CN105016544A - Hydroxy-benzonitril waste water processing technology - Google Patents
Hydroxy-benzonitril waste water processing technology Download PDFInfo
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- CN105016544A CN105016544A CN201510381162.9A CN201510381162A CN105016544A CN 105016544 A CN105016544 A CN 105016544A CN 201510381162 A CN201510381162 A CN 201510381162A CN 105016544 A CN105016544 A CN 105016544A
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Abstract
The invention provides a hydroxy-benzonitril waste water processing technology, which is characterized in that solid state salicylamide with concentration being 95-99% and liquid state xylene with solvent concentration being 95-99.5% are added in a slurry configuration kettle, stirring and dissolving; placing the configured material in the slurry configuration kettle in a photochemical reaction kettle, opening a steam jacket and heating, controlling the reaction vessel and introducing phosgene for a photochemical reaction, after the reaction is complete, introducing nitrogen for expelling bubble, adding liquid alkali and a phase-transfer catalyst in the reaction vessel, heating and fully stirring, conversing the waste water after water diversion to an extraction kettle with a preset solvent, adding liquid alkali for processing, and performing secondary water diversion. According to the invention, material recovery in waste water can be effectively carried out through liquid alkali processing and solvent extraction, waste water volume during whole synthesis can be simultaneously reduced, 500kg of waste water can be reduced in each ton of material, 50kg of material can be extracted in each ton of waste water, and each 100 tons of material can provide three hundred thousand profit for company.
Description
Technical field
The present invention relates to the production field of agricultural chemicals, be specifically related to a kind of waste water treatment process of salicylonitrile.
Background technology
Salicylonitrile, Chinese another name: salicylonitrile; 2-cyanophenol; 2-4-hydroxy-benzonitrile; O-hydroxy nitrile; Adjacent cyano group phenol, physico-chemical property: crystallization.Fusing point 92-95 DEG C (102-102.5 DEG C), the greyish white toner pulverulent solids of boiling point 149 DEG C/1.9kPa (14mmHg), has irritating smell, people can be allowed on a small quantity to breathe and be affected, and smell is pained.If opened wide by a small amount of salicylonitrile without under ventilation state, smell can spread all over rapidly whole indoor.Therefore the measure that must properly protect during operation, reduce the stimulation to respiratory tract.As intermediate, the sterilant azoxystrobin intermediate of organic synthesis bunitrolol.
Waste water after original salicylonitrile synthesis is directly transported to sewage work of company without workshop process and directly processes.Through the research of repetitious pilot plant test and large production test, finally explore a feasible treatment process route.
Summary of the invention
For above problems of the prior art, the invention provides a kind of waste water treatment process of salicylonitrile, effectively the material in waste water is reclaimed.
The present invention is achieved by the following technical solutions:
Concentration is first the solid-state salicylic amide of 95-99% and solvent strength by a waste water treatment process for salicylonitrile is that the liquid dimethyl benzene of 95-99.5% adds in slurry configuration still, opens stirring and dissolves, again slurry is configured the material configured in still and put into photochmeical reaction still, open jacket steam to heat, controlling temperature of reaction kettle, 90 ~ 100 DEG C time, pass into volumetric concentration be that the phosgene of 65-75V/V carries out photochmeical reaction, reaction end passes into concentration >=99% nitrogen and carries out catching up with gas, liquid caustic soda and phase-transfer catalyst is added again in reactor, through heating up, and temperature rises to 90-100 DEG C, abundant stirring, be cooled to 50-60 DEG C and carry out a point water, dividing the waste water after water to go to has stayed in the extraction kettle of solvent in advance, add the liquid caustic soda process of 90-110KG, be warming up to 70-80 DEG C, leave standstill 5-10h, carry out secondary again and divide water.
Further, by concentration be first 99% solid-state salicylic amide and solvent strength be 99.5% liquid dimethyl benzene add slurry configuration still in, open stirring dissolve, again slurry is configured the material configured in still and put into photochmeical reaction still, open jacket steam to heat, controlling temperature of reaction kettle, 95 DEG C time, pass into volumetric concentration be that the phosgene of 75V/V carries out photochmeical reaction, reaction end passes into concentration >=99% nitrogen and carries out catching up with gas, liquid caustic soda and phase-transfer catalyst is added again in reactor, through heating up, and temperature rises to 90 DEG C, abundant stirring, be cooled to 60 DEG C and carry out a point water, dividing the waste water after water to go to has stayed in the extraction kettle of solvent in advance, add the liquid caustic soda process of 110KG, be warming up to 80 DEG C, leave standstill 7h, carry out secondary again and divide water.
Wherein reaction equation is as follows:
Main reaction:
Side reaction:
Beneficial effect of the present invention is: by this liquid caustic soda process, solvent extraction, effectively the material in waste water is reclaimed, decrease the wastewater flow rate of whole synthesis simultaneously, namely average material per ton reduces about 500kg waste water, waste water per ton extracts about 50kg material, and the every 100 tons of materials of COMPREHENSIVE CALCULATING are the profit that company brings 300,000 yuan.
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
A waste water treatment process for salicylonitrile, by concentration be first 95% solid-state salicylic amide and solvent strength be 95% liquid dimethyl benzene add slurry configuration still in, open stirring dissolve, again slurry is configured the material configured in still and put into photochmeical reaction still, open jacket steam to heat, controlling temperature of reaction kettle, 90 DEG C time, pass into volumetric concentration be that the phosgene of 65V/V carries out photochmeical reaction, reaction end passes into concentration >=99% nitrogen and carries out catching up with gas, liquid caustic soda and phase-transfer catalyst is added again in reactor, through heating up, and temperature rises to 90 DEG C, abundant stirring, be cooled to 50 DEG C and carry out a point water, dividing the waste water after water to go to has stayed in the extraction kettle of solvent in advance, add the liquid caustic soda process of 90KG, be warming up to 70 DEG C, leave standstill 5h, carry out secondary again and divide water, by this liquid caustic soda process, solvent extraction, effectively the material in waste water is reclaimed, decrease the wastewater flow rate of whole synthesis simultaneously, namely average material per ton reduces about 500kg waste water, waste water per ton extracts about 50kg material, and the every 100 tons of materials of COMPREHENSIVE CALCULATING are the profit that company brings 300,000 yuan.
Embodiment 2
A waste water treatment process for salicylonitrile, by concentration be first 99% solid-state salicylic amide and solvent strength be 99.5% liquid dimethyl benzene add slurry configuration still in, open stirring dissolve, again slurry is configured the material configured in still and put into photochmeical reaction still, open jacket steam to heat, controlling temperature of reaction kettle, 100 DEG C time, pass into volumetric concentration be that the phosgene of 75V/V carries out photochmeical reaction, reaction end passes into concentration >=99% nitrogen and carries out catching up with gas, liquid caustic soda and phase-transfer catalyst is added again in reactor, through heating up, and temperature rises to 90 DEG C, abundant stirring, be cooled to 60 DEG C and carry out a point water, dividing the waste water after water to go to has stayed in the extraction kettle of solvent in advance, add the liquid caustic soda process of 94KG, be warming up to 72 DEG C, leave standstill 6h, carry out secondary again and divide water, by this liquid caustic soda process, solvent extraction, effectively the material in waste water is reclaimed, decrease the wastewater flow rate of whole synthesis simultaneously, namely average material per ton reduces about 500kg waste water, waste water per ton extracts about 50kg material, and the every 100 tons of materials of COMPREHENSIVE CALCULATING are the profit that company brings 300,000 yuan.
Embodiment 3
A waste water treatment process for salicylonitrile, by concentration be first 96% solid-state salicylic amide and solvent strength be 97% liquid dimethyl benzene add slurry configuration still in, open stirring dissolve, again slurry is configured the material configured in still and put into photochmeical reaction still, open jacket steam to heat, controlling temperature of reaction kettle, 93 DEG C time, pass into volumetric concentration be that the phosgene of 75V/V carries out photochmeical reaction, reaction end passes into concentration >=99% nitrogen and carries out catching up with gas, liquid caustic soda and phase-transfer catalyst is added again in reactor, through heating up, and temperature rises to 100 DEG C, abundant stirring, be cooled to 55 DEG C and carry out a point water, dividing the waste water after water to go to has stayed in the extraction kettle of solvent in advance, add the liquid caustic soda process of 98KG, be warming up to 74 DEG C, leave standstill 7h, carry out secondary again and divide water, by this liquid caustic soda process, solvent extraction, effectively the material in waste water is reclaimed, decrease the wastewater flow rate of whole synthesis simultaneously, namely average material per ton reduces about 500kg waste water, waste water per ton extracts about 50kg material, and the every 100 tons of materials of COMPREHENSIVE CALCULATING are the profit that company brings 300,000 yuan.
Embodiment 4
A waste water treatment process for salicylonitrile, by concentration be first 98% solid-state salicylic amide and solvent strength be 99.5% liquid dimethyl benzene add slurry configuration still in, open stirring dissolve, again slurry is configured the material configured in still and put into photochmeical reaction still, open jacket steam to heat, controlling temperature of reaction kettle, 95 DEG C time, pass into volumetric concentration be that the phosgene of 69V/V carries out photochmeical reaction, reaction end passes into concentration >=99% nitrogen and carries out catching up with gas, liquid caustic soda and phase-transfer catalyst is added again in reactor, through heating up, and temperature rises to 97 DEG C, abundant stirring, be cooled to 60 DEG C and carry out a point water, dividing the waste water after water to go to has stayed in the extraction kettle of solvent in advance, add the liquid caustic soda process of 100KG, be warming up to 76 DEG C, leave standstill 8h, carry out secondary again and divide water, by this liquid caustic soda process, solvent extraction, effectively the material in waste water is reclaimed, decrease the wastewater flow rate of whole synthesis simultaneously, namely average material per ton reduces about 500kg waste water, waste water per ton extracts about 50kg material, and the every 100 tons of materials of COMPREHENSIVE CALCULATING are the profit that company brings 300,000 yuan.
Embodiment 5
A waste water treatment process for salicylonitrile, by concentration be first 96% solid-state salicylic amide and solvent strength be 99.5% liquid dimethyl benzene add slurry configuration still in, open stirring dissolve, again slurry is configured the material configured in still and put into photochmeical reaction still, open jacket steam to heat, controlling temperature of reaction kettle, 99 DEG C time, pass into volumetric concentration be that the phosgene of 75V/V carries out photochmeical reaction, reaction end passes into concentration >=99% nitrogen and carries out catching up with gas, liquid caustic soda and phase-transfer catalyst is added again in reactor, through heating up, and temperature rises to 98 DEG C, abundant stirring, be cooled to 60 DEG C and carry out a point water, dividing the waste water after water to go to has stayed in the extraction kettle of solvent in advance, add the liquid caustic soda process of 105KG, be warming up to 78 DEG C, leave standstill 9h, carry out secondary again and divide water, by this liquid caustic soda process, solvent extraction, effectively the material in waste water is reclaimed, decrease the wastewater flow rate of whole synthesis simultaneously, namely average material per ton reduces about 500kg waste water, waste water per ton extracts about 50kg material, and the every 100 tons of materials of COMPREHENSIVE CALCULATING are the profit that company brings 300,000 yuan.
Embodiment 6
A waste water treatment process for salicylonitrile, by concentration be first 99% solid-state salicylic amide and solvent strength be 98% liquid dimethyl benzene add slurry configuration still in, open stirring dissolve, again slurry is configured the material configured in still and put into photochmeical reaction still, open jacket steam to heat, controlling temperature of reaction kettle, 99 DEG C time, pass into volumetric concentration be that the phosgene of 75V/V carries out photochmeical reaction, reaction end passes into concentration >=99% nitrogen and carries out catching up with gas, liquid caustic soda and phase-transfer catalyst is added again in reactor, through heating up, and temperature rises to 95 DEG C, abundant stirring, be cooled to 59 DEG C and carry out a point water, dividing the waste water after water to go to has stayed in the extraction kettle of solvent in advance, add the liquid caustic soda process of 110KG, be warming up to 80 DEG C, leave standstill 10h, carry out secondary again and divide water, by this liquid caustic soda process, solvent extraction, effectively the material in waste water is reclaimed, decrease the wastewater flow rate of whole synthesis simultaneously, namely average material per ton reduces about 500kg waste water, waste water per ton extracts about 50kg material, and the every 100 tons of materials of COMPREHENSIVE CALCULATING are the profit that company brings 300,000 yuan.
Embodiment 7
By concentration be first 99% solid-state salicylic amide and solvent strength be 99.5% liquid dimethyl benzene add slurry configuration still in, open stirring dissolve, again slurry is configured the material configured in still and put into photochmeical reaction still, open jacket steam to heat, controlling temperature of reaction kettle, 95 DEG C time, pass into volumetric concentration be that the phosgene of 75V/V carries out photochmeical reaction, reaction end passes into concentration >=99% nitrogen and carries out catching up with gas, liquid caustic soda and phase-transfer catalyst is added again in reactor, through heating up, and temperature rises to 90 DEG C, abundant stirring, be cooled to 60 DEG C and carry out a point water, dividing the waste water after water to go to has stayed in the extraction kettle of solvent in advance, add the liquid caustic soda process of 110KG, be warming up to 80 DEG C, leave standstill 7h, carry out secondary again and divide water, by this liquid caustic soda process, solvent extraction, effectively the material in waste water is reclaimed, decrease the wastewater flow rate of whole synthesis simultaneously, namely average material per ton reduces about 500kg waste water, waste water per ton extracts about 50kg material, the every 100 tons of materials of COMPREHENSIVE CALCULATING are the profit that company brings 300,000 yuan.
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 waste water treatment process for salicylonitrile, is characterized in that: the liquid dimethyl benzene of to be first the solid-state salicylic amide of 95-99% and solvent strength by concentration be 95-99.5% adds in slurry configuration still, opens stirring and dissolves, again slurry is configured the material configured in still and put into photochmeical reaction still, open jacket steam to heat, controlling temperature of reaction kettle, 90 ~ 100 DEG C time, pass into volumetric concentration be that the phosgene of 65-75V/V carries out photochmeical reaction, reaction end passes into concentration >=99% nitrogen and carries out catching up with gas, liquid caustic soda and phase-transfer catalyst is added again in reactor, through heating up, and temperature rises to 90-100 DEG C, abundant stirring, be cooled to 50-60 DEG C and carry out a point water, dividing the waste water after water to go to has stayed in the extraction kettle of solvent in advance, add the liquid caustic soda process of 90-110KG, be warming up to 70-80 DEG C, leave standstill 5-10h, carry out secondary again and divide water.
2. the waste water treatment process of a kind of salicylonitrile according to claim 1, is characterized in that: by concentration be first 99% solid-state salicylic amide and solvent strength be 99.5% liquid dimethyl benzene add slurry configuration still in, open stirring dissolve, again slurry is configured the material configured in still and put into photochmeical reaction still, open jacket steam to heat, controlling temperature of reaction kettle, 95 DEG C time, pass into volumetric concentration be that the phosgene of 75V/V carries out photochmeical reaction, reaction end passes into concentration >=99% nitrogen and carries out catching up with gas, liquid caustic soda and phase-transfer catalyst is added again in reactor, through heating up, and temperature rises to 90 DEG C, abundant stirring, be cooled to 60 DEG C and carry out a point water, dividing the waste water after water to go to has stayed in the extraction kettle of solvent in advance, add the liquid caustic soda process of 110KG, be warming up to 80 DEG C, leave standstill 7h, carry out secondary again and divide water.
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| CN201510381162.9A CN105016544A (en) | 2015-06-29 | 2015-06-29 | Hydroxy-benzonitril waste water processing technology |
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| CN201510381162.9A CN105016544A (en) | 2015-06-29 | 2015-06-29 | Hydroxy-benzonitril waste water processing technology |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108558704A (en) * | 2018-05-29 | 2018-09-21 | 安徽广信农化股份有限公司 | A kind of process of methyl carbamate wastewater treatment |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN204017827U (en) * | 2014-06-10 | 2014-12-17 | 安徽广信农化股份有限公司 | A kind of pretreatment unit for salicylonitrile solvent recovery |
| CN204364918U (en) * | 2014-12-02 | 2015-06-03 | 安徽东至广信农化有限公司 | A kind of salicylonitrile production rectifying column |
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- 2015-06-29 CN CN201510381162.9A patent/CN105016544A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN204017827U (en) * | 2014-06-10 | 2014-12-17 | 安徽广信农化股份有限公司 | A kind of pretreatment unit for salicylonitrile solvent recovery |
| CN204364918U (en) * | 2014-12-02 | 2015-06-03 | 安徽东至广信农化有限公司 | A kind of salicylonitrile production rectifying column |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108558704A (en) * | 2018-05-29 | 2018-09-21 | 安徽广信农化股份有限公司 | A kind of process of methyl carbamate wastewater treatment |
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Application publication date: 20151104 |