloro-5-chloromethylthiazole residue in an autoclave includes:
[0026] S1, place the 2-chloro-5-chloromethylthiazole residue from the distillation apparatus into the reaction vessel, and lower the temperature of the 2-chloro-5-chloromethylthiazole residue;
[0027] S2, maintain the reactor temperature and add hydroxyl compound to the reactor;
[0028] S3, let stand and wait for the hydroxyl compound to react with the 2-chloro-5-chloromethylthiazole residue in the reactor and gradually solidify;
[0029] S4, the completely solidified 2-chloro-5-chloromethylthiazole residue is removed from the reactor and stored.
[0030] The method for solidifying 2-chloro-5-chloromethylthiazole residue provided in this embodiment differs from existing technologies. In this method, the 2-chloro-5-chloromethylthiazole residue, formed after distillation of 2-chloro-5-chloromethylthiazole and other solvents in the distillation apparatus, is first transferred to a reaction vessel. Next, the temperature of the residue is lowered while maintaining the temperature of the reaction vessel. Then, a hydroxyl compound is added to the reaction vessel, and the mixture is allowed to stand and react with the residue to gradually solidify. Finally, the completely solidified residue is removed and stored. This method effectively prevents the residue from swelling and causing environmental pollution by lowering its temperature and adding a hydroxyl compound to react with it.
[0031] Please see Figure 1 As a specific embodiment of the method for solidifying 2-chloro-5-chloromethylthiazole residue provided by the present invention, in step S1, the temperature of the 2-chloro-5-chloromethylthiazole residue is reduced to 80℃-90℃. Since the temperature is 90℃-110℃ and the pressure is 2000Pa when distilling 2-chloro-5-chloromethylthiazole and other solvents in the distillation apparatus, after transferring the 2-chloro-5-chloromethylthiazole residue to the reaction vessel, it is necessary to reduce the temperature of the 2-chloro-5-chloromethylthiazole residue to 80℃-90℃ so that the 2-chloro-5-chloromethylthiazole residue can react with the hydroxyl compound.
[0032] Please see Figure 1 As a specific embodiment of the method for solidifying 2-chloro-5-chloromethylthiazole reactor residue provided by the present invention, the reactor temperature is maintained at no less than 70°C in step S2; during the reaction between the hydroxyl compound and the 2-chloro-5-chloromethylthiazole reactor residue, in order to ensure the normal progress of the reaction, it is necessary to maintain the reactor temperature at no less than 70°C.
[0033] Please see Figure 1In one specific embodiment of the method for solidifying 2-chloro-5-chloromethylthiazole reactor residue provided by the present invention, the content of the added hydroxyl compound is 3%-10% of the 2-chloro-5-chloromethylthiazole reactor residue; the content of the added hydroxyl compound is 3%-10% of the content of the 2-chloro-5-chloromethylthiazole reactor residue in the reactor, so as to ensure that the hydroxyl compound can fully react with the 2-chloro-5-chloromethylthiazole reactor residue, thereby making all the 2-chloro-5-chloromethylthiazole reactor residue solid.
[0034] Please see Figure 1 As a specific embodiment of the method for solidifying 2-chloro-5-chloromethylthiazole reactor residue provided by the present invention, the 2-chloro-5-chloromethylthiazole reactor residue and the hydroxyl compound are continuously stirred during the addition of the hydroxyl compound; during the addition of the hydroxyl compound to the reactor, the hydroxyl compound and the 2-chloro-5-chloromethylthiazole reactor residue are continuously stirred so that the hydroxyl compound and the 2-chloro-5-chloromethylthiazole reactor residue can fully contact and react.
[0035] Please see Figure 1 As a specific embodiment of the method for solidifying 2-chloro-5-chloromethylthiazole reactor residue provided by the present invention, the hydroxyl compound is added to the reactor at a uniform rate for 30-40 minutes. The hydroxyl compound is added within 30-40 minutes to prevent the reaction between the hydroxyl compound and the 2-chloro-5-chloromethylthiazole reactor residue from being too rapid, which would make it impossible to stir the 2-chloro-5-chloromethylthiazole reactor residue and the hydroxyl compound.
[0036] Please see Figure 1 In one specific embodiment of the method for solidifying 2-chloro-5-chloromethylthiazole reactor residue provided by the present invention, the time for standing and waiting in step S3 is 50-70 minutes; after adding the hydroxyl compound, stand and wait for 50-70 minutes, while maintaining the temperature inside the reactor at no less than 70°C during this period, so as to ensure that the hydroxyl compound reacts with the 2-chloro-5-chloromethylthiazole reactor residue to form a solid 2-chloro-5-chloromethylthiazole reactor residue.
[0037] Please see Figure 1 In one specific embodiment of the method for solidifying 2-chloro-5-chloromethylthiazole reactor residue provided by the present invention, the hydroxyl compound is methanol, ethanol, or formic acid; when methanol is used, the content of methanol added to the reactor is 5% of the content of 2-chloro-5-chloromethylthiazole reactor residue; when ethanol is used, the content of ethanol added is 10% of the content of 2-chloro-5-chloromethylthiazole reactor residue; when formic acid is used, the content of formic acid added is 10% of the content of 2-chloro-5-chloromethylthiazole reactor residue.
[0038] Please see Figure 1In a specific embodiment of the method for solidifying 2-chloro-5-chloromethylthiazole reactor residue provided by the present invention, in step S4, the temperature of the 2-chloro-5-chloromethylthiazole reactor residue is reduced to below 50°C, and the solidified 2-chloro-5-chloromethylthiazole reactor residue is crushed and bagged; after the hydroxyl compound reacts with the 2-chloro-5-chloromethylthiazole reactor residue, the temperature of the 2-chloro-5-chloromethylthiazole reactor residue is reduced to below 50°C so that workers can easily remove the solidified 2-chloro-5-chloromethylthiazole reactor residue; at the same time, the solidified 2-chloro-5-chloromethylthiazole reactor residue is crushed and bagged, thereby reducing environmental pollution.
[0039] Not shown in the figure, as a specific embodiment of the method for solidifying 2-chloro-5-chloromethylthiazole reactor residue provided by the present invention, a screw conveyor is provided in the reactor for removing the solidified 2-chloro-5-chloromethylthiazole reactor residue; the screw conveyor is provided in the reactor to facilitate the removal of the solidified 2-chloro-5-chloromethylthiazole reactor residue.
[0040] The above are merely preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention should be included within the protection scope of the present invention.
Claims
1. A method for solidifying 2-chloro-5-chloromethylthiazole residue in an autoclave, characterized in that, include: S1: Place the 2-chloro-5-chloromethylthiazole residue from the distillation apparatus into the reaction vessel, and lower the temperature of the 2-chloro-5-chloromethylthiazole residue; the temperature of the 2-chloro-5-chloromethylthiazole residue is lowered to 80℃-90℃; S2: Maintain the temperature of the reactor and add a hydroxyl compound to the reactor; maintain the temperature inside the reactor at no less than 70°C; the hydroxyl compound is methanol, ethanol, or formic acid; S3: Let stand and wait for the hydroxyl compound to react with the 2-chloro-5-chloromethylthiazole residue in the reactor and gradually solidify; S4: Remove the completely solidified 2-chloro-5-chloromethylthiazole residue from the reactor and store it; reduce the temperature of the 2-chloro-5-chloromethylthiazole residue to below 50°C.
2. The method for solidifying 2-chloro-5-chloromethylthiazole residue as described in claim 1, characterized in that, The content of the added hydroxyl compound is 3%-10% of the residue content of the 2-chloro-5-chloromethylthiazole in the reactor.
3. The method for solidifying 2-chloro-5-chloromethylthiazole residue as described in claim 2, characterized in that, During the addition of the hydroxyl compound, the 2-chloro-5-chloromethylthiazole residue and the hydroxyl compound are continuously stirred.
4. The method for solidifying 2-chloro-5-chloromethylthiazole residue as described in claim 3, characterized in that, The hydroxyl compound is added to the reaction vessel at a constant rate over a period of 30-40 minutes.
5. The method for solidifying 2-chloro-5-chloromethylthiazole residue as described in claim 1, characterized in that, In step S3, the time for resting and waiting is 50-70 minutes.
6. The method for solidifying 2-chloro-5-chloromethylthiazole residue as described in claim 1, characterized in that, In step S4, the solidified 2-chloro-5-chloromethylthiazole residue is removed from the reactor, crushed, and bagged.
7. The method for solidifying 2-chloro-5-chloromethylthiazole residue as described in claim 6, characterized in that, The reactor is equipped with a screw conveyor for removing the solidified 2-chloro-5-chloromethylthiazole reactor residue.
Citation Information
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