CN214571632U - Economic and environment-friendly triazine amide production system - Google Patents

Abstract

The utility model provides a triazine amide production system of economic environmental protection, including the alkylation cauldron, it adds the pipeline to be provided with toluene on the alkylation cauldron, chloroacetone adds pipeline and solid material inlet, the bottom of alkylation cauldron sets up alkylate liquid outlet line and links to each other with the washing cauldron, it adds the pipeline to be provided with the washing water on the washing cauldron, there is toluene on the extraction cauldron to add the pipeline, the lower part of washing cauldron and the lower part of extraction cauldron are provided with organic phase fluid-discharge tube respectively and desolventizing the cauldron and link to each other, desolventizing the kettle desolventizing the material export and expand the ring cauldron and link to each other, desolventizing the solvent export of cauldron and toluene recycling system link to each other, the crystallization cauldron links to each other with centrifuge, centrifuge's centrifugal mother liquor removes centrifugal mother liquor recovery system. The triazine amide and the solvent in the centrifugal mother liquor can be recovered, the solvent can be recycled, automatic production can be realized, environmental pollution is reduced, harm of organic matters to the body of workers is reduced, and the cost is reduced.

Description

Economic and environment-friendly triazine amide production system

Technical Field

The utility model relates to an economic environmental protection's triazine amide production system belongs to the chemical production field.

Background

After years of research and development, the synthesis process of pymetrozine is basically mature. At present, hydrazine hydrate and ethyl acetate are generally adopted as starting materials to synthesize intermediate triazine amide at home and abroad, and then the intermediate triazine amide is reacted with tobacco aldehyde to generate pymetrozine technical. The synthesis process for synthesizing triazine amide by using oxadiazolone comprises the following steps: and (3) synthesizing oxazole acetone, sequentially putting toluene, oxadiazolone and sodium methoxide into an alkylation kettle, heating to react and remove a solvent, and finishing a salt forming reaction. Then adding a catalyst, adding acetone chloride, and transferring to a washing kettle after the heat preservation is finished. Adding water into a washing kettle for washing and layering, transferring the lower layer to an extraction kettle, adding toluene for extraction, and transferring to a triazine amide synthesis procedure together with the upper layer of the washing kettle; synthesizing triazine amide, desolventizing the upper layer of a washing kettle, completely removing a solvent toluene, transferring to a toluene recovery process, transferring the material after the solvent removal to an ring expanding kettle, adding methanol and hydrazine hydrate, preserving heat, and crystallizing, centrifuging and drying after the heat preservation to obtain the triazine amide.

At present, manual feeding is adopted for feeding, the labor cost is high, organic matters are volatile, the environmental pollution is caused, and the body of workers is injured.

The solvent used in the reaction process, such as toluene, is directly used as three wastes for treatment, which not only causes a great deal of waste, but also has high treatment cost. The mother liquor after the triazine amide crystallization centrifugation contains triazine amide products and methanol solvent, and the three wastes are directly treated, so that the cost is increased and the products are wasted. Therefore, how to realize the recovery of the solvent and the product and reduce the treatment cost of the mother liquor becomes a problem to be solved.

SUMMERY OF THE UTILITY MODEL

In order to solve the technical problems, the utility model aims to provide an economic and environment-friendly triazine amide production system,

in order to realize the above object of the present invention, the present invention provides an economic and environmental-friendly triazine amide production system, which is characterized in that: comprises an alkylation kettle, wherein a toluene adding pipeline, a chloroacetone adding pipeline and a solid material adding port are arranged on the alkylation kettle, an alkylation liquid outlet pipeline is arranged at the bottom of the alkylation kettle and connected with a washing kettle, a washing water adding pipeline is arranged on the washing kettle, a lower-layer aqueous phase liquid discharge pipe is arranged at the bottom of the washing kettle and connected with an extraction kettle, a toluene adding pipeline is arranged on the extraction kettle, organic phase liquid discharge pipes are respectively arranged at the lower part of the washing kettle and the lower part of the extraction kettle and connected with a desolventizing kettle, a desolventizing material outlet of the desolventizing kettle is connected with an expanding kettle, a solvent outlet of the desolventizing kettle is connected with a toluene recycling system, a hydrazine hydrate adding pipeline and a methanol adding pipeline are arranged on the expanding kettle, a material outlet pipeline of the expanding kettle is connected with a crystallization kettle, the crystallization kettle is connected with a centrifuge, and a centrifugal mother liquor of the centrifuge is removed to a centrifugal mother liquor recycling system, and drying the filter cake of the centrifugal machine in a dryer.

By adopting the scheme, a toluene adding pipeline and a chloroacetone adding pipeline are arranged on the alkylation kettle, a hydrazine hydrate adding pipeline and a methanol adding pipeline are arranged on the ring expansion kettle, automatic control valves are arranged on the adding pipelines, the toluene adding pipeline, the chloroacetone adding pipeline, the hydrazine hydrate adding pipeline and the methanol adding pipeline are respectively connected with a toluene metering tank, a chloroacetone metering tank, a hydrazine hydrate metering tank and a methanol metering tank, and dropping liquid pipes can be further arranged on the chloroacetone adding pipeline and the hydrazine hydrate adding pipeline. The toluene metering tank, the chloroacetone metering tank, the hydrazine hydrate metering tank and the methanol metering tank are respectively connected with the toluene storage tank, the chloroacetone storage tank, the hydrazine hydrate storage tank and the methanol storage tank, and toluene, chloroacetone, hydrazine hydrate and methanol in the toluene storage tank, the chloroacetone storage tank, the hydrazine hydrate storage tank and the methanol storage tank are added into the toluene metering tank, the chloroacetone metering tank, the hydrazine hydrate metering tank and the methanol metering tank through a pump or nitrogen, so that automatic production can be realized, volatilization of organic compounds is reduced, and the factory environment is improved.

In the scheme, the method comprises the following steps: the mother liquor recovery system comprises a mother liquor desolventizing kettle, wherein a solvent recovery pipeline of the mother liquor desolventizing kettle is connected with a methanol receiving tank through a cooler, the methanol receiving tank is connected with a rectifying tower, a desolventizing liquid outlet at the bottom of the mother liquor desolventizing kettle is connected with a mother liquor crystallizing kettle, a kettle residual liquid discharge pipeline is further arranged at the bottom of the mother liquor desolventizing kettle, the mother liquor crystallizing kettle is connected with a mother liquor centrifugal machine, and a mother liquor outlet pipeline of the mother liquor centrifugal machine is connected with the mother liquor desolventizing kettle. Transferring the centrifugal mother liquor to a mother liquor desolventizing kettle for primary desolventizing, crystallizing, centrifuging and drying to obtain triazine amide, returning the secondary centrifugal mother liquor to the mother liquor desolventizing kettle again to remove the solvent, taking the mother liquor as a kettle residue bucket, and sending the removed solvent to a rectification process to recover methanol.

In the scheme, the method comprises the following steps: the toluene recycling system comprises a washing kettle, an alkali liquor adding pipeline and a washing water adding pipeline are arranged on the washing kettle, a water phase liquid discharge pipe is arranged at the bottom of the washing kettle and connected with a rectifying tower, an upper organic phase liquid discharge pipe is arranged at the bottom of the washing kettle and connected with a dehydration kettle, and a solvent outlet pipeline of the dehydration kettle is connected with a toluene adding pipeline of an alkylation kettle. And (3) adding washing water and alkali liquor into the toluene in a washing kettle for washing, sending lower-layer methanol and water to a rectification process for recovering methanol, putting the toluene in a dehydration kettle for temperature rise and dehydration, and returning the toluene to the triazine amide process for reuse after the toluene is qualified.

In the scheme, the method comprises the following steps: and automatic control valves are arranged on the toluene adding pipeline, the chloropropanone adding pipeline, the washing water adding pipeline, the hydrazine hydrate adding pipeline, the methanol adding pipeline and the alkali liquor adding pipeline.

Has the advantages that: the utility model discloses a triazine amide production system of economic environmental protection can realize retrieving triazine amide and solvent in the centrifugal mother liquor, can realize the recycle of solvent, can realize automated production, reduces environmental pollution, reduces the injury of organic matter to workman's health, reduce cost.

Drawings

Fig. 1 is a schematic structural diagram of the present invention.

The specific implementation mode is as follows:

the present invention will be described in further detail with reference to the following examples and drawings.

Example 1

As shown in figure 1, the utility model discloses an economic environmental protection's triazine amide production system comprises alkylation cauldron 1, washing kettle 2, extraction cauldron 3, desolventizing cauldron 4, ring expanding cauldron 5, crystallization kettle 6, centrifuge 7, drying-machine 8 that link to each other in proper order.

The alkylation kettle 1 is provided with a toluene adding pipeline, a chloropropanone adding pipeline and a solid material adding port, wherein the solid material comprises oxadiazolone, sodium methoxide, a catalyst and the like. The bottom of the alkylation kettle 1 is provided with an alkylation liquid outlet pipeline connected with a washing kettle 2, the washing kettle 2 is provided with a washing water inlet pipeline, the washing water inlet pipeline is provided with an automatic control valve, the bottom of the washing kettle 2 is provided with a lower-layer aqueous phase liquid discharge pipe connected with an extraction kettle 3, the lower-layer aqueous phase liquid discharge pipe is provided with an automatic control valve, the extraction kettle 3 is provided with a toluene inlet pipeline, the toluene inlet pipeline is provided with an automatic control valve, the lower part of the washing kettle 2 and the lower part of the extraction kettle 3 are respectively provided with an organic phase liquid discharge pipe (provided with an automatic control valve) connected with a desolventizing kettle 4, a desolventizing material outlet (provided with an automatic control valve) of the desolventizing kettle 4 is connected with an expanded ring kettle 5, a solvent outlet pipeline of the desolventizing kettle 4 is connected with a toluene recycling system after passing through a condenser, the expanded ring kettle 5 is provided with a hydrazine hydrate inlet pipeline (provided with an automatic control valve) and a methanol inlet pipeline (provided with an automatic control valve), the material outlet pipeline (provided with an automatic control valve) of the ring expanding kettle 5 is connected with the crystallization kettle 6, the crystallization kettle 6 is connected with the centrifuge 7, the centrifugal mother liquor of the centrifuge 7 is sent to a centrifugal mother liquor recovery system, and the filter cake of the centrifuge 7 is sent to the dryer 8 for drying.

The toluene adding pipeline, the chloropropanone adding pipeline, the hydrazine hydrate adding pipeline and the methanol adding pipeline are respectively connected with the toluene metering tank, the chloropropanone metering tank, the hydrazine hydrate metering tank and the methanol metering tank, wherein dropping pipes can be further arranged on the chloropropanone adding pipeline and the hydrazine hydrate adding pipeline. The toluene metering tank, the chloroacetone metering tank, the hydrazine hydrate metering tank and the methanol metering tank are respectively connected with the toluene storage tank, the chloroacetone storage tank, the hydrazine hydrate storage tank and the methanol storage tank, and toluene, chloroacetone, hydrazine hydrate and methanol in the toluene storage tank, the chloroacetone storage tank, the hydrazine hydrate storage tank and the methanol storage tank are added into the toluene metering tank, the chloroacetone metering tank, the hydrazine hydrate metering tank and the methanol metering tank through a pump or nitrogen, so that automatic production can be realized, volatilization of organic compounds is reduced, and the factory environment is improved.

The mother liquor recovery system comprises a mother liquor desolventizing kettle 9, a solvent recovery pipeline of the mother liquor desolventizing kettle 9 is connected with a methanol receiving tank 10 through a cooler, the methanol receiving tank 10 is connected with a rectifying tower 14, a desolventizing liquid outlet (provided with an automatic control valve) at the bottom of the mother liquor desolventizing kettle 9 is connected with a mother liquor crystallizing kettle 11, a kettle bottom of the mother liquor desolventizing kettle 9 is also provided with a kettle residual liquid discharge pipeline (provided with an automatic control valve), the mother liquor crystallizing kettle 11 is connected with a mother liquor centrifugal machine 12, and a mother liquor outlet pipeline (provided with an automatic control valve) of the mother liquor centrifugal machine 12 is connected with the mother liquor desolventizing kettle 9. Transferring the centrifugal mother liquor to a mother liquor desolventizing kettle for primary desolventizing, crystallizing, centrifuging and drying to obtain triazine amide, returning the secondary centrifugal mother liquor to the mother liquor desolventizing kettle again to remove the solvent, taking the mother liquor as a kettle residue bucket, and sending the removed solvent to a rectification process to recover methanol.

The toluene recycling system comprises a washing kettle 13, an alkali liquor adding pipeline and a washing water adding pipeline are arranged on the washing kettle 13, automatic control valves are respectively arranged on the alkali liquor adding pipeline and the washing water adding pipeline, a water phase liquid discharge pipe is arranged at the bottom of the washing kettle 13 and connected with a rectifying tower 14, an upper organic phase liquid discharge pipe is arranged at the bottom of the washing kettle 13 and connected with a dehydration kettle 15, and a solvent outlet pipeline of the dehydration kettle 15 is connected with a toluene adding pipeline of an alkylation kettle. And (3) adding washing water and alkali liquor into the toluene in a washing kettle for washing, sending the lower layer of methanol and aqueous solution to a rectification process for recovering the methanol, putting the toluene in a dehydration kettle for temperature rise and dehydration, and returning the toluene to the triazine amide process for reuse after the toluene is qualified.

The above description is provided for the purpose of describing the present invention in more detail with reference to the preferred embodiments, and it should not be construed that the present invention is limited to these descriptions, and it will be apparent to those skilled in the art that the present invention can be implemented in many ways without departing from the spirit and scope of the present invention.

Claims (4)

1. An economical and environment-friendly triazine amide production system is characterized in that: comprises an alkylation kettle, wherein a toluene adding pipeline, a chloroacetone adding pipeline and a solid material adding port are arranged on the alkylation kettle, an alkylation liquid outlet pipeline is arranged at the bottom of the alkylation kettle and connected with a washing kettle, a washing water adding pipeline is arranged on the washing kettle, a lower-layer aqueous phase liquid discharge pipe is arranged at the bottom of the washing kettle and connected with an extraction kettle, a toluene adding pipeline is arranged on the extraction kettle, organic phase liquid discharge pipes are respectively arranged at the lower part of the washing kettle and the lower part of the extraction kettle and connected with a desolventizing kettle, a desolventizing material outlet of the desolventizing kettle is connected with an expanding kettle, a solvent outlet of the desolventizing kettle is connected with a toluene recycling system, a hydrazine hydrate adding pipeline and a methanol adding pipeline are arranged on the expanding kettle, a material outlet pipeline of the expanding kettle is connected with a crystallization kettle, the crystallization kettle is connected with a centrifuge, and a centrifugal mother liquor of the centrifuge is removed to a centrifugal mother liquor recycling system, and drying the filter cake of the centrifugal machine in a dryer.

2. The economical and environment-friendly triazine amide production system according to claim 1, wherein: the mother liquor recovery system comprises a mother liquor desolventizing kettle, wherein a solvent recovery pipeline of the mother liquor desolventizing kettle is connected with a methanol receiving tank through a cooler, the methanol receiving tank is connected with a rectifying tower, a desolventizing liquid outlet at the bottom of the mother liquor desolventizing kettle is connected with a mother liquor crystallizing kettle, a kettle residual liquid discharge pipeline is further arranged at the bottom of the mother liquor desolventizing kettle, the mother liquor crystallizing kettle is connected with a mother liquor centrifugal machine, and a mother liquor outlet pipeline of the mother liquor centrifugal machine is connected with the mother liquor desolventizing kettle.

3. The economical and environment-friendly triazine amide production system according to claim 2, wherein: the toluene recycling system comprises a washing kettle, an alkali liquor adding pipeline and a washing water adding pipeline are arranged on the washing kettle, a water phase liquid discharge pipe is arranged at the bottom of the washing kettle and connected with a rectifying tower, an upper organic phase liquid discharge pipe is arranged at the bottom of the washing kettle and connected with a dehydration kettle, and a solvent outlet pipeline of the dehydration kettle is connected with a toluene adding pipeline of an alkylation kettle.

4. Economical and environmentally friendly triazine amide production system according to any of claims 1-3, characterized in that: and automatic control valves are arranged on the toluene adding pipeline, the chloropropanone adding pipeline, the washing water adding pipeline, the hydrazine hydrate adding pipeline, the methanol adding pipeline and the alkali liquor adding pipeline.

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