CN105384641A - Wastewater treatment process for paranitrobenzoyl chloride - Google Patents
Wastewater treatment process for paranitrobenzoyl chloride Download PDFInfo
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- CN105384641A CN105384641A CN201510705643.0A CN201510705643A CN105384641A CN 105384641 A CN105384641 A CN 105384641A CN 201510705643 A CN201510705643 A CN 201510705643A CN 105384641 A CN105384641 A CN 105384641A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/12—Preparation of nitro compounds by reactions not involving the formation of nitro groups
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/20—Treatment of water, waste water, or sewage by degassing, i.e. liberation of dissolved gases
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a wastewater treatment process for paranitrobenzoyl chloride. The process comprises the following steps: adding a toluene solution into a reaction vessel, and introducing phosgene into the reaction vessel; dropwise adding paranitrobenzoic acid into the reaction vessel; introducing nitrogen gas into the solution in the reaction vessel for gas purging; transferring the solution subjected to gas purging into a rectifying still; and filtrating the cooled solution, and adding water into filtrated residue for flushing. The process has the beneficial effects that by adopting the production process, waste liquid can be further treated, and the product can be partially recovered, so that environmental pollution caused by direct discharge is avoided, and meanwhile, the yield of the product is increased.
Description
Technical field
The present invention relates to plastics fine chemistry industry production field, be specifically related to a kind of waste water treatment process of paranitrobenzoyl chloride.
Background technology
Paranitrobenzoyl chloride is a kind of medical raw material, is used for preparing vovocan, NSC 71042 and folic acid etc.; As dye material, substantive dyestuff palm fibre 100 can be prepared for leather and paper; Can also be used to manufacture matching stain, foodstuff additive (milk powder conditioning agent), color developer and organic synthesis intermediate, discriminating alcohol, phenol reagent etc.
Paranitrobenzoyl chloride is the important intermediate of the vitamins pharmaceutical prods such as synthesis folic acid, vovocan, N-p-benzoyl-Pidolidone, is also widely used in the production of pigment, color developer.Particularly in recent years, along with the rise of fodder industry and the development of information industry, the consumption of paranitrobenzoyl chloride is increasing;
The existing production technique of paranitrobenzoyl chloride is roughly following several: 1. carry out reacting with p-nitrobenzoic acid and phosgene and obtain; 2. be raw material with p-nitrobenzoic acid, react with phosphorus oxychloride (or phosphorus pentachloride) and prepare; 3. be raw material with p-nitrobenzoic acid, with sulfur oxychloride Reactive Synthesis under catalyst action.All exist certain not enough in existing several preparation method: if phosgene and phosphorus oxychloride are violent in toxicity, personal security and environment are easily worked the mischief; Phosphorus pentachloride is solid, need add solvent and just can add fast response, easily increases impurity and lock out operation; When taking sulfur oxychloride as chlorizating agent, the reaction times is longer, and needs strutting to distill removal of impurities, increases energy consumption etc.
Easily produce after producing waste liquid directly discharge can cause the solution of environment, and solution be difficult to degraded.
Summary of the invention
For above problems of the prior art, the invention provides a kind of waste water treatment process of paranitrobenzoyl chloride, avoid the environmental pollution of directly discharging and causing.
The present invention is achieved by the following technical solutions:
A waste water treatment process for paranitrobenzoyl chloride, its step is as follows:
1) add toluene solution by reactor, in reactor, pass into phosgene, and continue to pass into phosgene simultaneously; In reactor, drip p-nitrobenzoic acid, dropping limit, limit is stirred, and passes into phosgene simultaneously always, and the intake of phosgene is 1.0-1.5L/s, until the pH value extracting solution is 8-10, stops stirring, and stops passing into phosgene;
2) solution of reactor in step 1 is passed into nitrogen and catch up with gas, and the intake of nitrogen is 0.5-1.0L/s, and continuous stirred autoclave;
3) will the solution after gas in step 2, be caught up with to be transferred in rectifying still, temperature in rectifying still is remained on 115-120 DEG C, solution after rectifying catches up with gas again, and NaOH solution is added in solution, then after leaving standstill rectifying still, upper solution is transferred in cooling reactor, and by the greenhouse cooling of cooling reactor to 50-60 DEG C;
4) filtered by the solution after cooling, add water filter residue flushing, and carried out being heated to 100-108 DEG C by washing fluid.
Further, its step is as follows:
1) add toluene solution by reactor, in reactor, pass into phosgene, and continue to pass into phosgene simultaneously; In reactor, drip p-nitrobenzoic acid, dropping limit, limit is stirred, and passes into phosgene simultaneously always, and the intake of phosgene is 1.2L/s, until the pH value extracting solution is 10, stops stirring, and stops passing into phosgene;
2) solution of reactor in step 1 is passed into nitrogen and catch up with gas, and the intake of nitrogen is 0.8L/s, and continuous stirred autoclave;
3) will the solution after gas in step 2, be caught up with to be transferred in rectifying still, temperature in rectifying still is remained on 117 DEG C, solution after rectifying catches up with gas again, and NaOH solution is added in solution, then after leaving standstill rectifying still, upper solution is transferred in cooling reactor, and by the greenhouse cooling to 55 of cooling reactor DEG C;
4) filtered by the solution after cooling, add water filter residue flushing, and carried out being heated to 105 DEG C by washing fluid.
Further, the concentration of the NaOH solution of described step 3 is 15-25%.
Beneficial effect of the present invention is: the present invention adopts above-mentioned production technique, can be processed further by waste liquid, can carry out partially recycled product, therefore avoids directly discharging the environmental pollution caused, improves the output of product simultaneously.
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 add toluene solution by reactor, in reactor, pass into phosgene, and continue to pass into phosgene simultaneously; In reactor, drip p-nitrobenzoic acid, dropping limit, limit is stirred, and passes into phosgene simultaneously always, and the intake of phosgene is 1.0L/s, until the pH value extracting solution is 8, stop stirring, and stop passing into phosgene, can phosgene be dissolved in toluene solution, can increase the reaction efficiency of phosgene and remaining reaction thing like this, and avoid the danger such as the blast that direct reaction causes, dropwise reaction improves the efficiency of reaction, decrease the generation of side reaction, and reaction very easily controls;
Again the solution of reactor is passed into nitrogen and catch up with gas, and the intake of nitrogen is 0.5L/s, and continuous stirred autoclave, tail gas in reaction product can be driven out of, improve the purity of product, the pollution of the environment also avoiding the volatilizations such as phosgene to cause;
To the solution after gas be caught up with to be transferred in rectifying still again, temperature in rectifying still is remained on 115 DEG C, solution after rectifying catches up with gas again, and NaOH solution is added in solution, the concentration of NaOH solution is 15%, after then leaving standstill rectifying still, upper solution is transferred in cooling reactor, and by the greenhouse cooling to 50 of cooling reactor DEG C, improve the precision of product, and waste liquid can process further;
Finally the solution after cooling is filtered, add water filter residue flushing, and washing fluid is carried out being heated to 100 DEG C, tar-like substance in waste liquid can filter out by filtration, and is rinsed through water by filter residue, the filtrate remained is rinsed out in filter residue, then evaporative crystallization again, can partially recycled product be carried out, therefore avoid directly discharging the environmental pollution caused, improve the output of product simultaneously.
The present invention adopts above-mentioned production technique, can be processed further by waste liquid, can carry out partially recycled product, therefore avoids directly discharging the environmental pollution caused, improves the output of product simultaneously.
Embodiment 2
First add toluene solution by reactor, in reactor, pass into phosgene, and continue to pass into phosgene simultaneously; In reactor, drip p-nitrobenzoic acid, dropping limit, limit is stirred, and passes into phosgene simultaneously always, and the intake of phosgene is 1.1L/s, until the pH value extracting solution is 9, stop stirring, and stop passing into phosgene, can phosgene be dissolved in toluene solution, can increase the reaction efficiency of phosgene and remaining reaction thing like this, and avoid the danger such as the blast that direct reaction causes, dropwise reaction improves the efficiency of reaction, decrease the generation of side reaction, and reaction very easily controls;
Again the solution of reactor is passed into nitrogen and catch up with gas, and the intake of nitrogen is 0.6L/s, and continuous stirred autoclave, tail gas in reaction product can be driven out of, improve the purity of product, the pollution of the environment also avoiding the volatilizations such as phosgene to cause;
To the solution after gas be caught up with to be transferred in rectifying still again, temperature in rectifying still is remained on 116 DEG C, solution after rectifying catches up with gas again, and NaOH solution is added in solution, the concentration of NaOH solution is 18%, after then leaving standstill rectifying still, upper solution is transferred in cooling reactor, and by the greenhouse cooling to 53 of cooling reactor DEG C, improve the precision of product, and waste liquid can process further;
Finally the solution after cooling is filtered, add water filter residue flushing, and washing fluid is carried out being heated to 104 DEG C, tar-like substance in waste liquid can filter out by filtration, and is rinsed through water by filter residue, the filtrate remained is rinsed out in filter residue, then evaporative crystallization again, can partially recycled product be carried out, therefore avoid directly discharging the environmental pollution caused, improve the output of product simultaneously.
The present invention adopts above-mentioned production technique, can be processed further by waste liquid, can carry out partially recycled product, therefore avoids directly discharging the environmental pollution caused, improves the output of product simultaneously.
Embodiment 3
First add toluene solution by reactor, in reactor, pass into phosgene, and continue to pass into phosgene simultaneously; In reactor, drip p-nitrobenzoic acid, dropping limit, limit is stirred, and passes into phosgene simultaneously always, and the intake of phosgene is 1.2L/s, until the pH value extracting solution is 10, stop stirring, and stop passing into phosgene, can phosgene be dissolved in toluene solution, can increase the reaction efficiency of phosgene and remaining reaction thing like this, and avoid the danger such as the blast that direct reaction causes, dropwise reaction improves the efficiency of reaction, decrease the generation of side reaction, and reaction very easily controls;
Again the solution of reactor is passed into nitrogen and catch up with gas, and the intake of nitrogen is 0.8L/s, and continuous stirred autoclave, tail gas in reaction product can be driven out of, improve the purity of product, the pollution of the environment also avoiding the volatilizations such as phosgene to cause;
To the solution after gas be caught up with to be transferred in rectifying still again, temperature in rectifying still is remained on 117 DEG C, solution after rectifying catches up with gas again, and NaOH solution is added in solution, the concentration of NaOH solution is 20%, after then leaving standstill rectifying still, upper solution is transferred in cooling reactor, and by the greenhouse cooling to 55 of cooling reactor DEG C, improve the precision of product, and waste liquid can process further;
Finally the solution after cooling is filtered, add water filter residue flushing, and washing fluid is carried out being heated to 105 DEG C, tar-like substance in waste liquid can filter out by filtration, and is rinsed through water by filter residue, the filtrate remained is rinsed out in filter residue, then evaporative crystallization again, can partially recycled product be carried out, therefore avoid directly discharging the environmental pollution caused, improve the output of product simultaneously.
The present invention adopts above-mentioned production technique, can be processed further by waste liquid, can carry out partially recycled product, therefore avoids directly discharging the environmental pollution caused, improves the output of product simultaneously.
Embodiment 4
First add toluene solution by reactor, in reactor, pass into phosgene, and continue to pass into phosgene simultaneously; In reactor, drip p-nitrobenzoic acid, dropping limit, limit is stirred, and passes into phosgene simultaneously always, and the intake of phosgene is 1.3L/s, until the pH value extracting solution is 10, stop stirring, and stop passing into phosgene, can phosgene be dissolved in toluene solution, can increase the reaction efficiency of phosgene and remaining reaction thing like this, and avoid the danger such as the blast that direct reaction causes, dropwise reaction improves the efficiency of reaction, decrease the generation of side reaction, and reaction very easily controls;
Again the solution of reactor is passed into nitrogen and catch up with gas, and the intake of nitrogen is 0.9L/s, and continuous stirred autoclave, tail gas in reaction product can be driven out of, improve the purity of product, the pollution of the environment also avoiding the volatilizations such as phosgene to cause;
To the solution after gas be caught up with to be transferred in rectifying still again, temperature in rectifying still is remained on 119 DEG C, solution after rectifying catches up with gas again, and NaOH solution is added in solution, the concentration of NaOH solution is 22%, after then leaving standstill rectifying still, upper solution is transferred in cooling reactor, and by the greenhouse cooling to 57 of cooling reactor DEG C, improve the precision of product, and waste liquid can process further;
Finally the solution after cooling is filtered, add water filter residue flushing, and washing fluid is carried out being heated to 106 DEG C, tar-like substance in waste liquid can filter out by filtration, and is rinsed through water by filter residue, the filtrate remained is rinsed out in filter residue, then evaporative crystallization again, can partially recycled product be carried out, therefore avoid directly discharging the environmental pollution caused, improve the output of product simultaneously.
The present invention adopts above-mentioned production technique, can be processed further by waste liquid, can carry out partially recycled product, therefore avoids directly discharging the environmental pollution caused, improves the output of product simultaneously.
Embodiment 5
First add toluene solution by reactor, in reactor, pass into phosgene, and continue to pass into phosgene simultaneously; In reactor, drip p-nitrobenzoic acid, dropping limit, limit is stirred, and passes into phosgene simultaneously always, and the intake of phosgene is 1.5L/s, until the pH value extracting solution is 9, stop stirring, and stop passing into phosgene, can phosgene be dissolved in toluene solution, can increase the reaction efficiency of phosgene and remaining reaction thing like this, and avoid the danger such as the blast that direct reaction causes, dropwise reaction improves the efficiency of reaction, decrease the generation of side reaction, and reaction very easily controls;
Again the solution of reactor is passed into nitrogen and catch up with gas, and the intake of nitrogen is 1.0L/s, and continuous stirred autoclave, tail gas in reaction product can be driven out of, improve the purity of product, the pollution of the environment also avoiding the volatilizations such as phosgene to cause;
To the solution after gas be caught up with to be transferred in rectifying still again, temperature in rectifying still is remained on 120 DEG C, solution after rectifying catches up with gas again, and NaOH solution is added in solution, the concentration of NaOH solution is 25%, after then leaving standstill rectifying still, upper solution is transferred in cooling reactor, and by the greenhouse cooling to 60 of cooling reactor DEG C, improve the precision of product, and waste liquid can process further;
Finally the solution after cooling is filtered, add water filter residue flushing, and washing fluid is carried out being heated to 108 DEG C, tar-like substance in waste liquid can filter out by filtration, and is rinsed through water by filter residue, the filtrate remained is rinsed out in filter residue, then evaporative crystallization again, can partially recycled product be carried out, therefore avoid directly discharging the environmental pollution caused, improve the output of product simultaneously.
The present invention adopts above-mentioned production technique, can be processed further by waste liquid, can carry out partially recycled product, therefore avoids directly discharging the environmental pollution caused, improves the output of product simultaneously.
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 (3)
1. a waste water treatment process for paranitrobenzoyl chloride, is characterized in that: its step is as follows:
1) add toluene solution by reactor, in reactor, pass into phosgene, and continue to pass into phosgene simultaneously; In reactor, drip p-nitrobenzoic acid, dropping limit, limit is stirred, and passes into phosgene simultaneously always, and the intake of phosgene is 1.0-1.5L/s, until the pH value extracting solution is 8-10, stops stirring, and stops passing into phosgene;
2) solution of reactor in step 1 is passed into nitrogen and catch up with gas, and the intake of nitrogen is 0.5-1.0L/s, and continuous stirred autoclave;
3) will the solution after gas in step 2, be caught up with to be transferred in rectifying still, temperature in rectifying still is remained on 115-120 DEG C, solution after rectifying catches up with gas again, and NaOH solution is added in solution, then after leaving standstill rectifying still, upper solution is transferred in cooling reactor, and by the greenhouse cooling of cooling reactor to 50-60 DEG C;
4) filtered by the solution after cooling, add water filter residue flushing, and carried out being heated to 100-108 DEG C by washing fluid.
2. the waste water treatment process of a kind of paranitrobenzoyl chloride according to claim 1, is characterized in that: its step is as follows:
1) add toluene solution by reactor, in reactor, pass into phosgene, and continue to pass into phosgene simultaneously; In reactor, drip p-nitrobenzoic acid, dropping limit, limit is stirred, and passes into phosgene simultaneously always, and the intake of phosgene is 1.2L/s, until the pH value extracting solution is 10, stops stirring, and stops passing into phosgene;
2) solution of reactor in step 1 is passed into nitrogen and catch up with gas, and the intake of nitrogen is 0.8L/s, and continuous stirred autoclave;
3) will the solution after gas in step 2, be caught up with to be transferred in rectifying still, temperature in rectifying still is remained on 117 DEG C, solution after rectifying catches up with gas again, and NaOH solution is added in solution, then after leaving standstill rectifying still, upper solution is transferred in cooling reactor, and by the greenhouse cooling to 55 of cooling reactor DEG C;
4) filtered by the solution after cooling, add water filter residue flushing, and carried out being heated to 105 DEG C by washing fluid.
3. the waste water treatment process of a kind of paranitrobenzoyl chloride according to claim 1 and 2, is characterized in that: the concentration of the NaOH solution of described step 3 is 15-25%.
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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 |
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2015
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JPH09323953A (en) * | 1996-02-29 | 1997-12-16 | Rhone Poulenc Agrochim | Phosgenation of acid and/or acid anhydride under pressure for preparation of acid chloride |
CN1562946A (en) * | 2004-03-17 | 2005-01-12 | 烟台万华聚氨酯股份有限公司 | Method for preparing m-phthaloyl chloride in high purity |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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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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