CN102874786A - Processing method of glyphosate mother liquor - Google Patents
Processing method of glyphosate mother liquor Download PDFInfo
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- CN102874786A CN102874786A CN2012103848600A CN201210384860A CN102874786A CN 102874786 A CN102874786 A CN 102874786A CN 2012103848600 A CN2012103848600 A CN 2012103848600A CN 201210384860 A CN201210384860 A CN 201210384860A CN 102874786 A CN102874786 A CN 102874786A
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Abstract
The invention relates to a processing method of glyphosate mother liquor. The processing method includes the following steps: adding alkaline substances into glyphosate crystallized mother liquor, adjusting pH into 3-7 and layering, upper-layer liquid is mother liquor rich in triethylamine, and lower-layer liquid is high-concentration phosphorus containing mother liquor; adding alkaline substances into the upper-layer liquid continuously, adjusting pH to 10-12, separating liquid to obtain organic-phase triethylamine, rectifying a water phase to recover triethylamine fraction, and rectifying waste water to be up to standard and discharged after conducting further biological processing; evaporating and concentrating the lower-layer liquid in multiple-effect mode, cooling to reach the room temperature, filtering to obtain filter cakes, and washing to remove organic substances, namely inorganic salt is obtained; and incinerating filtrate through an incinerator at the temperature of 600-900 DEG C to obtain pyrophosphate. The processing method achieves high-yield recovery of chlorine, phosphorus and triethylamine in the glyphosate mother liquor and is simple in process, environment-friendly, free of pollution and suitable for popularization and application of industrial mass production.
Description
Technical field
The present invention relates to a kind for the treatment of process of glyphosate mother solution, particularly relate to the treatment process that a kind of dialkyl phosphite method is produced the glyphosate crystalline mother solution that glyphosate obtains.
Technical background
Glyphosate is as the steriland herbicide of a kind of efficient, wide spectrum, low toxicity, and range of application is more and more extensive, has become at present the in the world weedicide of consumption maximum, and Present Domestic prepares glyphosate and adopts dialkyl phosphite method and iminodiacetic acid (salt) acid system more.
The glyphosate crystalline mother solution treatment process that produces in the at present dialkyl phosphite method production glyphosate process mainly is that crystalline mother solution is added the liquid caustic soda neutralization, make in the mother liquor triethylamine layering out, change synthetic the use after the dehydration over to, the separation mother liquor advances rectifying tower and carries out rectifying, the gyphosate solution of membrane concentration preparation 10% is carried out in the triethylamine reuse utilization that steams, the mother liquor after the rectifying.
But along with the progressively raising of country to environmental requirement, active constituent content is lower than 30% gyphosate solution and has not allowed to carry out production and selling.This means that present glyphosate enterprise has been not suitable with present requirement to the technique of mother liquid disposal, how to process phosphorus containg substances that triethylamine in the glyphosate crystalline mother solution and mother liquor reclaimed triethylamine and be the problem that needs that glyphosate enterprise faces solve.
Patent CN1277835C and CN101190926A propose to pass into ammonia and reclaim triethylamine in glyphosate mother solution, the ammonium glyphosate that ammonium chloride obtains concentrating is removed in the redistillation dehydration, but the concentrated ammonium glyphosate salts solution that obtains is difficult for recycling, the triethylamine rate of recovery is also lower, the secondary benefit is low, the distillation power consumption is also higher, so processing cost is higher.Patent application CN101307002A discloses a kind of novel method that reclaims the triethylamine in glyphosate mother liquid of dialkyl phosphite method production, the method has solved the low problem of the triethylamine rate of recovery, but this invented technology is loaded down with trivial details, also to use organic solvent in the treating processes, processing cost is higher, and the feature of environmental protection is also poor; Patent application CN101985426A discloses a kind for the treatment of process of glyphosate mother solution of dialkyl phosphite method production.The method triethylamine rate of recovery is more than 98.5%, although the triethylamine rate of recovery is higher, but the waste water COD of discharging is less than 500mg/L, TP is less than 1.0mg/L, and ammonia nitrogen is less than 15mg/L, and environmental benefit is also not outstanding, simultaneously, this invention is not made efforts to reducing the processing cost aspect, except triethylamine without other regenerants, cause processing cost higher.
These disclosed technology have all related to the recovery problem of triethylamine in the glyphosate crystalline mother solution, how to recycle and but do not have effective solution but the glyphosate crystalline mother solution has been reclaimed phosphorus containg substances behind the triethylamine.
Now, seek a kind of triethylamine that can height satisfy and reclaim yield, can reduce again waste water and discharge, alleviate environmental protection pressure, the treatment process that can effectively reclaim phosphorus containg substances simultaneously is the problem that the glyphosate industry needs to be resolved hurrily.
Summary of the invention
In order to solve the problems of the technologies described above, the invention provides the treatment process that a kind of dialkyl phosphite method is produced the glyphosate mother solution that obtains.Present method has solved the deficiency that exists in the existing technique, has embodied the progress of glyphosate mother solution treatment technology.
Concrete technical scheme of the present invention is as follows:
A kind for the treatment of process of glyphosate mother solution may further comprise the steps:
(1) in the glyphosate crystalline mother solution, add alkaline matter, make the layering to the 3-7 of mother liquor pH regulator, effective separation triethylamine and phosphorous thing, the upper strata is the mother liquor that is rich in triethylamine, lower floor is the high-density phosphorus mother liquor;
(2) continue to add alkaline matter in the upper strata liquid of step (1) gained and regulate separatory behind the pH to 10-12, tell the organic phase triethylamine, water rectifying is collected and is contained the triethylamine cut, gained waste water qualified discharge after further biochemical treatment after the rectifying;
(3) subnatant of step (1) gained is concentrated through multiple-effect evaporation again, be cooled to room temperature after, filter, effective separation salt and phosphorus containg substances, filter cake is removed organism through washing, namely gets inorganic salt; Filtrate is crossed 600-900 ℃ of incinerator through burning, and gets pyrophosphate salt.Can be further waste heat and solid in burning recovered flue gas simultaneously.
Described glyphosate mother solution is when adopting the standby glyphosate of dialkyl phosphite legal system, remaining glyphosphonic acid aqueous mother liquor behind the glyphosate crystallization.
In above-mentioned steps (1) and (2), alkaline matter is sodium hydroxide, potassium hydroxide, calcium hydroxide or calcium oxide.Inventing used alkaline matter is pH adjusting agent, and its state, concentration are not particularly limited, for considering of wastewater flow rate and processing cost, and preferred sodium hydroxide.
In the above-mentioned steps (2), rectification temperature is 90-110 ℃.
In the above-mentioned steps (3), multiple-effect evaporation is concentrated into the 60-90% of former weight.
Adopt the present invention to process the glyphosate crystalline mother solution and have following advantages:
(1) technique is simple, efficient, and the chlorion transformation efficiency is more than 99%, and the triethylamine rate of recovery is more than 98.8%, and gained pyrophosphate salt content is more than 98.2%, and the phosphorus containg substances transformation efficiency reaches more than 97.8%;
The waste water COD of (2) discharging is less than 20mg/L, and TP is less than 0.5mg/L, and ammonia nitrogen is less than 9mg/L, and COD, TP and ammonia nitrogen have reduced respectively 60%, 50% and 40% than existing technique (CN101985426A); Substantially realized the zero release of waste water, efficiently solved the processing problem of glyphosate mother solution, environmental benefit of the present invention is outstanding;
(3) the gained Industrial Salt can be used for the industries such as chemical industry, papermaking, building, and the pyrophosphate salt of gained can be used for chemical industry, plating, wool spinning, paper industry, so economic benefit of the present invention is outstanding.
Embodiment
Below by specific embodiment the present invention is further set forth, should be understood that, following explanation only is in order to explain the present invention, its particular content not to be limited.
Embodiment 1
Get glyphosate crystalline mother solution 1000g, detect to get triethylamine 19.6%, chlorion 9.6%, total phosphorus 2.88%, adding quality percentage composition is 30% sodium hydroxide solution, makes the rear layering of mother liquor pH regulator to 3.Upper strata liquid continues hydro-oxidation sodium and regulates the rear separatory of pH to 10, tells the organic phase triethylamine, and wherein triethylamine cut is reclaimed in 90 ℃ of rectifying of water, and the total triethylamine quality of gained is 195.6g, content 99.2%, the triethylamine rate of recovery 99.0%.Rectifying gained waste water is through further surveying COD 19mg/L after the biochemical treatment, TP 0.4mg/L, ammonia nitrogen 8mg/L, discharging.Subnatant is concentrated into 60% of former weight through multiple-effect evaporation, filters, and filter cake is removed a small amount of organism through washing, namely gets sodium-chlor 157.44g, and the chlorion transformation efficiency is 99.5%; Filtrate passes into incinerator, through 600 ℃ of burnings, namely gets trisodium phosphate 123.48g, and content 98.2%, phosphorus containg substances transformation efficiency are 98.2%, simultaneously heat and the solid in the recovered flue gas.
Embodiment 2
Get glyphosate crystalline mother solution 1000g, detect to get triethylamine 19.6%, chlorion 9.6%, total phosphorus 2.88%, adding quality percentage composition is 40% sodium hydroxide solution, makes the rear layering of mother liquor pH regulator to 4.Get upper strata liquid and continue the rear separatory of hydro-oxidation sodium adjusting pH to 11, tell the organic phase triethylamine, wherein triethylamine cut is reclaimed in 100 ℃ of rectifying of water, and the total triethylamine quality of gained is 195.7g, content 99.3%, the triethylamine rate of recovery 99.1%.Rectifying gained waste water is COD 17mg/L after further biochemical treatment, TP 0.3mg/L, ammonia nitrogen 6mg/L.Subnatant is concentrated into 70% of former weight through multiple-effect evaporation, filters, and filter cake is removed a small amount of organism through washing, namely gets sodium-chlor 156.8g, and the chlorion transformation efficiency is 99.1%; Filtrate passes into incinerator, through 700 ℃ of burnings, namely gets trisodium phosphate 122.88g, content 98.4%, phosphorus containg substances transformation efficiency 97.9%, simultaneously heat and the solid in the recovered flue gas.
Embodiment 3
Get and contain triethylamine 19.6%, chlorion 9.6%, the glyphosate crystalline mother solution 1000g of total phosphorus 2.88% adds the quality percentage composition and is 50% sodium hydroxide solution, makes the rear layering of mother liquor pH regulator to 5.Get upper strata liquid and continue the rear separatory of hydro-oxidation sodium adjusting pH to 12, tell the organic phase triethylamine, wherein triethylamine cut is reclaimed in 110 ℃ of rectifying of water, and the total triethylamine quality of gained is 195.6g, content 99.4%, the triethylamine rate of recovery 99.2%.Rectifying gained waste water is COD 10mg/L after further biochemical treatment, TP 0.3mg/L, ammonia nitrogen 7mg/L.Subnatant is concentrated into 80% of former weight through multiple-effect evaporation, filters, and filter cake is removed a small amount of organism through washing, namely gets sodium-chlor 156.7g, and the chlorion transformation efficiency is 99.1%; Filtrate passes into incinerator, through 800 ℃ of burnings, namely gets trisodium phosphate 123.0g, content 98.2%, phosphorus containg substances transformation efficiency 97.8%, simultaneously heat and the solid in the recovered flue gas.
Embodiment 4
Get and contain triethylamine 19.6%, chlorion 9.6%, the glyphosate crystalline mother solution 1000g of total phosphorus 2.88% adds solid sodium hydroxide, makes the rear layering of mother liquor pH regulator to 6.Get upper strata liquid and continue the rear separatory of hydro-oxidation sodium adjusting pH to 10, tell the organic phase triethylamine, wherein triethylamine cut is reclaimed in 110 ℃ of rectifying of water, and the total triethylamine quality of gained is 196.0g, content 99.6%, the triethylamine rate of recovery 99.6%.Rectifying gained waste water is COD 12mg/L after further biochemical treatment, TP 0.3mg/L, ammonia nitrogen 5mg/L.Subnatant is concentrated into 90% of former weight through multiple-effect evaporation, filters, and filter cake is removed a small amount of organism through washing, namely gets sodium-chlor 158.08g, and the chlorion transformation efficiency is 99.9%; Filtrate passes into incinerator, through 900 ℃ of burnings, namely gets trisodium phosphate 123.48g, content 99.5%, phosphorus containg substances transformation efficiency 99.5%, simultaneously heat and the solid in the recovered flue gas.
Embodiment 5
Get and contain triethylamine 19.6%, chlorion 9.6%, the glyphosate crystalline mother solution 1000g of total phosphorus 2.88% adds solid potassium hydroxide, makes the rear layering of mother liquor pH regulator to 7.Get upper strata liquid and continue the rear separatory of hydro-oxidation potassium adjusting pH to 11, tell the organic phase triethylamine, wherein triethylamine cut is reclaimed in 110 ℃ of rectifying of water, and the total triethylamine quality of gained is 196.0g, content 99.1%, the triethylamine rate of recovery 99.1%.Rectifying gained waste water is COD 12mg/L after further biochemical treatment, TP 0.4mg/L, ammonia nitrogen 5mg/L.Subnatant is concentrated into 80% of former weight through multiple-effect evaporation, filters, and filter cake is removed a small amount of organism through washing, namely gets Repone K 199.8g, and the chlorion transformation efficiency is 99.0%; Filtrate passes into incinerator, through 650 ℃ of burnings, namely gets potassium pyrophosphate 153.48, content 98.8%, phosphorus containg substances transformation efficiency 98.8%, simultaneously heat and the solid in the recovered flue gas.
Embodiment 6
Get and contain triethylamine 19.6%, chlorion 9.6%, the glyphosate crystalline mother solution 1000g of total phosphorus 2.88% adds calcium hydroxide, makes the rear layering of mother liquor pH regulator to 5.Get upper strata liquid and continue the rear separatory of adding calcium hydroxide adjusting pH to 11, tell the organic phase triethylamine, wherein triethylamine cut is reclaimed in 110 ℃ of rectifying of water, and the total triethylamine quality of gained is 195.0g, content 99.3%, the triethylamine rate of recovery 98.8%.Rectifying gained waste water is COD 17mg/L after further biochemical treatment, TP 0.4mg/L, ammonia nitrogen 7mg/L.Subnatant is concentrated into 80% of former weight through multiple-effect evaporation, is cooled to room temperature, filters, and filter cake is removed a small amount of organism through washing, namely gets calcium chloride 148.8g, and the chlorion transformation efficiency is 99.1%; Filtrate passes into incinerator, through 750 ℃ of burnings, namely gets Calcium Pyrophosphate 118.08g, content 98.6%, phosphorus containg substances transformation efficiency 98.6%, simultaneously heat and the solid in the recovered flue gas.
Embodiment 7
Get and contain triethylamine 19.6%, chlorion 9.6%, the glyphosate crystalline mother solution 1000g of total phosphorus 2.88% adds calcium oxide, makes the rear layering of mother liquor pH regulator to 3.Get upper strata liquid and continue to add the rear separatory of calcium oxide adjusting pH to 10, tell the organic phase triethylamine, the triethylamine cut is reclaimed in 110 ℃ of rectifying of water, and the total triethylamine quality of gained is 195.6g, content 99.0%, the triethylamine rate of recovery 98.8%.Rectifying gained waste water is COD 12mg/L after further biochemical treatment, TP 0.3mg/L, ammonia nitrogen 4mg/L.Subnatant is concentrated into 80% of former weight through multiple-effect evaporation, filters, and filter cake is removed a small amount of organism through washing, namely gets calcium chloride 148.9g, and the chlorion transformation efficiency is 99.2%; Filtrate passes into incinerator, through 850 ℃ of burnings, namely gets Calcium Pyrophosphate 118.0g, content 98.8%, and the phosphorus containg substances transformation efficiency need to reach 98.8%, simultaneously heat and the solid in the recovered flue gas.
Claims (6)
1. the treatment process of a glyphosate mother solution is characterized in that may further comprise the steps:
In the glyphosate crystalline mother solution, add alkaline matter, transfer pH to 3-7, layering, upper strata liquid is the mother liquor that is rich in triethylamine, subnatant is the high-density phosphorus mother liquor;
Continue to add alkaline matter in the liquid of step (1) gained upper strata, regulate pH to 10-12, separatory is told the organic phase triethylamine, and the triethylamine cut is reclaimed in water rectifying, and rectifying gained waste water is qualified discharge after further biochemical treatment;
Get step (1) gained subnatant, multiple-effect evaporation is concentrated, be cooled to room temperature after, filter, get filter cake, organism is removed in washing, namely gets inorganic salt; Get filtrate and burn under 600-900 ℃ through incinerator, namely get pyrophosphate salt;
When described glyphosate mother solution is the standby glyphosate of dialkyl phosphite legal system, remaining glyphosphonic acid aqueous mother liquor after the glyphosate crystallization.
2. treatment process according to claim 1, it is characterized in that: described alkaline matter is sodium hydroxide, potassium hydroxide, calcium hydroxide or calcium oxide.
3. out method according to claim 2 is characterized in that, described alkaline matter is sodium hydroxide.
4. treatment process according to claim 1, it is characterized in that: in the step (2), rectification temperature is 90-110 ℃.
5. treatment process according to claim 1, it is characterized in that: in the step (3), multiple-effect evaporation is concentrated into the 60-90% of former weight.
6. treatment process according to claim 1 is characterized in that, in the step (3), also comprises the flue gas heat and the solid that reclaim after burning.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103274380A (en) * | 2013-05-08 | 2013-09-04 | 山东潍坊润丰化工有限公司 | Glyphosate mother liquid treatment method and device |
| CN104591424A (en) * | 2014-03-14 | 2015-05-06 | 山东潍坊润丰化工股份有限公司 | IDA method glyphosate wastewater resource treatment method |
| CN105111088A (en) * | 2015-09-02 | 2015-12-02 | 江苏瑞克医药科技有限公司 | Method for recycling triethylamine from wastewater containing triethylamine hydrochloride |
| CN105130822A (en) * | 2015-09-21 | 2015-12-09 | 四川乐创科技有限公司 | Method for recovering triethylamine, removing phosphorus pollutants and recovering phosphorus resources in glyphosate mother liquor |
| CN105152150A (en) * | 2015-08-12 | 2015-12-16 | 上海泓济环保工程有限公司 | Technology for separating and recovering mother liquor produced during production of catalyst |
| CN105541909A (en) * | 2015-12-07 | 2016-05-04 | 四川乐创科技有限公司 | Method for reducing total phosphor of glyphosate mother liquor subjected to triethylamine recovery |
| CN110396048A (en) * | 2018-04-25 | 2019-11-01 | 刘德亮 | The comprehensive recovering process of glyphosate mother solution |
| CN110393189A (en) * | 2018-04-25 | 2019-11-01 | 刘德亮 | The comprehensive processing technique of glyphosate mother solution |
| CN114105181A (en) * | 2021-09-23 | 2022-03-01 | 浙江巨化技术中心有限公司 | Method for treating waste containing organic phosphorus chlorohydrocarbon |
| CN115784900A (en) * | 2022-11-09 | 2023-03-14 | 湖北泰盛化工有限公司 | Triethylamine purification method in glyphosate production process |
| CN115959643A (en) * | 2022-12-05 | 2023-04-14 | 上海安赐环保科技股份有限公司 | Resource utilization method of byproduct phosphorus salt and byproduct iron salt in steel pickling |
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| CN103274380A (en) * | 2013-05-08 | 2013-09-04 | 山东潍坊润丰化工有限公司 | Glyphosate mother liquid treatment method and device |
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| CN104591424A (en) * | 2014-03-14 | 2015-05-06 | 山东潍坊润丰化工股份有限公司 | IDA method glyphosate wastewater resource treatment method |
| CN105152150A (en) * | 2015-08-12 | 2015-12-16 | 上海泓济环保工程有限公司 | Technology for separating and recovering mother liquor produced during production of catalyst |
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| CN105130822A (en) * | 2015-09-21 | 2015-12-09 | 四川乐创科技有限公司 | Method for recovering triethylamine, removing phosphorus pollutants and recovering phosphorus resources in glyphosate mother liquor |
| CN105541909A (en) * | 2015-12-07 | 2016-05-04 | 四川乐创科技有限公司 | Method for reducing total phosphor of glyphosate mother liquor subjected to triethylamine recovery |
| CN105541909B (en) * | 2015-12-07 | 2017-12-29 | 四川乐创科技有限公司 | A kind of method for reducing total phosphorus in the glyphosate mother solution for having reclaimed triethylamine |
| CN110396048A (en) * | 2018-04-25 | 2019-11-01 | 刘德亮 | The comprehensive recovering process of glyphosate mother solution |
| CN110393189A (en) * | 2018-04-25 | 2019-11-01 | 刘德亮 | The comprehensive processing technique of glyphosate mother solution |
| CN114105181A (en) * | 2021-09-23 | 2022-03-01 | 浙江巨化技术中心有限公司 | Method for treating waste containing organic phosphorus chlorohydrocarbon |
| CN115784900A (en) * | 2022-11-09 | 2023-03-14 | 湖北泰盛化工有限公司 | Triethylamine purification method in glyphosate production process |
| CN115959643A (en) * | 2022-12-05 | 2023-04-14 | 上海安赐环保科技股份有限公司 | Resource utilization method of byproduct phosphorus salt and byproduct iron salt in steel pickling |
| CN115959643B (en) * | 2022-12-05 | 2024-05-03 | 上海安赐环保科技股份有限公司 | Method for recycling byproduct phosphate and iron and steel pickling byproduct ferric salt |
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