A production system of imazamox quaternary ammonium salt intermediate

Abstract

The utility model relates to a kind of methoxymetominostrobin quaternary ammonium salt intermediate production system, belong to chemical equipment technical field.Quaternary ammonium salt synthesis kettle upper portion entrance is connected with dimethyl benzylamine high tank, lower portion outlet is connected with centrifuge, centrifuge outlet is respectively connected with mother liquor receiving tank and double-cone drying machine through pipeline, mother liquor receiving tank is connected with quaternary ammonium salt synthesis kettle upper portion by circulation pipeline, quaternary ammonium salt synthesis kettle upper end is also connected with first condenser by pipeline, and first condenser outlet is connected with first methanol receiving tank by pipeline;Double-cone drying machine upper portion outlet is connected with second condenser by pipeline, and second condenser outlet is connected with second methanol receiving tank by pipeline.The utility model optimizes methoxymetominostrobin quaternary ammonium salt intermediate production system device, realizes methanol mother liquor to hit back quaternary ammonium salt synthesis kettle, carries out in-circulation, after equipment adjustment, avoid the generation of waste water, reaction cycle is short, environmental protection energy saving, suitable for large-batch industrial application.

Description

Technical Field

[0001] This utility model relates to a production system for methoxymethylene nicotine quaternary ammonium salt intermediates, belonging to the field of chemical equipment technology. Background Technology

[0002] Methoxyfenozide is an imidazolinone herbicide developed by BASF (now cyanamide). It is an inhibitor of acetolactate synthase (ALS) or acetate-hydroxy acid synthase (AHAs), disrupting protein synthesis, interfering with DNA synthesis, and hindering cell division and growth, ultimately leading to plant death. It is effective against most annual grasses and broadleaf weeds, such as wild oats, barnyard grass, foxtail grass, golden foxtail grass, wild oats, millet, barnyard grass, crabgrass, dayflower (before the 3-leaf stage), black nightshade, velvetleaf, amaranth, lambsquarters, small lambsquarters, cocklebur, elm, waterthorn, wolfsbane, chickweed, willow-leaved knotweed, weasel petals, shepherd's purse, etc., and also inhibits perennial weeds such as sow thistle and thistle. As an important intermediate in methoxyfenozide, the demand for 5-bromomethylpyridine-2,3-dicarboxylic acid dimethyl benzylamine quaternary ammonium salt (hereinafter referred to as quaternary ammonium salt) is also significant. Existing processes for synthesizing quaternary ammonium salts suffer from problems such as long reaction cycles, strong odors, and difficulty in treating wastewater. The basis for process improvement lies in equipment design. Currently, there is a lack of complete sets of equipment specifically designed for the synthesis of methoxymethylene quaternary ammonium salts, and this field is still in a technological vacuum. Summary of the Invention

[0003] To overcome the shortcomings of the prior art, this utility model proposes a production system for methoxymethylene nicotine quaternary ammonium salt intermediates.

[0004] To achieve the above objectives, this utility model employs the following technical solution: A production system for a methoxymethylene quaternary ammonium salt intermediate includes a quaternary ammonium salt synthesis reactor. A dimethyl benzylamine high-level tank is connected to the upper inlet of the reactor, and a centrifuge is connected to the lower outlet. The centrifuge outlet is connected via pipelines to a mother liquor receiving tank and a double-cone dryer. The mother liquor receiving tank is connected to the upper part of the quaternary ammonium salt synthesis reactor via a circulation pipeline. The upper end of the quaternary ammonium salt synthesis reactor is also connected via a pipeline to a first condenser. The outlet of the first condenser is connected via a pipeline to a first methanol receiving tank. The upper outlet of the double-cone dryer is connected via a pipeline to a second condenser, and the outlet of the second condenser is connected via a pipeline to a second methanol receiving tank.

[0005] Preferably, a material valve and a material pump are provided between the mother liquor receiving tank and the quaternary ammonium salt synthesis reactor, and material valves are provided between the quaternary ammonium salt synthesis reactor and the dimethyl benzylamine high-level tank, between the quaternary ammonium salt synthesis reactor and the centrifuge, and between the centrifuge and the double cone dryer.

[0006] Preferably, the bottom of the dimethylbenzylamine high-level tank is horizontally higher than the top of the quaternary ammonium salt synthesis reactor, the bottom of the quaternary ammonium salt synthesis reactor is horizontally higher than the top of the centrifuge, and the bottom of the centrifuge is horizontally higher than the double cone dryer.

[0007] Compared with the prior art, the advantages and positive effects of this utility model are as follows: This invention optimizes the production system of methoxymethylene quaternary ammonium salt intermediates, enabling the methanol mother liquor to be returned to the quaternary ammonium salt synthesis reactor for internal circulation. After the equipment is adjusted, the water introduction step is omitted, avoiding the generation of wastewater. The reaction cycle is short, environmentally friendly and energy-saving, and suitable for large-scale industrial applications. Attached Figure Description

[0008] Figure 1 This is a schematic diagram of the structure of this utility model.

[0009] The attached figures are labeled as follows: 1 Quaternary ammonium salt synthesis reactor, 2 Dimethylbenzylamine high-level tank, 3 First condenser, 4 First methanol receiving tank, 5 Centrifuge, 6 Double cone dryer, 7 Second condenser, 8 Second methanol receiving tank, 9 Mother liquor receiving tank, 10 Material valve, 11 Material pump. Detailed Implementation

[0010] 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.

[0011] 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.

[0012] Example 1 The attached figure shows a specific embodiment of this utility model, such as... Figure 1The production system for the intermediate of methoxymethylene nicotine quaternary ammonium salt shown has two material inlets at the top of the quaternary ammonium salt synthesis reactor 1, which are connected to the bottom outlet of the dimethyl benzylamine high-level tank 2 and the outlet of the circulation pipeline of the mother liquor receiving tank 9 via pipelines. The bottom of the quaternary ammonium salt synthesis reactor 1 is connected to a centrifuge 5 via pipelines. The lower part of the centrifuge 5 has two outlets: a liquid outlet and a solid outlet. The liquid outlet is connected to the inlet of the material circulation pipeline and then to the upper end of the mother liquor receiving tank 9. The solid outlet is connected to a double-cone dryer 6 via pipelines. The lower end of the mother liquor receiving tank 9 is further connected to the upper part of the quaternary ammonium salt synthesis reactor 1 via a circulation pipeline, and a material valve 10 and a material pump 11 are installed on the circulation pipeline at the lower end of the mother liquor receiving tank 9. The material outlet at the top of the quaternary ammonium salt synthesis reactor 1 is connected to a first condenser 3 via pipelines, and the lower outlet of the first condenser 3 is connected to a first methanol receiving tank 4 via pipelines. The upper end of the double-cone dryer 6 is connected to a second condenser 7 via a pipeline, and the lower part of the second condenser 7 is connected to a second methanol receiving tank 8 via a pipeline. A material valve 10 and a material pump 11 are installed between the mother liquor receiving tank 9 and the quaternary ammonium salt synthesis reactor 1. Material valves 10 are also installed between the quaternary ammonium salt synthesis reactor 1 and the dimethylbenzylamine high-level tank 2, between the quaternary ammonium salt synthesis reactor 1 and the centrifuge 5, and between the centrifuge 5 and the double-cone dryer 6. Preferably, the material valves 10 are manual valves. To save energy and allow materials to flow downwards under gravity between some parts of the equipment, in this invention, the bottom horizontal position of the dimethylbenzylamine high-level tank 2 is higher than the top horizontal position of the quaternary ammonium salt synthesis reactor 1, the bottom horizontal position of the quaternary ammonium salt synthesis reactor 1 is higher than the top horizontal position of the centrifuge 5, and the bottom horizontal position of the centrifuge 5 is higher than the double-cone dryer 6.

[0013] A typical process route is as follows: 367 kg of the brominated product (provided by Shanghai Changfeng Biomedical Technology Co., Ltd., the main component of which is methyl 5-bromomethylpyridine-2,3-pyridinedicarboxylate) and 1000 kg of methanol were added to the quaternary ammonium salt synthesis reactor 1, with the stirring speed maintained at 200 rpm. 150 kg of N,N-dimethylbenzylamine was added to the dimethylbenzylamine high-level tank 2, and the manual valve below the dimethylbenzylamine high-level tank 2 was opened to add dimethylbenzylamine dropwise at room temperature, ensuring the reaction solution temperature did not exceed 40°C. The dropwise temperature was 35°C, and the dropwise time was 2 hours. After the dropwise addition was complete, the temperature was raised to 40°C and maintained for 2 hours. After the reaction was completed, the methanol was distilled under reduced pressure (-0.09 MPa). The methanol vapor was condensed by condenser 3 and then entered the methanol receiving tank 4 under gravity. After distillation, the reaction solution was cooled to 0-5°C and maintained for 1 hour. It was then centrifuged by centrifuge 5, and the filter cake was dried in a double cone dryer 6 at 50°C for 2 hours. The mother liquor entered the mother liquor receiving tank 9 and was then transferred to the quaternary ammonium salt synthesis reactor 1 via transfer pump 11 for use in the synthesis of the next batch. The final yield was 478 kg of quaternary ammonium salt product with 98% purity, a yield of 96%.

[0014] 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 present utility model.

Claims

1. A production system for a methoxymethylene quaternary ammonium salt intermediate, characterized in that, The apparatus includes a quaternary ammonium salt synthesis reactor. The upper inlet of the reactor is connected to a dimethyl benzylamine high-level tank, and the lower outlet is connected to a centrifuge. The centrifuge outlet is connected via pipelines to a mother liquor receiving tank and a double-cone dryer. The mother liquor receiving tank is connected to the upper part of the quaternary ammonium salt synthesis reactor via a circulation pipeline. The upper end of the reactor is also connected to a first condenser via a pipeline, and the outlet of the first condenser is connected to a first methanol receiving tank via a pipeline. The upper outlet of the double-cone dryer is connected to a second condenser via a pipeline, and the outlet of the second condenser is connected to a second methanol receiving tank via a pipeline.

2. The production system for the methoxymethylene quaternary ammonium salt intermediate according to claim 1, characterized in that, Material valves and material pumps are installed between the mother liquor receiving tank and the quaternary ammonium salt synthesis reactor. Material valves are also installed between the quaternary ammonium salt synthesis reactor and the dimethyl benzylamine high-level tank, between the quaternary ammonium salt synthesis reactor and the centrifuge, and between the centrifuge and the double cone dryer.

3. The production system for the methoxymethylene quaternary ammonium salt intermediate according to claim 1, characterized in that, The bottom of the dimethylbenzylamine high-level tank is horizontally higher than the top of the quaternary ammonium salt synthesis reactor, the bottom of the quaternary ammonium salt synthesis reactor is horizontally higher than the top of the centrifuge, and the bottom of the centrifuge is horizontally higher than the double cone dryer.

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