A production system of quinoclamine
Patent Information
- Application Number
- CN202522458583.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-20
- Publication Date
- 2026-10-20
- Estimated Expiration
- 2035-11-20
AI Technical Summary
目前，现有技术中，合成喹草酮反应步数多、反应周期长，通常需要先将甲基物和氰化亚铜进行氰化反应，再硫酸水解成酸，最后通过氯化亚砜进行酰化、1,3-环己二酮酯化、丙酮氰醇转位反应得到喹草酮产品，现有的合成喹草酮的生产装置存在反应设备多、生产周期长的问题；而现有技术中尚缺乏
[0008]与现有技术相比，本实用新型的优点和积极效果在于：
Smart Images
Figure CN224865385U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to a production system for quinacrine, belonging to the field of chemical equipment technology. Background Technology
[0002] Quinalazine is a p-hydroxyphenylpyruvate dioxygenase (HPPD) inhibitor (triketone). It works by inhibiting the activity of key pigment enzymes controlling photosynthesis in plants, thus hindering the conversion of substrates into hydantoin. This prevents the normal synthesis of tocopherols and plastoquinones, affecting carotenoid synthesis in the target plant, leading to yellowing and whitening of leaves, impairing normal photosynthesis, and ultimately causing complete plant death. It is absorbed by the plant's stems and leaves after application, showing effects within 3-4 days, causing weeds to die after their stems and leaves turn white. Quinalazine is decomposed within sorghum, exhibiting high safety for sorghum. It can be applied to sorghum, wheat, corn, sugarcane, peanuts, cotton, etc., and has good effects on weeds such as foxtail grass, barnyard grass, wild millet, wild sorghum, sedge, sedge, velvetleaf, burdock, cocklebur, amaranth, lambsquarters, sedge, sedge, sedge, sedge, sedge, sedge, speedwell, chickweed, etc., and has a broad market. Currently, in existing technologies, the synthesis of quinclorac involves many reaction steps and a long reaction cycle. It usually requires first cyaniding the methyl compound and cuprous cyanide, then hydrolyzing it with sulfuric acid to form acid, and finally acylation, 1,3-cyclohexanedione esterification, and acetone cyanohydrin transposition reaction to obtain the quinclorac product. Existing quinclorac synthesis production equipment suffers from the problems of multiple reaction equipment and long production cycle; and there is currently a lack of such technologies. Summary of the Invention
[0003] To overcome the shortcomings of the prior art, this utility model proposes a novel quinacrine production system.
[0004] To achieve the above objectives, this utility model employs the following technical solution: A quinacrine production system includes a mixing vessel, a high-pressure vessel at the bottom of the mixing vessel, and a quinacrine distillation vessel connected to the outlet of the high-pressure vessel. A hydrochloric acid high-level tank is located at the upper inlet of the quinacrine distillation vessel. A three-in-one filter is connected to the lower outlet of the quinacrine distillation vessel, and a first condenser is connected to the upper outlet. A vibrating screen and a bagging machine are sequentially connected to the lower outlet of the three-in-one filter. A second condenser is located at the upper outlet of the three-in-one filter. An ethylene glycol dimethyl ether receiving tank is connected to the lower outlet of the first condenser, and a water receiving tank is connected to the lower outlet of the second condenser. A nitrogen inlet pipe and a carbon monoxide inlet pipe are located at the inlet of the high-pressure vessel.
[0005] Preferably, material valves are provided between the nitrogen inlet pipe and the high-pressure vessel, between the carbon monoxide inlet pipe and the high-pressure vessel, between the mixing vessel and the high-pressure vessel, between the high-pressure vessel and the quinacrine distillation vessel, between the hydrochloric acid high-level tank and the quinacrine distillation vessel, between the quinacrine distillation vessel and the three-in-one filter, between the three-in-one filter and the vibrating screen, and between the vibrating screen and the bagging machine.
[0006] Preferably, the three-in-one filter is equipped with a stirring paddle and a heating jacket.
[0007] Preferably, the bottom of the mixing vessel is higher than the top of the high-pressure vessel, the bottom of the quinacrine distillation vessel is higher than the top of the three-in-one filter, the bottom of the three-in-one filter is higher than the top of the vibrating screen, and the bottom of the hydrochloric acid high-level tank is higher than the top of the quinacrine distillation vessel.
[0008] Compared with the prior art, the advantages and positive effects of this utility model are as follows: The device provided by this invention can adjust and improve the existing production system, reduce the number of devices in the system, shorten the reaction time, reduce the production cost, and improve the production efficiency. Moreover, the quinacrine prepared by this system has a high product purity. Attached Figure Description
[0009] Figure 1 This is a schematic diagram of the structure of this utility model.
[0010] The attached figures are labeled as follows: 1 Mixing vessel, 2 High pressure vessel, 3 Quinaloxone distillation vessel, 4 Hydrochloric acid high-level tank, 5 First condenser, 6 Ethylene glycol dimethyl ether receiving tank, 7 Three-in-one filter, 8 Second condenser, 9 Water receiving tank, 10 Vibrating screen, 11 Bagging machine, 12 Nitrogen inlet pipe, 13 Carbon monoxide inlet pipe, 14 Manual valve. Detailed Implementation
[0011] To better understand the above-mentioned objectives, features, and advantages of this utility model, the present utility model will be further described below with reference to the accompanying drawings and embodiments. It should be noted that, unless otherwise specified, the embodiments and features described in these embodiments can be combined with each other.
[0012] Many specific details are set forth in the following description in order to provide a full understanding of the present invention. However, the present invention may also be implemented in other ways different from those described herein. Therefore, the present invention is not limited to the specific embodiments disclosed in the following specification.
[0013] Example 1 The attached figure shows a specific embodiment of this utility model, such as... Figure 1The quinacrine production system shown includes a mixing vessel 1. The lower part of the mixing vessel 1 is connected to a high-pressure vessel 2 via a pipeline. A gas pipeline is installed above the high-pressure vessel 2, with its inlet branching into two branches: a nitrogen inlet pipe 12 and a carbon monoxide inlet pipe 13. These two inlet pipes are initially connected separately, then merged into a main inlet pipe via an adapter, which in turn connects to the upper part of the high-pressure vessel 2. The inlet end of the liquid outlet pipeline of the high-pressure vessel 2 extends to the lower end of the vessel, and its outlet end connects to the upper end of a quinacrine distillation vessel 3. The upper end of the quinacrine distillation vessel 3 is also equipped with another liquid inlet pipeline connecting to a hydrochloric acid high-level tank. The lower part of the quinacrine distillation vessel 3 connects to the upper end of a three-in-one filter 7. The lower part of the three-in-one filter 7 is connected sequentially to a vibrating screen 10 and a bagging machine 11 via pipelines. The upper end of the quinacrine distillation kettle is connected to the first condenser 5 via a pipeline. The outlet end of the first condenser 5 is connected to the ethylene glycol dimethyl ether receiving tank 6 via a pipeline. The upper end of the three-in-one filter 7 is connected to the second condenser 8 via a pipeline. The lower end of the second condenser 8 is connected to the water receiving tank 9 via a pipeline.
[0014] Material valves 14, preferably manual valves, are installed between the nitrogen inlet pipe 12 and the high-pressure vessel 2, between the carbon monoxide inlet pipe 13 and the high-pressure vessel 2, between the mixing vessel 1 and the high-pressure vessel 2, between the high-pressure vessel 2 and the quinclorac distillation vessel 3, between the hydrochloric acid high-level tank 4 and the quinclorac distillation vessel 3, between the quinclorac distillation vessel 3 and the three-in-one filter 7, between the three-in-one filter 7 and the vibrating screen 10, and between the vibrating screen 10 and the bagging machine 11. The three-in-one filter 7 is equipped with a stirring paddle and a heating jacket. To save energy input and achieve self-flow of materials under gravity, the bottom of the mixing vessel 1 is higher than the top of the high-pressure vessel 2, the bottom of the quinclorac distillation vessel 3 is higher than the top of the three-in-one filter 7, the bottom of the three-in-one filter 7 is higher than the top of the vibrating screen 10, and the bottom of the hydrochloric acid high-level tank 4 is higher than the top of the quinclorac distillation vessel 3.
[0015] A typical production process is as follows: 400 kg of methylated compound (6-bromo-3-(2,6-dimethyl)-5-methylquinazoline-2,4(1H,3H)dione) (provided by Shanghai Changfeng Biomedical Technology Co., Ltd.), 450 kg of triethylamine, 138 kg of 1,3-cyclohexanedione, 0.8 kg of palladium chloride catalyst (CAS No.: 7647-10-1), and 2800 kg of ethylene glycol dimethyl ether (moisture content <0.1%) are added to a mixing vessel and stirred for 1 hour at a stirring speed of 200 rpm. The mixture is then discharged into a high-pressure reactor 2. Then, carbon monoxide is introduced into the high-pressure reactor 2 to 3.5 MPa, and the carbonylation reaction is carried out at 130°C for 40 h. Afterward, the manual valve on the nitrogen inlet pipe 12 is opened, and nitrogen enters the high-pressure reactor 2 through the nitrogen inlet pipe 12 to 0.3 MPa. The reaction material in the high-pressure reactor 2 is then pumped into the quinacrine distillation vessel 3 for distillation. The temperature of the quinacrine distillation vessel is maintained at 90°C. The ethylene glycol dimethyl ether vapor generated during the distillation process is condensed by the first condenser 5 and stored in the ethylene glycol dimethyl ether receiving tank 6. After the distillation is completed, 500 kg of deionized water is added, and about 800 kg of 30% hydrochloric acid solution is added dropwise to adjust the pH to 1. The material is then discharged into the three-in-one filter 7 for filtration, rinsing, and drying (50°C). During the drying process, the water vapor is condensed by the second condenser 8 and stored in the water receiving tank 9. After drying, the product passes through a vibrating screen 10 and is then bagged by an automatic bagging machine 11 to obtain 410 kg of quinacrine product with a content of 98%, with a yield of 90%. Unless otherwise specified, the process conditions in the above process are consistent with the traditional quinacrine preparation route.
[0016] The above description is merely a preferred embodiment of the present utility model and is not intended to limit the present utility model in any other way. Any person skilled in the art may make changes or modifications to the above-disclosed technical content to create equivalent embodiments for application in other fields. However, any simple modifications, equivalent changes, and modifications made to the above embodiments based on the technical essence of the present utility model without departing from the technical solution of the present utility model shall still fall within the protection scope of the technical solution of the present utility model.
Claims
1. A system for producing quinclorac, characterized in that, The apparatus includes a mixing vessel, with a high-pressure vessel at its lower part. The outlet of the high-pressure vessel is connected to a quinacrine distillation vessel. A hydrochloric acid high-level tank is installed at the upper inlet of the quinacrine distillation vessel. A three-in-one filter is connected to the lower outlet of the quinacrine distillation vessel, and a first condenser is connected to the upper outlet. A vibrating screen and a bagging machine are sequentially connected to the lower outlet of the three-in-one filter. A second condenser is installed at the upper outlet of the three-in-one filter. An ethylene glycol dimethyl ether receiving tank is connected to the lower outlet of the first condenser, and a water receiving tank is connected to the lower outlet of the second condenser. A nitrogen inlet pipe and a carbon monoxide inlet pipe are installed at the inlet of the high-pressure vessel.
2. The quinacrine production system according to claim 1, characterized in that, Material valves are installed between the nitrogen inlet pipe and the high-pressure vessel, the carbon monoxide inlet pipe and the high-pressure vessel, the mixing vessel and the high-pressure vessel, the high-pressure vessel and the quinacrine distillation vessel, the hydrochloric acid high-level tank and the quinacrine distillation vessel, the quinacrine distillation vessel and the three-in-one filter, the three-in-one filter and the vibrating screen, and the vibrating screen and the bagging machine.
3. The quinacrine production system according to claim 1, characterized in that, The three-in-one filter is equipped with a stirring paddle and a heating jacket.
4. The quinacrine production system according to claim 1, characterized in that, The bottom of the mixing vessel is higher than the top of the high-pressure vessel, the bottom of the quinacrine distillation vessel is higher than the top of the three-in-one filter, the bottom of the three-in-one filter is higher than the top of the vibrating screen, and the bottom of the hydrochloric acid high-level tank is higher than the top of the quinacrine distillation vessel.