CN106044731B - A method of based on glyphosate mother solution preparing phosphoric acid disodium hydrogen - Google Patents
A method of based on glyphosate mother solution preparing phosphoric acid disodium hydrogen Download PDFInfo
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- CN106044731B CN106044731B CN201610665750.XA CN201610665750A CN106044731B CN 106044731 B CN106044731 B CN 106044731B CN 201610665750 A CN201610665750 A CN 201610665750A CN 106044731 B CN106044731 B CN 106044731B
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- crystallization
- disodium hydrogen
- mother solution
- degradation
- glyphosate mother
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/30—Alkali metal phosphates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Treatment Of Water By Ion Exchange (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The invention discloses a kind of method based on glyphosate mother solution preparing phosphoric acid disodium hydrogen, step is：(1) glyphosate mother solution is after pH value adjustment, into MVR evaporators；(2) material is transferred completely into progress normal pressure crystallization in crystallization kettle；(3) it is separated by solid-liquid separation after material crystallization；(4) normal pressure degradation is carried out in catalytic degradation tower；(5) sodium chloride, disodium hydrogen phosphate, tertiary sodium phosphate are extracted, the waste water after degradation is cooled to room temperature through heat exchange, is transferred in extraction tank and is carried out crystallisation by cooling operation, and the extract liquor after crystallization is transported to the filtering of two-in-one press filter through pump；(6) filtered solid spout bag after washing twice, which takes on, sells.The present invention is concentrated using MVR evaporators, it can be ensured that the purity of product；Catalytic degradation is carried out to glyphosate waste water using electro-catalytic oxidation technology, can therefrom extract sodium chloride, disodium hydrogen phosphate, tertiary sodium phosphate, as byproduct, saves cost.
Description
Technical field
The present invention relates to the preparation methods of disodium hydrogen phosphate, and in particular to one kind being based on glyphosate mother solution preparing phosphoric acid hydrogen two
The method of sodium.
Background technology
Glyphosate be it is a kind of efficiently, go out natural disposition highy potent herbicide after the bud of low toxicity, low-residual, broad weed-killing spectrum, have well
Interior suction, conductive performance.It is maximum for dosage in the world today, the most violent also most herbicide kind of the market competitiveness of growth
One of.But also along with the generation of a large amount of waste water, the pollution problem of glyphosate production is mainly shown as the production of glyphosate simultaneously
Waste water, the waste water is with discharge capacity is big, pollutant concentration is high, toxicity is big, salt content is high, compounds content difficult to degrade is high, administers
The features such as difficulty is big.The application of pollutant control technology lags behind the development of product at present.Glyphosate waste water, which is administered, becomes puzzlement
One of problem of industry is the sector common problem in the urgent need to address.
Phosphor resource, salt are resourceful in glyphosate mother solution, and wastewater flow rate is larger, to Phosphorus From Wastewater, salt, water resource recycling again
It utilizes, realizes the production of by-product industrialization, economic benefit can be significantly improved, realize industrialization production.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of sides based on glyphosate mother solution preparing phosphoric acid disodium hydrogen
Method.
The present invention can be achieved through the following technical solutions：
A method of based on glyphosate mother solution preparing phosphoric acid disodium hydrogen, the described method comprises the following steps：
(1) glyphosate mother solution is after the adjustment after pH value to 10-11, into MVR evaporators, beforehand control temperature at 70-80 DEG C,
Latter stage temperature is controlled at 85-95 DEG C, and vacuum degree control is in -0.08MPa；
(2) when the enrichment of glyphosate mother solution is in 30-60%, material is transferred completely into progress normal pressure knot in crystallization kettle
Crystalline substance, control crystallization temperature are 0-10 DEG C, time 1-3h；
(3) it is separated by solid-liquid separation after material crystallization, isolates sodium chloride crude product, industry is reached after desalinization of soil by flooding or leaching equipment clean
Product salt standard；
(4) it after mixing the evaporation raffinate of liquid material and step (1) in step (3), is transferred in catalytic degradation tower
Normal pressure degradation is carried out, control degradation temperature is 120-150 DEG C, time 5-8h；
(5) after the completion of degrading, sodium chloride, disodium hydrogen phosphate, tertiary sodium phosphate are therefrom extracted, the waste water after degradation is dropped through heat exchange
It to room temperature, is transferred in extraction tank and carries out crystallisation by cooling operation, the extract liquor after crystallization is transported to two-in-one press filter through pump
Filtering；
(6) filtered solid spout bag after washing twice, which takes on, sells, and filtered fluid carries out membrane filtration, ensures waste water
Effluent quality is preferable, it is ensured that subsequent processing energy qualified discharge.
Further, the catalytic degradation tower described in step (4) is Electro-catalytic Oxidation Process tower.
Beneficial effects of the present invention are：1) it is concentrated using MVR evaporators, it can be ensured that the purity of product；2) it utilizes
Electro-catalytic oxidation technology carries out catalytic degradation to glyphosate waste water, can therefrom extract sodium chloride, disodium hydrogen phosphate, tricresyl phosphate
Sodium saves cost as byproduct, resource also recoverable；3) using two-in-one press filter be separated by filtration recycling effectively at
Point.
Specific implementation mode：
It is made an explanation below to the specific implementation mode of the present invention with embodiment.
Embodiment
A method of based on glyphosate mother solution preparing phosphoric acid disodium hydrogen, the described method comprises the following steps：(1) glyphosate
PH value is to after 10 after the adjustment for mother liquor, and into MVR evaporators, beforehand control temperature is at 75 DEG C, and the control of latter stage temperature is at 90 DEG C, vacuum
Degree control is in -0.08MPa；(2) when the enrichment of glyphosate mother solution is 50%, material is transferred completely into crystallization kettle and is carried out
Normal pressure crystallizes, and control crystallization temperature is 5 DEG C, time 1h；(3) it is separated by solid-liquid separation after material crystallization, isolates sodium chloride
Crude product reaches Nacl product standard after desalinization of soil by flooding or leaching equipment clean；(4) by the steaming of liquid material and step (1) in step (3)
It after sending out raffinate mixing, is transferred in Electro-catalytic Oxidation Process tower and carries out normal pressure degradation, control degradation temperature is 130 DEG C, and the time is
5h；(5) after the completion of degrading, sodium chloride, disodium hydrogen phosphate, tertiary sodium phosphate are therefrom extracted, the waste water after degradation is down to room through heat exchange
Wen Hou is transferred in extraction tank and carries out crystallisation by cooling operation, and the extract liquor after crystallization is transported to the filtering of two-in-one press filter through pump；
(6) filtered solid spout bag after washing twice, which takes on, sells, and filtered fluid carries out membrane filtration, ensures the effluent quality of waste water
Preferably, it is ensured that subsequent processing energy qualified discharge.
Beneficial effects of the present invention are：1) it is concentrated using MVR evaporators, it can be ensured that the purity of product；2) it utilizes
Electro-catalytic oxidation technology carries out catalytic degradation to glyphosate waste water, can therefrom extract sodium chloride, disodium hydrogen phosphate, tricresyl phosphate
Sodium saves cost as byproduct, resource also recoverable；3) using two-in-one press filter be separated by filtration recycling effectively at
Point.
Claims (2)
1. a kind of method based on glyphosate mother solution preparing phosphoric acid disodium hydrogen, which is characterized in that the described method comprises the following steps：
(1) glyphosate mother solution is after pH value is adjusted, and into MVR evaporators, beforehand control temperature is at 70-80 DEG C, latter stage temperature control
System is at 85-95 DEG C, and vacuum degree control is in -0.08MPa；
(2) when the enrichment of glyphosate mother solution is in 30-60%, material is transferred completely into progress normal pressure crystallization in crystallization kettle,
It is 0-10 DEG C to control crystallization temperature, time 1-3h；
(3) it is separated by solid-liquid separation after material crystallization, isolates sodium chloride crude product, Nacl production is reached after desalinization of soil by flooding or leaching equipment clean
Product standard；
(4) it after mixing the evaporation raffinate of liquid material and step (1) in step (3), is transferred in catalytic degradation tower and carries out
Normal pressure is degraded, and control degradation temperature is 120-150 DEG C, time 5-8h；
(5) after the completion of degrading, sodium chloride, disodium hydrogen phosphate, tertiary sodium phosphate are therefrom extracted, the waste water after degradation is down to room through heat exchange
Wen Hou is transferred in extraction tank and carries out crystallisation by cooling operation, and the extract liquor after crystallization is transported to the filtering of two-in-one press filter through pump；
(6) filtered solid spout bag after washing twice, which takes on, sells, and filtered fluid carries out membrane filtration, ensures the water outlet of waste water
Water quality is preferable, it is ensured that subsequent processing energy qualified discharge.
2. a kind of method based on glyphosate mother solution preparing phosphoric acid disodium hydrogen according to claim 1, which is characterized in that step
Suddenly the catalytic degradation tower described in (4) is Electro-catalytic Oxidation Process tower.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610665750.XA CN106044731B (en) | 2016-08-13 | 2016-08-13 | A method of based on glyphosate mother solution preparing phosphoric acid disodium hydrogen |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610665750.XA CN106044731B (en) | 2016-08-13 | 2016-08-13 | A method of based on glyphosate mother solution preparing phosphoric acid disodium hydrogen |
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| CN106044731A CN106044731A (en) | 2016-10-26 |
| CN106044731B true CN106044731B (en) | 2018-10-23 |
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| CN201610665750.XA Active CN106044731B (en) | 2016-08-13 | 2016-08-13 | A method of based on glyphosate mother solution preparing phosphoric acid disodium hydrogen |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107902825A (en) * | 2017-10-30 | 2018-04-13 | 安徽东至广信农化有限公司 | A kind of method using ECO methods preparing phosphoric acid disodium hydrogen from glyphosate mother solution |
| CN109704367A (en) * | 2018-12-27 | 2019-05-03 | 镇江江南化工有限公司 | A kind of glyphosate by-product Nacl process for refining and purifying |
| CN114044527A (en) * | 2021-09-30 | 2022-02-15 | 北京航天环境工程有限公司 | Recycling system and process method of waste glyphosate salt |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103012474B (en) * | 2012-12-31 | 2016-05-18 | 浙江金帆达生化股份有限公司 | A kind of circular production method of glyphosate |
| CN103288065A (en) * | 2013-05-08 | 2013-09-11 | 浙江悦瑞环保工程有限公司 | Process for preparing disodium hydrogen phosphate from glyphosate |
| CN104310692B (en) * | 2014-11-14 | 2016-08-24 | 河南红东方化工股份有限公司 | The processing method of glyphosate mother solution |
| CN104944398B (en) * | 2015-06-29 | 2017-09-19 | 江西金龙化工有限公司 | Glyphosate mother solution recoverying and utilizing method |
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