Continuous production device for trans-3-chloro-2-propenyl hydroxylamine

Abstract

The utility model belongs to the technical field of chemical equipment, and discloses a trans-3-chloro-2-allyl hydroxylamine continuous production device which comprises a mixer, a tubular reactor, a receiving tank, an extraction kettle and a distillation kettle which are sequentially communicated through pipelines, valves and pumps, a feeding hole of the mixer is respectively communicated with an acetohydroxamic acid storage tank and a 1, 3-dichloropropene storage tank through a pipeline and a metering pump; the feeding hole of the tubular reactor is also communicated with a liquid caustic soda storage tank through a pipeline and a metering pump; the feed port of the extraction kettle is also communicated with a dichloromethane head tank through a pipeline and a metering pump, and the discharge port of the extraction kettle is respectively communicated with a water receiving tank and a distillation kettle through pipelines and valves; and a steam outlet of the distillation kettle is communicated with a dichloromethane receiving tank through a pipeline and a condenser. The device disclosed by the utility model can realize continuous production, is high in production efficiency and yield and good in product quality, and can meet the requirements of large-scale production.

Description

Technical Field

[0001] The utility model belongs to the technical field of chemical equipment, and particularly relates to a continuous production device for trans-3-chloro-2-propenylhydroxylamine. Background Art

[0002] Allyloxyamine (chloroamine) is the main raw material for the production of the pesticide clethodim, and is currently mainly used as a herbicide, with a broad market. In the production process of allyloxyamine, trans-3-chloro-2-propenylhydroxylamine is an important raw material, and the production demand is also relatively large. In the existing production process of trans-3-chloro-2-propenylhydroxylamine, the raw materials are added into the reaction kettle at one time for synthesis, and then the finished product is obtained through post-treatment; because the reaction is completed in the reaction kettle at one time, more impurities are generated in the reaction, and the yield of trans-3-chloro-2-propenylhydroxylamine is relatively low; this production method is also intermittent production, with low production capacity, which is not conducive to large-scale industrial production. Summary of the Invention

[0003] The technical problem to be solved by the utility model is to provide a continuous production device for trans-3-chloro-2-propenylhydroxylamine, which overcomes the defects of the prior art, can continuously produce, has high production efficiency and yield, good product quality, and can meet the needs of large-scale production.

[0004] To solve the above technical problem, the technical solution of the utility model is as follows:

[0005] A continuous production device for trans-3-chloro-2-propenylhydroxylamine, comprising a mixer, a tubular reactor, a receiving tank, an extraction kettle and a distillation kettle which are sequentially connected through pipelines, valves and pumps; the feed inlet of the mixer is respectively connected with an acetoxime acid storage tank and a 1,3-dichloropropene storage tank through pipelines and metering pumps; the feed inlet of the tubular reactor is also connected with a liquid caustic soda storage tank through a pipeline and a metering pump; the feed inlet of the extraction kettle is also connected with a dichloromethane high-level tank through a pipeline and a metering pump, and the discharge outlet of the extraction kettle is respectively connected with a water receiving tank and the distillation kettle through pipelines and valves; the steam outlet of the distillation kettle is connected to a dichloromethane receiving tank through a pipeline and a condenser.

[0006] Preferably, the mixer is a mixing reaction kettle, which is provided with a stirring device and a heat exchange device.

[0007] Preferably, the tubular reactor is provided with a heating device to ensure the reaction temperature in the reactor. The tubular reactor is an HL microchannel reactor, and the manufacturer is Guizhou Weihua Technology Co., Ltd.

[0008] Preferably, the receiving tank is provided with a venting device at the top to vent the steam generated by the high-temperature material, etc., to avoid the formation of high pressure in the tank and bring danger.

[0009] Preferably, the dichloromethane header tank is connected to the dichloromethane storage tank through a pipeline, a valve and a metering pump. Dichloromethane is provided to the dichloromethane header tank and transported to the extraction kettle to extract trans-3-chloro-2-propenylhydroxylamine.

[0010] Preferably, a window is provided on the side wall of the extraction kettle (for observing the stratification), and an online liquid density tester (for real-time detection of the stratification, and providing a detection signal to the automatic control system when the lower layer of water is detected to be drained) and an electric diverter valve are provided at the discharge port at the bottom of the kettle; the online liquid density tester and the electric diverter valve are both electrically connected to the DCS automatic control system. The online liquid density tester is provided by Xiamen Laisde Scientific Instrument Co., Ltd. The model of the electric diverter valve is DN50, and the manufacturer is Shanghai Fadeng Valve Co., Ltd.

[0011] Preferably, the distillation kettle is provided with a heating device to ensure the temperature of the material and to fractionate the material.

[0012] Preferably, the condenser is a wound tube condenser, and the manufacturer is Shandong Haomai Machinery Manufacturing Co., Ltd.

[0013] Due to the adoption of the above technical solution, the beneficial effects of the utility model are:

[0014] The utility model mixes acetohydroxamic acid aqueous solution and 1,3-dichloropropylene through a mixer, and then injects them into a tubular reactor together with liquid alkali, and reacts in the tubular reactor maintained at 50°C; the reaction liquid flows out of the tubular reactor and is collected by a receiving tank, and when it accumulates to a certain amount, it is transferred to an extraction kettle and added with dichloromethane for extraction; the dichloromethane layer is then transferred to a distillation kettle for distillation to obtain an allylic amide product, and the distilled dichloromethane vapor is condensed through a condenser and collected in a dichloromethane receiving tank under the action of gravity; the water layer after extraction in the extraction kettle is transferred to a water receiving tank for treatment. Through the above treatment, the defects of intermittent production in the prior art are overcome, continuous production is achieved, the impurity content of the product is reduced from 8% in the prior art to less than 1%, and the yield is also significantly improved; because continuous production is achieved, production efficiency and capacity are also significantly improved, and manual operations are greatly reduced, reducing labor costs, and therefore, it is very suitable for industrial production.

[0015] In short, the utility model can produce continuously, has high production efficiency and yield, good product quality, and can meet the needs of large-scale production. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 It is a structural schematic diagram of an embodiment of the utility model;

[0017] In the figure, 1 is a mixer; 2 is a tubular reactor; 3 is a receiving tank; 4 is an extraction kettle; 5 is a distillation kettle; 6 is an acetohydroxamic acid storage tank; 7 is a 1,3-dichloropropene storage tank; 8 is a liquid caustic soda storage tank; 9 is a methylene chloride elevated tank; 10 is a water receiving tank; 11 is a condenser; 12 is a methylene chloride receiving tank; 13 is a methylene chloride storage tank. Detailed implementation mode

[0018] The present utility model will be further described below in conjunction with the accompanying drawings and embodiments.

[0019] Embodiment 1:

[0020] As Figure 1 shown, a continuous production device for trans-3-chloro-2-propenylhydroxylamine includes a mixer 1, a tubular reactor 2, a receiving tank 3, an extraction kettle 4 and a distillation kettle 5 which are sequentially connected through pipelines (not marked), valves (not marked) and pumps (not marked); the feed inlet of the mixer 1 is respectively connected to an acetohydroxamic acid storage tank 6 and a 1,3-dichloropropene storage tank 7 through pipelines and metering pumps (not marked); the feed inlet of the tubular reactor 2 is also connected to a liquid caustic soda storage tank 8 through a pipeline and a metering pump; the feed inlet of the extraction kettle 4 is also connected to a methylene chloride elevated tank 9 through a pipeline and a metering pump, and the discharge outlet of the extraction kettle 4 is respectively connected to a water receiving tank 10 and the distillation kettle 5 through pipelines and valves; the steam outlet of the distillation kettle 5 is connected to a methylene chloride receiving tank 12 through a pipeline and a condenser 11.

[0021] The methylene chloride elevated tank 9 is connected to a methylene chloride storage tank 13 through pipelines, valves and metering pumps.

[0022] During actual production: the acetohydroxamic acid aqueous solution and 1,3-dichloropropene in the acetohydroxamic acid storage tank 6 and the 1,3-dichloropropene storage tank 7 are respectively transported to the mixer 1 in proportion through their respective metering pumps for mixing, and the mixed liquid and the liquid caustic soda from the liquid caustic soda storage tank 8 are jointly pumped into the tubular reactor 2 for reaction at a temperature of 50 °C; after the reaction liquid flows out, it is first collected by the receiving tank 3, and when it accumulates to a certain amount, it is transferred to the extraction kettle 4, and methylene chloride is added for extraction; after extraction, the methylene chloride layer containing trans-3-chloro-2-propenylhydroxylamine is transferred to the distillation kettle 5 for distillation to obtain the trans-3-chloro-2-propenylhydroxylamine product. The methylene chloride steam is condensed by the condenser 11 and then enters the methylene chloride receiving tank 12 for collection and preparation for reuse; the water layer in the extraction kettle 4 is separated and sent to the water receiving tank 10 for treatment.

[0023] It should be understood that these embodiments are only used to illustrate the present utility model and not to limit the scope of the present utility model. In addition, it should be understood that after reading the content taught by the present utility model, those skilled in the art can make various changes or modifications to the present utility model, and these equivalent forms also fall within the scope defined by the appended claims of this application.

Claims

1. A continuous production device for trans-3-chloro-2-propenylhydroxylamine, characterized in that: The invention comprises a mixer, a tubular reactor, a receiving tank, an extraction kettle and a distillation kettle which are connected in sequence through pipelines, valves and pumps; the feed port of the mixer is connected to an acetohydroxamic acid storage tank and a 1,3-dichloropropylene storage tank respectively through pipelines and metering pumps; the feed port of the tubular reactor is also connected to a liquid alkali storage tank through pipelines and metering pumps; the feed port of the extraction kettle is also connected to a dichloromethane high-level tank through pipelines and metering pumps, and the discharge port of the extraction kettle is respectively connected to a water receiving tank and a distillation kettle through pipelines and valves; the steam outlet of the distillation kettle is connected to the dichloromethane receiving tank through pipelines and condensers.

2. The continuous production device of trans-3-chloro-2-propenylhydroxylamine according to claim 1, characterized in that: The tubular reactor is provided with a heating device.

3. The continuous production device of trans-3-chloro-2-propenylhydroxylamine according to claim 1, characterized in that: A venting device is provided on the top of the receiving tank.

4. The continuous production device of trans-3-chloro-2-propenylhydroxylamine according to claim 1, characterized in that: The dichloromethane high-level tank is connected to the dichloromethane storage tank through a pipeline, a valve and a metering pump.

5. The continuous production device of trans-3-chloro-2-propenylhydroxylamine according to claim 1, characterized in that: A viewing window is arranged on the side wall of the extraction kettle, and an online liquid density tester and an electric diverter valve are arranged at the discharge port at the bottom of the kettle.

6. The continuous production device of trans-3-chloro-2-propenylhydroxylamine according to claim 1, characterized in that: The distillation kettle is provided with a heating device.

7. The continuous production device of trans-3-chloro-2-propenylhydroxylamine according to claim 1, characterized in that: The condenser is a wound tube condenser.

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