CN109748443B - Treatment process of waste liquid generated in synthesis of 4, 6-dichloropyrimidine - Google Patents
Treatment process of waste liquid generated in synthesis of 4, 6-dichloropyrimidine Download PDFInfo
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Abstract
The invention discloses a process for treating waste liquid generated in synthesis of 4, 6-dichloropyrimidine, which comprises the following steps: collecting wastewater of the washing kettle, adjusting the pH value of the wastewater, evaporating and drying the wastewater to obtain crystals; collecting dangerous waste in a rectifying still for vacuum rectification, alkalifying residual alkali, reacidifying solid, washing with hot water and drying; acidifying the alkalized waste liquid, centrifuging, drying and collecting; the method carries out operations such as PH adjustment, evaporation, centrifugation, drying and the like after collecting the 4, 6-dichloropyrimidine synthesis waste liquid, timely collects and recycles useful components in the waste liquid, reduces toxic components in the waste liquid, avoids directly causing pollution and damage to the environment, reduces the synthesis production cost, improves the economic benefit, and has the advantages that the content of 4, 6-dihydroxypyrimidine in the waste water discharged by detection is less than or equal to 0.01 percent, the content of phosphide is less than or equal to 0.005 percent, the content of chloride ions is less than or equal to 0.001 percent, and the content of 4, 6-dichloropyrimidine is less than or equal to 0.008 percent.
Description
Technical Field
The invention relates to the technical field of organic synthesis post-treatment, in particular to a treatment process of waste liquid generated in synthesis of 4, 6-dichloropyrimidine.
Background
The pyrimidine compounds are heterocyclic compounds containing nitrogen elements, have specific properties due to the special structures, have certain effects of resisting fungi and regulating and promoting plant growth, and can be widely used for preparing herbicides, insecticides, bactericides and other chemicals. The pyrimidine compounds and metal ions can form complexes, so that the continuity of the original medicine can be improved, the increase of the effective period and the half-life period can be prolonged, and the toxicity to animals can be effectively reduced.
4, 6-dichloropyrimidine is a heterocyclic compound containing nitrogen elements, is one of important intermediates for synthesizing pyrimidine compounds, is widely applied to synthesis of medical products and pesticide pyrimidine products, and is representative of sulfonamides such as sulfametoxin and sulfanilamide-6-methoxypyrimidine, and 4, 6-dichloropyrimidine is a typical intermediate of the sulfonamides. As can be seen from the important roles of 4, 6-dichloropyrimidine in various fields, the market demand for 4, 6-dichloropyrimidine and 4, 6-dihydroxypyrimidine serving as a raw material thereof is increased continuously in a short time, and the industrial production of 4, 6-dichloropyrimidine is steadily increased.
The waste liquid generated in the synthesis process of 4, 6-dichloropyrimidine contains part of substances which can be recycled and also contains some toxic substances, and if the waste liquid is directly discharged into the environment, serious pollution and damage can be caused, and if the waste liquid in the synthesis process is treated, the problem which needs to be solved by people in the related technical field at present needs to be solved.
Disclosure of Invention
In order to solve the problems, the invention aims to recover useful components from the waste liquid generated in the synthesis process of the 4, 6-dichloropyrimidine, reduce the content of organic matters and toxic substances in the waste liquid, improve the economic benefit and reduce the production cost.
In order to realize the purpose of the invention, the adopted technical scheme is as follows: a waste liquid treatment process for synthesizing 4, 6-dichloropyrimidine comprises the following specific steps:
1) adjusting the pH value: collecting the lower-layer wastewater of a washing kettle for synthesizing 4, 6-dichloropyrimidine in a pH adjusting tank, dropwise adding dilute acid, starting stirring, monitoring the pH in the wastewater in time, stopping dropwise adding the dilute acid when the pH of the wastewater is 6.8-7.5, continuously stirring for 10-15 min, and transferring the wastewater after pH adjustment to an evaporation kettle;
2) evaporation: starting a vacuum system on an evaporation kettle, controlling the vacuum system to vacuumize to be more than-0.097 MPa, heating to 60-90 ℃, distilling water in the wastewater out of 1/2-2/3, cooling to normal temperature, adding an ethanol solution which is 2-5 times of the volume of the residual wastewater into the evaporation kettle, heating to 60-90 ℃ again, evaporating the wastewater until part of crystals are exposed, stopping heating, evaporating the residual solvent by using waste heat to obtain crystals, and drying the crystals in an oven at 60-90 ℃ to sell the crystals as byproducts;
3) distillation: collecting hazardous waste of a rectifying kettle for synthesizing 4, 6-dichloropyrimidine, starting a vacuum system on the distilling kettle, controlling the vacuum system to vacuumize to be more than-0.097 MPa, raising the temperature to 30-80 ℃, condensing and collecting distilled fractions, and transferring residue at the bottom of the kettle to an alkalization kettle after the fractions are completely evaporated;
4) alkalization: adding a hot alkali solution with the temperature of 50-60 ℃ into an alkalization kettle, starting stirring, heating the alkalization kettle to 50-60 ℃, stopping stirring when the residual solid is not dissolved any more, standing for layering, transferring an upper water layer into an acidification kettle, washing a lower solid layer for 2-3 times by using hot water with the temperature of 50-60 ℃, drying in a 60 ℃ drying oven, and collecting;
5) acidification: dropwise adding dilute acid into the alkali liquor in the acidification kettle, controlling the temperature to be 5-15 ℃, starting stirring, stopping adding acid when the mass of solid precipitated in the acidification kettle is not increased any more, continuously stirring for 10-15 min, and transferring the solid-liquid mixture into a centrifuge;
6) centrifuging: centrifuging the obtained solid-liquid mixture, washing the solid with absolute ethyl alcohol for 2-3 times, centrifuging again until the solid is dried, and transferring the solid into an oven;
7) drying: starting a vacuum system on the oven, controlling the vacuum system to vacuumize to be more than-0.097 MPa, controlling the temperature of the oven to be 30-40 ℃, baking for 2-5 h, and collecting the solid for mechanically applying to the synthesis of 4, 6-dichloropyrimidine.
Further, in the step 1 of the waste liquid treatment process, the dilute acid is dilute sulfuric acid, dilute hydrochloric acid or a mixture of the dilute sulfuric acid and the dilute hydrochloric acid, and the volume fraction concentration of the dilute acid is controlled to be 5-15%.
Further, the ethanol solution in the step 2 of the waste liquid treatment process is an ethanol water solution with the volume fraction concentration of 50-80%.
Further, in the step 4 of the waste liquid treatment process, the hot alkali solution is a sodium hydroxide solution, a potassium hydroxide solution or a sodium carbonate solution, and the mass fraction concentration of the hot alkali solution is controlled to be 10-20%.
Further, in the step 5 of the waste liquid treatment process, the dilute acid is dilute sulfuric acid, dilute hydrochloric acid or a mixture of the dilute sulfuric acid and the dilute hydrochloric acid, and the volume fraction concentration of the dilute acid is controlled to be 5-15%.
The invention has the beneficial effects that: the method carries out operations such as pH adjustment, evaporation, centrifugation, drying and the like after collecting the 4, 6-dichloropyrimidine synthesis waste liquid, timely collects and recycles useful components in the waste liquid, reduces toxic components in the waste liquid, avoids directly causing pollution and damage to the environment, reduces the synthesis production cost, improves the economic benefit, and has the advantages that the content of 4, 6-dihydroxypyrimidine in the waste water discharged by detection is less than or equal to 0.01 percent, the content of phosphide is less than or equal to 0.005 percent, the content of chloride ions is less than or equal to 0.001 percent, and the content of 4, 6-dichloropyrimidine is less than or equal to 0.008 percent.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A process for treating waste liquid generated in synthesis of 4, 6-dichloropyrimidine comprises the following specific steps:
1) adjusting the pH value: collecting the lower-layer wastewater of a washing kettle for synthesizing 4, 6-dichloropyrimidine in a pH adjusting tank, dropwise adding dilute sulfuric acid with the volume fraction concentration of 5%, starting stirring, monitoring the pH in the wastewater in time, stopping dropwise adding the dilute acid when the pH of the wastewater is 6.8, continuously stirring for 10min, and transferring the wastewater after pH adjustment to an evaporation kettle;
2) evaporation: starting a vacuum system on an evaporation kettle, controlling the vacuum system to vacuumize to-0.1 MPa, heating to 60 ℃, distilling out 1/2 water in the wastewater, cooling to normal temperature, adding an ethanol water solution with 2 times of the volume of the residual wastewater and 50% of integral number concentration of the residual wastewater into the evaporation kettle, heating again to 60 ℃, evaporating the wastewater until partial crystals are exposed, stopping heating, evaporating the residual solvent by using waste heat to obtain crystals, and drying the crystals in a drying oven at 60 ℃ to sell the crystals as byproducts;
3) distillation: collecting hazardous waste of a rectifying still for synthesizing 4, 6-dichloropyrimidine, starting a vacuum system on the distilling still, controlling the vacuum system to vacuumize to-0.1 MPa, raising the temperature to 30 ℃, condensing and collecting distilled fractions, and transferring residue at the bottom of the distilling still into an alkalization kettle after the fractions are completely distilled out;
4) alkalization: adding a sodium hydroxide solution with the mass fraction concentration of 10% and the temperature of 50 ℃ into an alkalization kettle, starting stirring, heating the alkalization kettle to 50 ℃, stopping stirring when the residual solid is not dissolved any more, standing for layering, transferring an upper water layer into the acidification kettle, washing a lower solid layer for 2 times by using hot water with the temperature of 50 ℃, drying in a 60 ℃ drying oven and collecting;
5) acidification: dropwise adding dilute sulfuric acid with volume fraction concentration of 5% into the alkali liquor in the acidification kettle, controlling the temperature at 5 ℃, starting stirring, stopping adding acid when the mass of the solid precipitated in the acidification kettle is not increased any more, continuously stirring for 10min, and transferring the solid-liquid mixture into a centrifuge;
6) centrifuging: centrifuging the obtained solid-liquid mixture, washing the solid with absolute ethyl alcohol for 2 times, centrifuging again until the solid is dried, and transferring the solid into an oven;
7) drying: starting a vacuum system on the oven, controlling the vacuum system to vacuumize to-0.1 MPa, controlling the temperature of the oven to be 30 ℃, drying for 5h, and collecting solid for mechanically applying to the synthesis of 4, 6-dichloropyrimidine;
the detection shows that the content of 4, 6-dihydroxypyrimidine in the discharged wastewater is 0.01 percent, the content of phosphide is 0.005 percent, the content of chloride ions is 0.001 percent, and the content of 4, 6-dichloropyrimidine is 0.008 percent.
Example 2
A process for treating waste liquid generated in synthesis of 4, 6-dichloropyrimidine comprises the following specific steps:
1) adjusting the pH value: collecting the lower-layer wastewater of a washing kettle for synthesizing 4, 6-dichloropyrimidine in a pH adjusting tank, dropwise adding dilute hydrochloric acid with the volume fraction concentration of 15%, starting stirring, monitoring the pH in the wastewater in time, stopping dropwise adding the dilute acid when the pH of the wastewater is 7.5, continuously stirring for 15min, and transferring the wastewater after pH adjustment to an evaporation kettle;
2) evaporation: starting a vacuum system on an evaporation kettle, controlling the vacuum system to vacuumize to-0.1 MPa, heating to 90 ℃, distilling out 2/3 water in the wastewater, cooling to normal temperature, adding an ethanol water solution with 80% of 5 times of integral number concentration of the volume of the residual wastewater into the evaporation kettle, heating to 90 ℃ again, evaporating the wastewater until partial crystals are exposed, stopping heating, evaporating the residual solvent by using waste heat to obtain crystals, and drying the crystals in a drying oven at 90 ℃ to be sold as byproducts;
3) distillation: collecting hazardous waste of a rectifying still for synthesizing 4, 6-dichloropyrimidine, starting a vacuum system on the distilling still, controlling the vacuum system to vacuumize to-0.1 MPa, raising the temperature to 80 ℃, condensing and collecting distilled fractions, and transferring residue at the bottom of the distilling still into an alkalization kettle after the fractions are completely distilled out;
4) alkalization: adding a potassium hydroxide solution with the mass fraction concentration of 20% and the temperature of 60 ℃ into an alkalization kettle, starting stirring, heating the alkalization kettle to 60 ℃, stopping stirring when the solid in the residual is not dissolved any more, standing for layering, transferring an upper water layer into the acidification kettle, washing a lower solid layer for 3 times by using hot water with the temperature of 60 ℃, drying in a 60 ℃ drying oven, and collecting;
5) acidification: dropwise adding dilute hydrochloric acid with volume fraction concentration of 15% into the alkali liquor in the acidification kettle, controlling the temperature at 15 ℃, starting stirring, stopping adding acid when the mass of solid precipitated in the acidification kettle is not increased any more, continuously stirring for 15min, and transferring the solid-liquid mixture into a centrifuge;
6) centrifuging: centrifuging the obtained solid-liquid mixture, washing the solid for 3 times by using absolute ethyl alcohol, centrifuging again until the solid is dried, and transferring the solid to an oven;
7) drying: starting a vacuum system on the oven, controlling the vacuum system to vacuumize to be more than-0.097 MPa, controlling the temperature of the oven to be 40 ℃, drying for 2h, and collecting solid for synthesis of 4, 6-dichloropyrimidine;
the detection shows that the content of 4, 6-dihydroxypyrimidine, phosphide and chloride ions in the discharged wastewater is 0.005%, 0.003%, 0.0006% and 0.005%.
Example 3
A process for treating waste liquid generated in synthesis of 4, 6-dichloropyrimidine comprises the following specific steps:
1) adjusting the pH value: collecting the lower-layer wastewater of a washing kettle for synthesizing 4, 6-dichloropyrimidine in a pH adjusting tank, dropwise adding a mixture of dilute sulfuric acid and dilute hydrochloric acid with the volume fraction concentration of 10%, starting stirring, monitoring the pH in the wastewater in time, stopping dropwise adding the dilute acid when the pH of the wastewater is 7.0, continuously stirring for 13min, and transferring the pH-adjusted wastewater into an evaporation kettle;
2) evaporation: starting a vacuum system on an evaporation kettle, controlling the vacuum system to vacuumize to-0.1 MPa, heating to 75 ℃, distilling out 2/3 water in the wastewater, cooling to normal temperature, adding an ethanol water solution with the integral number concentration of 60 percent of 3 times of the volume of the residual wastewater into the evaporation kettle, heating to 75 ℃ again, evaporating the wastewater until partial crystals are exposed, stopping heating, evaporating the residual solvent by using waste heat to obtain crystals, and drying the crystals in a 75 ℃ drying oven to be sold as byproducts;
3) distillation: collecting hazardous waste of a rectifying still for synthesizing 4, 6-dichloropyrimidine, starting a vacuum system on the distilling still, controlling the vacuum system to vacuumize to-0.1 MPa, raising the temperature to 50 ℃, condensing and collecting distilled fractions, and transferring residue at the bottom of the distilling still into an alkalization kettle after the fractions are completely distilled out;
4) alkalization: adding a sodium carbonate solution with the mass fraction concentration of 15% and the temperature of 55 ℃ into an alkalization kettle, starting stirring, heating the alkalization kettle to 55 ℃, stopping stirring when the solid in the residual is not dissolved any more, standing for layering, transferring an upper water layer into an acidification kettle, washing a lower solid layer for 3 times by using hot water with the temperature of 55 ℃, drying in a 60 ℃ drying oven, and collecting;
5) acidification: dropwise adding a mixture of dilute sulfuric acid and dilute hydrochloric acid or both with the volume fraction concentration of 10% into the alkali liquor in the acidification kettle, controlling the temperature at 10 ℃, starting stirring, stopping adding acid when the mass of solids precipitated in the acidification kettle is not increased any more, continuously stirring for 15min, and transferring the solid-liquid mixture into a centrifuge;
6) centrifuging: centrifuging the obtained solid-liquid mixture, washing the solid for 3 times by using absolute ethyl alcohol, centrifuging again until the solid is dried, and transferring the solid to an oven;
7) drying: starting a vacuum system on the oven, controlling the vacuum system to vacuumize to be more than-0.097 MPa, controlling the temperature of the oven to be 35 ℃, baking for 3 hours, and collecting solid to be applied to synthesis of 4, 6-dichloropyrimidine;
the detection shows that the content of 4, 6-dihydroxypyrimidine in the discharged wastewater is 0.008 percent, the content of phosphide is 0.003 percent, the content of chloride ion is 0.001 percent, and the content of 4, 6-dichloropyrimidine is 0.005 percent.
Example 4
A process for treating waste liquid generated in synthesis of 4, 6-dichloropyrimidine comprises the following specific steps:
1) adjusting the pH value: collecting the lower-layer wastewater of a washing kettle for synthesizing 4, 6-dichloropyrimidine in a pH adjusting tank, dropwise adding a mixture of dilute sulfuric acid and dilute hydrochloric acid with the volume fraction concentration of 8%, starting stirring, monitoring the pH in the wastewater in time, stopping dropwise adding the dilute acid when the pH of the wastewater is 7.0, continuously stirring for 13min, and transferring the pH-adjusted wastewater into an evaporation kettle;
2) evaporation: starting a vacuum system on an evaporation kettle, controlling the vacuum system to vacuumize to-0.1 MPa, heating to 80 ℃, distilling out 1/2 water in the wastewater, cooling to normal temperature, adding an ethanol water solution with the integral number concentration of 60% of 4 times of the volume of the residual wastewater into the evaporation kettle, heating again to 80 ℃, evaporating the wastewater until partial crystals are exposed, stopping heating, evaporating the residual solvent by using waste heat to obtain crystals, and drying the crystals in an oven at 80 ℃ to sell the crystals as byproducts;
3) distillation: collecting hazardous waste of a rectifying still for synthesizing 4, 6-dichloropyrimidine, starting a vacuum system on the distilling still, controlling the vacuum system to vacuumize to-0.1 MPa, raising the temperature to 60 ℃, condensing and collecting distilled fractions, and transferring residue at the bottom of the distilling still into an alkalization kettle after the fractions are completely distilled out;
4) alkalization: adding a mixture of a sodium hydroxide solution with a mass fraction concentration of 15%, a potassium hydroxide solution and a sodium carbonate solution at 55 ℃ into an alkalization kettle, starting stirring, heating the alkalization kettle to 55 ℃, stopping stirring when the residual solids are not dissolved, standing for layering, transferring an upper water layer into an acidification kettle, washing a lower solid layer for 3 times by using hot water at 55 ℃, drying in a 60 ℃ drying oven, and collecting;
5) acidification: dropwise adding a mixture of dilute sulfuric acid and dilute hydrochloric acid with the volume fraction concentration of 10% into the alkali liquor in the acidification kettle, controlling the temperature at 10 ℃, starting stirring, stopping adding acid when the mass of solid precipitated in the acidification kettle is not increased any more, continuously stirring for 13min, and transferring the solid-liquid mixture into a centrifuge;
6) centrifuging: centrifuging the obtained solid-liquid mixture, washing the solid for 3 times by using absolute ethyl alcohol, centrifuging again until the solid is dried, and transferring the solid to an oven;
7) drying: starting a vacuum system on the oven, controlling the vacuum system to vacuumize to-0.1 MPa, controlling the temperature of the oven to be 35 ℃, baking for 4h, and collecting solid for mechanically applying to the synthesis of 4, 6-dichloropyrimidine;
the detection shows that the content of 4, 6-dihydroxypyrimidine in the discharged wastewater is 0.008 percent, the content of phosphide is 0.001 percent, the content of chloride ions is 0.001 percent, and the content of 4, 6-dichloropyrimidine is 0.002 percent.
The method carries out operations such as pH adjustment, evaporation, centrifugation, drying and the like after collecting the 4, 6-dichloropyrimidine synthesis waste liquid, timely collects and recycles useful components in the waste liquid, reduces toxic components in the waste liquid, avoids directly causing pollution and damage to the environment, reduces the synthesis production cost, improves the economic benefit, and has the advantages that the content of 4, 6-dihydroxypyrimidine in the waste water discharged by detection is less than or equal to 0.01 percent, the content of phosphide is less than or equal to 0.005 percent, the content of chloride ions is less than or equal to 0.001 percent, and the content of 4, 6-dichloropyrimidine is less than or equal to 0.008 percent.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. A process for treating waste liquid generated in the synthesis of 4, 6-dichloropyrimidine is characterized by comprising the following steps: the waste liquid treatment process comprises the following specific steps:
1) adjusting the pH value: collecting the lower-layer wastewater of a washing kettle for synthesizing 4, 6-dichloropyrimidine in a pH adjusting tank, dropwise adding dilute acid, starting stirring, monitoring the pH in the wastewater in time, stopping dropwise adding the dilute acid when the pH of the wastewater is 6.8-7.5, continuously stirring for 10-15 min, and transferring the wastewater after pH adjustment to an evaporation kettle;
2) evaporation: starting a vacuum system on an evaporation kettle, controlling the vacuum system to vacuumize to be more than-0.097 MPa, heating to 60-90 ℃, distilling water in the wastewater out of 1/2-2/3, cooling to normal temperature, adding an ethanol solution which is 2-5 times of the volume of the residual wastewater into the evaporation kettle, heating to 60-90 ℃ again, evaporating the wastewater until part of crystals are exposed, stopping heating, evaporating the residual solvent by using waste heat to obtain crystals, and drying the crystals in an oven at 60-90 ℃ to sell the crystals as byproducts;
3) distillation: collecting hazardous waste of a rectifying kettle for synthesizing 4, 6-dichloropyrimidine, starting a vacuum system on the distilling kettle, controlling the vacuum system to vacuumize to be more than-0.097 MPa, raising the temperature to 30-80 ℃, condensing and collecting distilled fractions, and transferring residue at the bottom of the kettle to an alkalization kettle after the fractions are completely evaporated;
4) alkalization: adding a hot alkali solution with the temperature of 50-60 ℃ into an alkalization kettle, starting stirring, heating the alkalization kettle to 50-60 ℃, stopping stirring when the residual solid is not dissolved any more, standing for layering, transferring an upper water layer into an acidification kettle, washing a lower solid layer for 2-3 times by using hot water with the temperature of 50-60 ℃, drying in a 60 ℃ drying oven, and collecting;
5) acidification: dropwise adding dilute acid into the alkali liquor in the acidification kettle, controlling the temperature to be 5-15 ℃, starting stirring, stopping adding acid when the mass of solid precipitated in the acidification kettle is not increased any more, continuously stirring for 10-15 min, and transferring the solid-liquid mixture into a centrifuge;
6) centrifuging: centrifuging the obtained solid-liquid mixture, washing the solid with absolute ethyl alcohol for 2-3 times, centrifuging again until the solid is dried, and transferring the solid into an oven;
7) drying: starting a vacuum system on the oven, controlling the vacuum system to vacuumize to be more than-0.097 MPa, controlling the temperature of the oven to be 30-40 ℃, baking for 2-5 h, and collecting the solid for mechanically applying to the synthesis of 4, 6-dichloropyrimidine.
2. The process for treating waste liquid generated in the synthesis of 4, 6-dichloropyrimidine according to claim 1, characterized by comprising the following steps: in the step 1 of the waste liquid treatment process, the dilute acid is dilute sulfuric acid, dilute hydrochloric acid or a mixture of the dilute sulfuric acid and the dilute hydrochloric acid, and the volume fraction concentration of the dilute acid is controlled to be 5-15%.
3. The process for treating waste liquid generated in the synthesis of 4, 6-dichloropyrimidine according to claim 1, characterized by comprising the following steps: and in the step 2 of the waste liquid treatment process, the ethanol solution is an ethanol water solution with the volume fraction concentration of 50-80%.
4. The process for treating waste liquid generated in the synthesis of 4, 6-dichloropyrimidine according to claim 1, characterized by comprising the following steps: and in the step 4 of the waste liquid treatment process, the hot alkali solution is a sodium hydroxide solution, a potassium hydroxide solution or a sodium carbonate solution, and the mass fraction concentration of the hot alkali solution is controlled to be 10-20%.
5. The process for treating waste liquid generated in the synthesis of 4, 6-dichloropyrimidine according to claim 1, characterized by comprising the following steps: in the step 5 of the waste liquid treatment process, the dilute acid is dilute sulfuric acid, dilute hydrochloric acid or a mixture of the dilute sulfuric acid and the dilute hydrochloric acid, and the volume fraction concentration of the dilute acid is controlled to be 5-15%.
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| CN102633382A (en) * | 2012-04-10 | 2012-08-15 | 重庆紫光化工股份有限公司 | 4,6-dichloropyrimidine waste water treatment and resource recovery method |
| CN105859636A (en) * | 2016-05-13 | 2016-08-17 | 安徽广信农化股份有限公司 | Synthesis method of 4,6-dichloropyrimidine with 4,6-dihydroxypyrimidine serving as midbody |
| CN205953756U (en) * | 2016-08-29 | 2017-02-15 | 石家庄杰克化工有限公司 | Production 4, 6 dihydroxypyrimidine 's effluent disposal system |
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| CN102633382A (en) * | 2012-04-10 | 2012-08-15 | 重庆紫光化工股份有限公司 | 4,6-dichloropyrimidine waste water treatment and resource recovery method |
| CN105859636A (en) * | 2016-05-13 | 2016-08-17 | 安徽广信农化股份有限公司 | Synthesis method of 4,6-dichloropyrimidine with 4,6-dihydroxypyrimidine serving as midbody |
| CN205953756U (en) * | 2016-08-29 | 2017-02-15 | 石家庄杰克化工有限公司 | Production 4, 6 dihydroxypyrimidine 's effluent disposal system |
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