CN102583867A - Method for treating waste water in chloro pyrimidine combining process - Google Patents
Method for treating waste water in chloro pyrimidine combining process Download PDFInfo
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Abstract
The invention relates to a method for treating waste water in the production process of chloro pyrimidine, such as 4,6-dichloro-pyrimidine and 2-amino-4,6-dichloro-pyrimidine. The method finishes treatment of waste water by adopting a chemical method for treatment, adding water into products after recycling chloro reagent, dissolving the products, not controlling pH of material liquid in an extraction process, and then treating separated acid water and quick lime or Ca(OH)2, recycling and purifying organic amine, phosphate and chloridion in the waste water step by step. The method can treat waste water to enable the waste water to reach the standard and reduces treatment cost of three wastes.
Description
Technical field
The present invention relates to produce wastewater treatment method in the Chloropyrimide building-up process, said method reclaims organic amine, subphosphate and calcium chloride respectively through chemical process.
Background technology
Chloropyrimide is widely used in the organic synthesis field owing to having good reaction activity, has very application prospects.As 4, the 6-dichloro pyrimidine is as the critical materials of sterilant ICIA 5504, and 2-is amino-4, and the 6-dichloro pyrimidine is as agricultural chemicals chlorimuronethyl important source material etc.The main flow synthesis technique adopts chloro agent such as phosphoryl chloride, phosphorus trichloride or phosphorus pentachloride in the presence of trimethylamine or nitrogen heterocyclic ring amine, to react at present.Because wastewater flow rate is too big in the Chloropyrimide production process, and complicated component, a large amount of phosphoric acid salt that wherein contain and organic amine salt cause the eutrophication of water easily, destruction ecotope two and limited the industrial scale of Chloropyrimide greatly.Therefore, the exploitation of method of wastewater treatment is significant in the Chloropyrimide building-up process.
In the industrial production, waste water in the Chloropyrimide building-up process reclaims methods such as normally taking chemical precipitation behind the Chloropyrimide through extraction and handles, and obtains mixing salt, and filtrating is again through giving birth to, change processing, effluxes after up to standard.After treatment, though waste water can reach discharge index, carry out pH regulator at alkali such as extraction needs use before ammoniacal liquor; But this process is an exothermic process, the ammonia soln volatilization, and the workman can't operate and influence environment; Even use other alkali also need slowly handle, make that the treatment time is long, cost is high, influence the entire treatment cycle; In addition, handle the bad processing of gained by-product mixed salt, and total processing costs is higher.
Goal of the invention
The invention provides the approach of the effective constituent in a kind of effective separation, the recovery Chloropyrimide waste water, make wastewater treatment more economically, operability is stronger.
Technical scheme
The objective of the invention is to reach like this: after the Chloropyrimide hydrolysis,, directly under acidic conditions, extract with organic solvent without regulating pH.Extracted residual acid waste water adds unslaked lime or calcium hydroxide, reclaims organic amine through distillation, and cooling afterwards, suction filtration reclaim alkali calcium phosphate, filtrating through decolouring, concentrate, crystallization obtains calcium chloride.Through chemical precipitation-distillation-centrifugation method, not only realized recovery, and reached separation phosphate radical-cl ions in the waste water to organic amine in the waste water.
In the aforesaid method, handled waste water is regulated pH without alkaline matters such as ammoniacal liquor in extraction process;
In the aforesaid method, unslaked lime or calcium hydroxide add-on by processing waste water quality 15～45%;
In the aforesaid method, the temperature that adds unslaked lime or calcium hydroxide is at 30～60 ℃;
In the aforesaid method, the recovered temperature of organic amine is at 50～100 ℃;
In the aforesaid method, filtrating decolorization amount of activated is between 0.5～5%;
In the aforesaid method, the activated carbon decolorizing temperature is between 40～80 ℃.
In the aforesaid method, used organic solvent is a toluene.
Specifically, the treatment process that the present invention comprised comprises the steps:
1, reaction is finished and steam the Chloropyrimide reaction material of removing behind a large amount of POCl3s or phosphorus trichloride, the phosphorus pentachloride and add in the entry and be hydrolyzed,, directly extract separatory with organic solvent without neutralization;
2, quantitative unslaked lime or calcium hydroxide are joined in the waste water of above-mentioned separatory gained react;
3, will add mixing behind unslaked lime or the calcium hydroxide after material heat up gradually, organic amine is reclaimed in distillation;
The material that 4, will reclaim organic amine is lowered the temperature, crystallization, and suction filtration reclaims alkali calcium phosphate;
5, the filtrating that will reclaim behind the alkali calcium phosphate is decoloured, and removes organic impurity wherein;
6, the back feed liquid of will decolouring concentrates, and the calcium chloride solid is separated out in cooling.
The reaction equation that relates in the treating processes:
CaO+H
2O→Ca(OH)
2
Ca(OH)2+2HCl→CaCl2+2H2O
3Ca(OH)2+2H3PO4→Ca3(PO4)2+6H2O
Ca(OH)2+2(CH3CH2)3N.HCl→CaCl2+2H2O+2(CH3CH2)3N
3Ca3(PO4)2+Ca(OH)2→2Ca5(OH)(PO4)3
Beneficial effect
Therefore among the present invention, owing to do not carry out pH regulator in the extraction process, avoided the pollution of other alkaline organics to organic amine, made and reclaim the organic amine content that obtains more than 99%, the recovery is more than 90%; Handle waste water with unslaked lime or calcium hydroxide, can accomplish phosphatic effective separation, the phosphate content in the waste water is reduced to below the 0.5mg/L; The centrifugal after treatment alkali calcium phosphate content that obtains is more than 99%, can satisfy the request for utilization in the field such as separant, biomaterial, water conditioner, dyestuff, rubber, pharmacy of resin anti-stick; The CaCl that makes after concentrating
2Content can reach more than 99%, satisfies the industrial application requirement.
The unslaked lime or the calcium hydroxide that use among the present invention are cheap and easy to get; The organic amine that recovery obtains, alkali calcium phosphate and calcium chloride all have certain marketable value, therefore, adopt present method to handle Chloropyrimide waste water; Not only processing cost can be do not increased, and certain profit can be produced.Only remain the water that steams after the processing, index reaches the service water emission request.
Description of drawings
Fig. 1: processing flow chart of the present invention
Preferred forms
Through instance mentality of designing of the present invention is described below, but the present invention is not limited to following examples.
Embodiment 1,
Waste water produces: in four-hole bottle, add 4,6-dihydroxy-pyrimidine 114g (1mol), POCl3 465g (3mol), stirring and dissolving.Be warming up to 40～60 ℃, begin to drip 256g (2.5mol) triethylamine, controlled temperature is 40-60 ℃ in the dropping process, and 1h dropwises.Then, be warming up to 60～100 ℃, insulation 2h.Reduce to room temperature, the reclaim under reduced pressure phosphoryl chloride.Add 1000g toluene, after mixing, feed liquid slowly joined in the 1200g frozen water be hydrolyzed.Keeping the frozen water temperature in the batch turning process is 0-10 ℃.After stirring hydrolysis 60min, pour feed liquid into separating funnel, leave standstill separatory.Water leaves standstill separatory through extracted in toluene 3 times, and organic phase merges, and the gained water is acid waste water.
Acid waste water is handled: get acid waste water 900g, be warming up to 50～60 ℃, stirring down, gradation adds unslaked lime 190g; Insulation 30min; Triethylamine is reclaimed in the distillation that begins to heat up, and the cut between 60～100 ℃ of the interceptings stops distillation after detecting cut pH to 8～9; Reclaim the pure 116g of triethylamine, the recovery 90.6%.The cooling suction filtration obtains alkali calcium phosphate, dry weight 200g, content 98.5%.Filtrating adds gac 3g with in the hydrochloric acid and back, 50 ℃ of decolouring 30min, and the suction filtration recovered carbon, filtrating is concentrated, drying obtains calcium chloride 154g, content 98.3%.Concentrate water outlet COD 480mg/L, NH
3-N 2mg/L, pH 7.1, can directly discharge.
Building-up process: with example 1.
Acid waste water is handled: get acid waste water 900g, be warming up to 60～70 ℃, stirring down, gradation adds unslaked lime 180g; Insulation 30min; Triethylamine is reclaimed in the distillation that begins to heat up, and the cut between 60～100 ℃ of the interceptings stops distillation after detecting cut pH to 8～9; Reclaim the pure 101g of triethylamine, the recovery 78.9%.The cooling suction filtration obtains alkali calcium phosphate, dry weight 201g, content 98.9%.Add gac 3g, 50 ℃ of decolouring 30min, the suction filtration recovered carbon, the filtrating concentrate drying obtains calcium chloride 133g, content 98.5%.Concentrate water outlet COD 880mg/L, NH3-N6mg/L, pH 7.8.
Embodiment 3,
Building-up process: with example 1.
Acid waste water is handled: get acid waste water 900g, be warming up to 40～50 ℃, stirring down, gradation adds Ca (0H)
2286g, insulation 30min, triethylamine is reclaimed in the distillation that begins to heat up, and the cut between 60～100 ℃ of the interceptings stops distillation after detecting cut pH to 8～9, reclaims the pure 117g of triethylamine, the recovery 91.4%.The cooling suction filtration obtains alkali calcium phosphate, dry weight 200g, content 99.5%.Filtrating adds gac 3g with in the hydrochloric acid and back, 50 ℃ of decolouring 30min, and the suction filtration recovered carbon, the filtrating concentrate drying obtains calcium chloride 206g, content 99.3%.Concentrate water outlet COD350mg/L, NH3-N 1.4mg/L, pH 7.0.
Embodiment 4,
Building-up process: with example 1.
Acid waste water is handled: get acid waste water 900g, be warming up to 40～50 ℃, stirring down, gradation adds Ca (0H)
2286g, insulation 30min, triethylamine is reclaimed in the distillation that begins to heat up, and the cut between 75～101 ℃ of the interceptings stops distillation after detecting cut pH to 8～9, reclaims the pure 115g of triethylamine, the recovery 89.8%.The cooling suction filtration obtains alkali calcium phosphate, dry weight 197g, content 99.3%.Filtrating adds gac 5g with in the hydrochloric acid and back, 50 ℃ of decolouring 30min, and the suction filtration recovered carbon, filtrating is concentrated, drying obtains calcium chloride 205g, content 99.1%.Concentrate water outlet COD 380mg/L, NH3-N 1.7mg/L, pH 7.2.
The foregoing description only is explanation technical conceive of the present invention and characteristics, and its purpose is to let the personage who is familiar with this technology can understand content of the present invention and enforcement according to this, can not limit protection scope of the present invention with this.All equivalences that spirit is done according to the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (9)
1. a separation, reclaim the method for the effective constituent in the Chloropyrimide waste water, it is characterized in that: this method comprises the steps:
(1), reaction finished and steam the Chloropyrimide reaction material of removing behind a large amount of POCl3s or phosphorus trichloride, the phosphorus pentachloride to be added in the entry and is hydrolyzed, and without neutralization, directly extracts separatory with organic solvent;
(2), quantitative unslaked lime or calcium hydroxide are joined in the waste water of above-mentioned separatory gained react;
(3), will add the mixing behind unslaked lime or the calcium hydroxide after material heat up gradually, organic amine is reclaimed in distillation;
The material that (4), will reclaim organic amine is lowered the temperature crystallization, suction filtration, recovery alkali calcium phosphate;
(5), the filtrating that will reclaim behind the alkali calcium phosphate decolours, and removes organic impurity wherein;
(6), the back feed liquid of will decolouring concentrates, the calcium chloride solid is separated out in cooling.
2. the method for the effective constituent in separation as claimed in claim 1, the recovery Chloropyrimide waste water is characterized in that used organic solvent is a toluene.
3. separation as claimed in claim 1, reclaim the method for the effective constituent in the Chloropyrimide waste water, it is characterized in that handled waste water regulates pH without alkaline matters such as ammoniacal liquor in extraction process.
4. separation as claimed in claim 1, reclaim the method for the effective constituent in the Chloropyrimide waste water, it is characterized in that unslaked lime or calcium hydroxide add-on by processing waste water quality 15～45%.
5. the method for the effective constituent in separation as claimed in claim 1, the recovery Chloropyrimide waste water, the temperature that it is characterized in that adding unslaked lime or calcium hydroxide is at 30～60 ℃.
6. the method for the effective constituent in separation as claimed in claim 1, the recovery Chloropyrimide waste water, the recovered temperature that it is characterized in that organic amine is at 50～100 ℃.
7. the method for the effective constituent in separation as claimed in claim 1, the recovery Chloropyrimide waste water, the decolorization amount of activated that it is characterized in that filtrating is 0.5～5% of a waste water weight.
8. the method for the effective constituent in separation as claimed in claim 1, the recovery Chloropyrimide waste water is characterized in that the activated carbon decolorizing temperature is between 40～80 ℃.
9. the method for the effective constituent in separation as claimed in claim 1, the recovery Chloropyrimide waste water is characterized in that step is following:
In four-hole bottle, add 4,6-dihydroxy-pyrimidine 114g, POCl3 465g, stirring and dissolving.Be warming up to 40～60 ℃, begin to drip the 256g triethylamine, controlled temperature is 40-60 ℃ in the dropping process, and 1h dropwises; Then, be warming up to 60～100 ℃, insulation 2h reduces to room temperature, the reclaim under reduced pressure phosphoryl chloride.Add 1000g toluene, after mixing, feed liquid slowly joined in the 1200g frozen water be hydrolyzed; Keeping the frozen water temperature in the batch turning process is 0-10 ℃, stir hydrolysis 60min after, pour feed liquid into separating funnel, leave standstill separatory, water leaves standstill separatory through extracted in toluene 3 times, organic phase merges, the gained water is acid waste water;
Get acid waste water 900g, be warming up to 50～60 ℃, gradation adds unslaked lime 190g under stirring, insulation 30min; Triethylamine is reclaimed in the distillation that begins to heat up, and the cut between 60～100 ℃ of the interceptings stops distillation after detecting cut pH to 8～9, reclaims the pure 116g of triethylamine; The recovery 90.6%, the cooling suction filtration obtains alkali calcium phosphate, dry weight 200g, content 98.5%; Filtrating adds gac 3g with in the hydrochloric acid and back, 50 ℃ of decolouring 30min, and the suction filtration recovered carbon, filtrating is concentrated, drying obtains calcium chloride 154g; Content 98.3% concentrates water outlet COD 480mg/L, NH
3-N 2mg/L, pH 7.1, can directly discharge.10. the method for the effective constituent in separation as claimed in claim 1, the recovery Chloropyrimide waste water is characterized in that step is following:
In four-hole bottle, add 4,6-dihydroxy-pyrimidine 114g, POCl3 465g, stirring and dissolving.Be warming up to 40～60 ℃, begin to drip the 256g triethylamine, controlled temperature is 40-60 ℃ in the dropping process, and 1h dropwises; Then, be warming up to 60～100 ℃, insulation 2h reduces to room temperature, the reclaim under reduced pressure phosphoryl chloride.Add 1000g toluene, after mixing, feed liquid slowly joined in the 1200g frozen water be hydrolyzed; Keeping the frozen water temperature in the batch turning process is 0-10 ℃, stir hydrolysis 60min after, pour feed liquid into separating funnel, leave standstill separatory, water leaves standstill separatory through extracted in toluene 3 times, organic phase merges, the gained water is acid waste water;
Acid waste water is handled: get acid waste water 900g, be warming up to 60～70 ℃, gradation adds unslaked lime 180g under stirring, insulation 30min; Triethylamine is reclaimed in the distillation that begins to heat up, and the cut between 60～100 ℃ of the interceptings stops distillation after detecting cut pH to 8～9, reclaims the pure 101g of triethylamine; The recovery 78.9%, the cooling suction filtration obtains alkali calcium phosphate, dry weight 201g, content 98.9%; Add gac 3g, 50 ℃ of decolouring 30min, the suction filtration recovered carbon, the filtrating concentrate drying obtains calcium chloride 133g; Content 98.5% concentrates water outlet COD 880mg/L, NH3-N 6mg/L, and pH 7.8.
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| CN103482592A (en) * | 2013-09-13 | 2014-01-01 | 重庆紫光化工股份有限公司 | Method for treating phosphorus-containing waste liquor |
| CN103833180A (en) * | 2013-11-19 | 2014-06-04 | 华中药业股份有限公司 | Method for treating waste water obtained during synthesis of vitamin B6 through oxazole method |
| CN105130082A (en) * | 2015-09-17 | 2015-12-09 | 博天环境集团股份有限公司 | Method for treating triethylamine-contained wastewater |
| CN106187912A (en) * | 2016-07-19 | 2016-12-07 | 安徽广信农化股份有限公司 | A kind of production technology of 4,6 dichloro pyrimidines |
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| CN105130082A (en) * | 2015-09-17 | 2015-12-09 | 博天环境集团股份有限公司 | Method for treating triethylamine-contained wastewater |
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| CN107450614B (en) * | 2017-08-09 | 2020-05-19 | 中国大唐集团科学技术研究院有限公司 | Real-time accurate control system for discharge amount of limestone/lime wet desulphurization wastewater |
| CN107450614A (en) * | 2017-08-09 | 2017-12-08 | 中国大唐集团科学技术研究院有限公司 | The real-time accuracy-control system of limestone/lime wet desulphurization wastewater discharge |
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