CN105254467A - Diuron waste liquid treatment process - Google Patents

Diuron waste liquid treatment process Download PDF

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Publication number
CN105254467A
CN105254467A CN201510692496.8A CN201510692496A CN105254467A CN 105254467 A CN105254467 A CN 105254467A CN 201510692496 A CN201510692496 A CN 201510692496A CN 105254467 A CN105254467 A CN 105254467A
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China
Prior art keywords
toluene
transferred
phosgene
still
light still
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CN201510692496.8A
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Chinese (zh)
Inventor
过学军
胡安胜
吴建平
高焰兵
戴玉婷
张军
刘长庆
徐小兵
黄显超
朱张
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Anhui Guangxin Agrochemcial Co Ltd
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Anhui Guangxin Agrochemcial Co Ltd
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Priority to CN201510692496.8A priority Critical patent/CN105254467A/en
Publication of CN105254467A publication Critical patent/CN105254467A/en
Pending legal-status Critical Current

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Abstract

The invention provides a diuron waste liquid treatment process which comprises the following steps: quantitative toluene is fed into a cold light kettle for absorbing a certain amount of phosgene, after the toluene is analyzed to be up to standard, and a metered 3,4-dichloroaniline toluene solution is dropwisely added while light is fed; light is continuously fed into the cold light kettle for reaction, phosgene is continuously fed, stirring is stopped, the mixture is transferred to a hot light kettle, and the hot light kettle is heated slowly; the material is transferred to a solvent removal kettle, a phosgene toluene solution is transferred to a light removal kettle, and nitrogen is fed into the light removal kettle; the solution in the kettle is removed, rectification is continued, and gas is collected; finally, all collected gas is dried through a molecular sieve, and cooling is performed. With the adoption of the production process, the cost is saved, the environment is prevented from being polluted, at the same time, the solvent is recycled, the molecular sieve is used for drying to control toluene moisture within 50 ppm and the toluene content to be 99.2%, side reaction is reduced during light feeding reaction, and 3% of conversion rate is improved.

Description

A kind of process for treating waste liquor of Diuron Tech
Technical field
The present invention relates to plastics fine chemistry industry production field, be specifically related to a kind of process for treating waste liquor of Diuron Tech.
Background technology
Diuron Tech is colorless crystalline solid, and fusing point 158 ~ 159 DEG C, is soluble in hot alcohol, and when 27 DEG C, solubleness is 5.3% in acetone, is slightly dissolved in vinyl acetic monomer, ethanol and hot benzene.Water insoluble, the 42ppm when solubleness in water is 25 DEG C.In hydro carbons, solubleness is low.To oxidation and hydrolysis-stable.Another name N-(3,4-dichlorophenyl)-N', N'-dimethyl urea N'-(3,4-dichlorophenyl)-N, N-dimethyl urea; 3-(3,4-dichlorophenyl)-1,1-dimethyl urea; For preventing and kill off the general weeds in noncrop area, anti-weeds spread again.These product are also for the weeding of asparagus, citrus, cotton, pineapple, sugarcane, temperate zone trees and shrub fruit, and its structural formula is:
In Diuron Tech production process, the waste liquid of generation contains the toxic substances such as toluene, if the waste that directly discharge one side causes enterprise to produce, also result in environmental pollution on the other hand.
Summary of the invention
For above problems of the prior art, the invention provides a kind of process for treating waste liquor of Diuron Tech, improve the recovery purity of toluene, save the cost of enterprise.
The present invention is achieved by the following technical solutions:
A process for treating waste liquor for Diuron Tech, its step is as follows:
1) quantitative toluene is squeezed in cold light still absorb a certain amount of phosgene, after up to standard by analysis, while lead to the 3,4-DCA toluene solution that plain edge drips metering in step 1, and keep pressure in cold light still all the time under negative pressure, temperature 70-75 DEG C;
2) continue logical photoresponse in the cold light still in step 1, and the time of continuing logical phosgene is 1.5-2h, stops stirring, the material of logical photoresponse, under maintenance negative pressure, proceeds to thermo-optical still, and thermo-optical still is slowly warming up to 80-90 DEG C, rear sampling clear;
3) material in step 2 is transferred in desolventizing still, and deviates from the phosgene toluene liquid in material;
4) the phosgene toluene liquid in step 3 is transferred in de-light still, and passes into nitrogen in de-light still, and constantly stir, and the temperature in de-light still is slowly warming up to 40-50 DEG C;
5) solution in light still de-in step 4 is transferred in one-level rectifying tower, the temperature of one-level rectifying tower is remained on 115-120 DEG C, collects gas; Again the solution of one-level rectifying tower is transferred in two-stage rectification tower, the temperature of two-stage rectification tower is remained on 121-125 DEG C, again collects gas, again the solution in two-stage rectification tower is transferred in three grades of rectifying tower, the temperature of three grades of rectifying tower is remained on 118-120 DEG C, again collects gas;
6) by step 5 collect all gas all carry out gas drying by molecular sieve, after be cooled to 30-50 DEG C, collect liquid.
Further, its step is as follows:
1) quantitative toluene is squeezed in cold light still absorb a certain amount of phosgene, after up to standard by analysis, while lead to the 3,4-DCA toluene solution that plain edge drips metering in step 1, and keep pressure in cold light still all the time under negative pressure, temperature 73 DEG C;
2) continue logical photoresponse in the cold light still in step 1, and the time of continuing logical phosgene is 1.8h, stops stirring, the material of logical photoresponse, under maintenance negative pressure, proceeds to thermo-optical still, and thermo-optical still is slowly warming up to 85 DEG C, rear sampling clear;
3) material in step 2 is transferred in desolventizing still, and deviates from the phosgene toluene liquid in material;
4) the phosgene toluene liquid in step 3 is transferred in de-light still, and passes into nitrogen in de-light still, and constantly stir, and the temperature in de-light still is slowly warming up to 45 DEG C;
5) solution in light still de-in step 4 is transferred in one-level rectifying tower, the temperature of one-level rectifying tower is remained on 118 DEG C, collects gas; Again the solution of one-level rectifying tower is transferred in two-stage rectification tower, the temperature of two-stage rectification tower is remained on 123 DEG C, again collects gas, again the solution in two-stage rectification tower is transferred in three grades of rectifying tower, the temperature of three grades of rectifying tower is remained on 120 DEG C, again collects gas;
6) by step 5 collect all gas all carry out gas drying by molecular sieve, after be cooled to 40 DEG C, collect liquid.
Beneficial effect of the present invention is: the present invention adopts above-mentioned production technique, improve the recovery purity of toluene, save the cost of enterprise, avoid in addition environment, recycling design toluene adopts continuous rectification to reclaim simultaneously, then makes toluene moisture control at below 50ppm by molecular sieve drying, and toluene level is 99.5%, make to decrease side reaction during logical photoresponse, improve the transformation efficiency of 3%.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Embodiment 1
First quantitative toluene is squeezed in cold light still and absorb a certain amount of phosgene, after up to standard by analysis, while lead to that plain edge drips metering in step 13,4-dichlorphenamide bulk powder toluene solution, and the pressure in maintenance cold light still is all the time under negative pressure, temperature 70 C, can improve the reaction efficiency of reactant;
Logical photoresponse will be continued again in cold light still in aforementioned, and the time of continuing logical phosgene is 1.5h, stop stirring, the material of logical photoresponse is under maintenance negative pressure, proceed to thermo-optical still, and thermo-optical still is slowly warming up to 80 DEG C, rear sampling clear, decrease the generation of side reaction, improve product purity;
Again the material in aforementioned is transferred in desolventizing still, and deviates from the phosgene toluene liquid in material, waste liquid can be deviate from, improve the purity of product;
Again the phosgene toluene liquid in aforementioned is transferred in de-light still, and passes into nitrogen in de-light still, and constantly stir, and the temperature in de-light still is slowly warming up to 40 DEG C, phosgene can be discharged, slowly heat up while constantly stirring, the phosgene in solution all can be discharged;
Again the solution in light still de-in aforementioned is transferred in one-level rectifying tower, the temperature of one-level rectifying tower is remained on 115 DEG C, collects gas; Again the solution of one-level rectifying tower is transferred in two-stage rectification tower, the temperature of two-stage rectification tower is remained on 125 DEG C, again collect gas, again the solution in two-stage rectification tower is transferred in three grades of rectifying tower, the temperature of three grades of rectifying tower is remained on 118 DEG C, again collect gas, continuous rectification makes the toluene in de-light still more thorough, adds the output of toluene;
Finally all gas of aforementioned middle collection is all carried out gas drying by molecular sieve, after be cooled to 30 DEG C, collect liquid, make toluene moisture control at below 50ppm, toluene level, 99.2%, makes to decrease side reaction during logical photoresponse, improves the transformation efficiency of 3%.
The present invention adopts above-mentioned production technique, improve the recovery purity of toluene, save the cost of enterprise, avoid in addition environment, recycling design toluene adopts continuous rectification to reclaim simultaneously, then makes toluene moisture control at below 50ppm by molecular sieve drying, and toluene level is 99.2%, make to decrease side reaction during logical photoresponse, improve the transformation efficiency of 3%.
Embodiment 2
First quantitative toluene is squeezed in cold light still and absorb a certain amount of phosgene, after up to standard by analysis, while lead to that plain edge drips metering in step 13,4-dichlorphenamide bulk powder toluene solution, and the pressure in maintenance cold light still is all the time under negative pressure, temperature 71 DEG C, can improve the reaction efficiency of reactant;
Logical photoresponse will be continued again in cold light still in aforementioned, and the time of continuing logical phosgene is 1.2h, stop stirring, the material of logical photoresponse is under maintenance negative pressure, proceed to thermo-optical still, and thermo-optical still is slowly warming up to 83 DEG C, rear sampling clear, decrease the generation of side reaction, improve product purity;
Again the material in aforementioned is transferred in desolventizing still, and deviates from the phosgene toluene liquid in material, waste liquid can be deviate from, improve the purity of product;
Again the phosgene toluene liquid in aforementioned is transferred in de-light still, and passes into nitrogen in de-light still, and constantly stir, and the temperature in de-light still is slowly warming up to 42 DEG C, phosgene can be discharged, slowly heat up while constantly stirring, the phosgene in solution all can be discharged;
Again the solution in light still de-in aforementioned is transferred in one-level rectifying tower, the temperature of one-level rectifying tower is remained on 117 DEG C, collects gas; Again the solution of one-level rectifying tower is transferred in two-stage rectification tower, the temperature of two-stage rectification tower is remained on 124 DEG C, again collect gas, again the solution in two-stage rectification tower is transferred in three grades of rectifying tower, the temperature of three grades of rectifying tower is remained on 119 DEG C, again collect gas, continuous rectification makes the toluene in de-light still more thorough, adds the output of toluene;
Finally all gas of aforementioned middle collection is all carried out gas drying by molecular sieve, after be cooled to 35 DEG C, collect liquid, make toluene moisture control at below 50ppm, toluene level, 99.4%, makes to decrease side reaction during logical photoresponse, improves the transformation efficiency of 3.2%.
The present invention adopts above-mentioned production technique, improve the recovery purity of toluene, save the cost of enterprise, avoid in addition environment, recycling design toluene adopts continuous rectification to reclaim simultaneously, then makes toluene moisture control at below 50ppm by molecular sieve drying, and toluene level is 99.4%, make to decrease side reaction during logical photoresponse, improve the transformation efficiency of 3.2%.
Embodiment 3
First quantitative toluene is squeezed in cold light still and absorb a certain amount of phosgene, after up to standard by analysis, while lead to that plain edge drips metering in step 13,4-dichlorphenamide bulk powder toluene solution, and the pressure in maintenance cold light still is all the time under negative pressure, temperature 73 DEG C, can improve the reaction efficiency of reactant;
Logical photoresponse will be continued again in cold light still in aforementioned, and the time of continuing logical phosgene is 1.8h, stop stirring, the material of logical photoresponse is under maintenance negative pressure, proceed to thermo-optical still, and thermo-optical still is slowly warming up to 85 DEG C, rear sampling clear, decrease the generation of side reaction, improve product purity;
Again the material in aforementioned is transferred in desolventizing still, and deviates from the phosgene toluene liquid in material, waste liquid can be deviate from, improve the purity of product;
Again the phosgene toluene liquid in aforementioned is transferred in de-light still, and passes into nitrogen in de-light still, and constantly stir, and the temperature in de-light still is slowly warming up to 45 DEG C, phosgene can be discharged, slowly heat up while constantly stirring, the phosgene in solution all can be discharged;
Again the solution in light still de-in aforementioned is transferred in one-level rectifying tower, the temperature of one-level rectifying tower is remained on 118 DEG C, collects gas; Again the solution of one-level rectifying tower is transferred in two-stage rectification tower, the temperature of two-stage rectification tower is remained on 123 DEG C, again collect gas, again the solution in two-stage rectification tower is transferred in three grades of rectifying tower, the temperature of three grades of rectifying tower is remained on 120 DEG C, again collect gas, continuous rectification makes the toluene in de-light still more thorough, adds the output of toluene;
Finally all gas of aforementioned middle collection is all carried out gas drying by molecular sieve, after be cooled to 40 DEG C, collect liquid, make toluene moisture control at below 50ppm, toluene level, 99.7%, makes to decrease side reaction during logical photoresponse, improves the transformation efficiency of 3.4%.
The present invention adopts above-mentioned production technique, improve the recovery purity of toluene, save the cost of enterprise, avoid in addition environment, recycling design toluene adopts continuous rectification to reclaim simultaneously, then makes toluene moisture control at below 50ppm by molecular sieve drying, and toluene level is 99.7%, make to decrease side reaction during logical photoresponse, improve the transformation efficiency of 3.4%.
Embodiment 4
First quantitative toluene is squeezed in cold light still and absorb a certain amount of phosgene, after up to standard by analysis, while lead to that plain edge drips metering in step 13,4-dichlorphenamide bulk powder toluene solution, and the pressure in maintenance cold light still is all the time under negative pressure, temperature 74 DEG C, can improve the reaction efficiency of reactant;
Logical photoresponse will be continued again in cold light still in aforementioned, and the time of continuing logical phosgene is 1.5h, stop stirring, the material of logical photoresponse is under maintenance negative pressure, proceed to thermo-optical still, and thermo-optical still is slowly warming up to 87 DEG C, rear sampling clear, decrease the generation of side reaction, improve product purity;
Again the material in aforementioned is transferred in desolventizing still, and deviates from the phosgene toluene liquid in material, waste liquid can be deviate from, improve the purity of product;
Again the phosgene toluene liquid in aforementioned is transferred in de-light still, and passes into nitrogen in de-light still, and constantly stir, and the temperature in de-light still is slowly warming up to 48 DEG C, phosgene can be discharged, slowly heat up while constantly stirring, the phosgene in solution all can be discharged;
Again the solution in light still de-in aforementioned is transferred in one-level rectifying tower, the temperature of one-level rectifying tower is remained on 119 DEG C, collects gas; Again the solution of one-level rectifying tower is transferred in two-stage rectification tower, the temperature of two-stage rectification tower is remained on 122 DEG C, again collect gas, again the solution in two-stage rectification tower is transferred in three grades of rectifying tower, the temperature of three grades of rectifying tower is remained on 119 DEG C, again collect gas, continuous rectification makes the toluene in de-light still more thorough, adds the output of toluene;
Finally all gas of aforementioned middle collection is all carried out gas drying by molecular sieve, after be cooled to 45 DEG C, collect liquid, make toluene moisture control at below 50ppm, toluene level, 98.9%, makes to decrease side reaction during logical photoresponse, improves the transformation efficiency of 3.5%.
The present invention adopts above-mentioned production technique, improve the recovery purity of toluene, save the cost of enterprise, avoid in addition environment, recycling design toluene adopts continuous rectification to reclaim simultaneously, then makes toluene moisture control at below 50ppm by molecular sieve drying, and toluene level is 98.9%, make to decrease side reaction during logical photoresponse, improve the transformation efficiency of 3.5%.
Embodiment 5
First quantitative toluene is squeezed in cold light still and absorb a certain amount of phosgene, after up to standard by analysis, while lead to that plain edge drips metering in step 13,4-dichlorphenamide bulk powder toluene solution, and the pressure in maintenance cold light still is all the time under negative pressure, temperature 75 DEG C, can improve the reaction efficiency of reactant;
Logical photoresponse will be continued again in cold light still in aforementioned, and the time of continuing logical phosgene is 2.0h, stop stirring, the material of logical photoresponse is under maintenance negative pressure, proceed to thermo-optical still, and thermo-optical still is slowly warming up to 90 DEG C, rear sampling clear, decrease the generation of side reaction, improve product purity;
Again the material in aforementioned is transferred in desolventizing still, and deviates from the phosgene toluene liquid in material, waste liquid can be deviate from, improve the purity of product;
Again the phosgene toluene liquid in aforementioned is transferred in de-light still, and passes into nitrogen in de-light still, and constantly stir, and the temperature in de-light still is slowly warming up to 50 DEG C, phosgene can be discharged, slowly heat up while constantly stirring, the phosgene in solution all can be discharged;
Again the solution in light still de-in aforementioned is transferred in one-level rectifying tower, the temperature of one-level rectifying tower is remained on 120 DEG C, collects gas; Again the solution of one-level rectifying tower is transferred in two-stage rectification tower, the temperature of two-stage rectification tower is remained on 121 DEG C, again collect gas, again the solution in two-stage rectification tower is transferred in three grades of rectifying tower, the temperature of three grades of rectifying tower is remained on 118 DEG C, again collect gas, continuous rectification makes the toluene in de-light still more thorough, adds the output of toluene;
Finally all gas of aforementioned middle collection is all carried out gas drying by molecular sieve, after be cooled to 50 DEG C, collect liquid, make toluene moisture control at below 50ppm, toluene level, 99.5%, makes to decrease side reaction during logical photoresponse, improves the transformation efficiency of 3.6%.
The present invention adopts above-mentioned production technique, improve the recovery purity of toluene, save the cost of enterprise, avoid in addition environment, recycling design toluene adopts continuous rectification to reclaim simultaneously, then makes toluene moisture control at below 50ppm by molecular sieve drying, and toluene level is 99.5%, make to decrease side reaction during logical photoresponse, improve the transformation efficiency of 3.6%.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.

Claims (2)

1. a process for treating waste liquor for Diuron Tech, is characterized in that: its step is as follows:
1) quantitative toluene is squeezed in cold light still absorb a certain amount of phosgene, after up to standard by analysis, while lead to the 3,4-DCA toluene solution that plain edge drips metering in step 1, and keep pressure in cold light still all the time under negative pressure, temperature 70-75 DEG C;
2) continue logical photoresponse in the cold light still in step 1, and the time of continuing logical phosgene is 1.5-2h, stops stirring, the material of logical photoresponse, under maintenance negative pressure, proceeds to thermo-optical still, and thermo-optical still is slowly warming up to 80-90 DEG C, rear sampling clear;
3) material in step 2 is transferred in desolventizing still, and deviates from the phosgene toluene liquid in material;
4) the phosgene toluene liquid in step 3 is transferred in de-light still, and passes into nitrogen in de-light still, and constantly stir, and the temperature in de-light still is slowly warming up to 40-50 DEG C;
5) solution in light still de-in step 4 is transferred in one-level rectifying tower, the temperature of one-level rectifying tower is remained on 115-120 DEG C, collects gas; Again the solution of one-level rectifying tower is transferred in two-stage rectification tower, the temperature of two-stage rectification tower is remained on 121-125 DEG C, again collects gas, again the solution in two-stage rectification tower is transferred in three grades of rectifying tower, the temperature of three grades of rectifying tower is remained on 118-120 DEG C, again collects gas;
6) by step 5 collect all gas all carry out gas drying by molecular sieve, after be cooled to 30-50 DEG C, collect liquid.
2. the process for treating waste liquor of a kind of Diuron Tech according to claim 1, is characterized in that: its step is as follows:
1) quantitative toluene is squeezed in cold light still absorb a certain amount of phosgene, after up to standard by analysis, while lead to the 3,4-DCA toluene solution that plain edge drips metering in step 1, and keep pressure in cold light still all the time under negative pressure, temperature 73 DEG C;
2) continue logical photoresponse in the cold light still in step 1, and the time of continuing logical phosgene is 1.8h, stops stirring, the material of logical photoresponse, under maintenance negative pressure, proceeds to thermo-optical still, and thermo-optical still is slowly warming up to 85 DEG C, rear sampling clear;
3) material in step 2 is transferred in desolventizing still, and deviates from the phosgene toluene liquid in material;
4) the phosgene toluene liquid in step 3 is transferred in de-light still, and passes into nitrogen in de-light still, and constantly stir, and the temperature in de-light still is slowly warming up to 45 DEG C;
5) solution in light still de-in step 4 is transferred in one-level rectifying tower, the temperature of one-level rectifying tower is remained on 118 DEG C, collects gas; Again the solution of one-level rectifying tower is transferred in two-stage rectification tower, the temperature of two-stage rectification tower is remained on 123 DEG C, again collects gas, again the solution in two-stage rectification tower is transferred in three grades of rectifying tower, the temperature of three grades of rectifying tower is remained on 120 DEG C, again collects gas;
6) by step 5 collect all gas all carry out gas drying by molecular sieve, after be cooled to 40 DEG C, collect liquid.
CN201510692496.8A 2015-10-20 2015-10-20 Diuron waste liquid treatment process Pending CN105254467A (en)

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Application Number Priority Date Filing Date Title
CN201510692496.8A CN105254467A (en) 2015-10-20 2015-10-20 Diuron waste liquid treatment process

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Publication Number Publication Date
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101709041A (en) * 2009-11-13 2010-05-19 安徽广信集团铜陵化工有限公司 Process for producing diuron
CN103739518A (en) * 2013-12-26 2014-04-23 安徽广信农化股份有限公司 Synthesis process for 2-hydroxybenzonitrile

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101709041A (en) * 2009-11-13 2010-05-19 安徽广信集团铜陵化工有限公司 Process for producing diuron
CN103739518A (en) * 2013-12-26 2014-04-23 安徽广信农化股份有限公司 Synthesis process for 2-hydroxybenzonitrile

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Application publication date: 20160120