CN106044731A - Method for preparing disodium hydrogen phosphate based on glyphosate mother solution - Google Patents
Method for preparing disodium hydrogen phosphate based on glyphosate mother solution Download PDFInfo
- Publication number
- CN106044731A CN106044731A CN201610665750.XA CN201610665750A CN106044731A CN 106044731 A CN106044731 A CN 106044731A CN 201610665750 A CN201610665750 A CN 201610665750A CN 106044731 A CN106044731 A CN 106044731A
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- CN
- China
- Prior art keywords
- mother solution
- disodium hydrogen
- crystallization
- glyphosate mother
- hydrogen phosphate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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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
Abstract
The invention discloses a method for preparing disodium hydrogen phosphate based on a glyphosate mother solution, wherein the method comprises the following steps: (1) adjusting the pH value of the glyphosate mother solution, and then allowing the glyphosate mother solution to enter an MVR evaporator; (2) transferring the whole material into a crystallization kettle, and carrying out normal pressure crystallization; (3) after the material is crystallized, carrying out solid-liquid separation; (4) carrying out normal pressure degradation in a catalytic degradation tower; (5) extracting sodium chloride, disodium hydrogen phosphate and trisodium phosphate, cooling wastewater after degradation to room temperature through heat transfer, then transferring into an extraction tank, carrying out cooling crystallization operation, transporting an extract liquid after crystallization to a two-in-one filter press through a pump, and filtering; and (6) washing a solid after filtration with water for two times, then discharging, and packing for sale. The MVR evaporator is used for concentration, so the purity of the product can be ensured; the glyphosate wastewater is subjected to catalytic degradation by an electrocatalytic oxidation technology, sodium chloride, disodium hydrogen phosphate and trisodium phosphate are extracted to be used as by-products, and the costs are saved.
Description
Technical field
The present invention relates to the preparation method of disodium hydrogen phosphate, be specifically related to a kind of based on glyphosate mother solution preparing phosphoric acid hydrogen two
The method of sodium.
Background technology
Glyphosate be a kind of efficiently, go out after the bud of low toxicity, low-residual, broad weed-killing spectrum natural disposition highy potent herbicide, has good
Interior suction, conductive performance.Maximum for consumption in the world today, the herbicide kind of the most violent the most most market competitiveness of growth
One of.But the production of glyphosate is also along with the generation of a large amount of waste water, and the pollution problem of glyphosate production mainly shows as simultaneously
Waste water, this waste water has that discharge capacity is big, pollutant levels are high, toxicity is big, salinity is high, difficult degradation compounds content is high, administer
The features such as difficulty is big.The application of pollutant control technology at present lags behind the development of product.Glyphosate waste water is administered becomes puzzlement
One of difficult problem of industry, is the sector common problem in the urgent need to address.
Phosphor resource, salt aboundresources in glyphosate mother solution, wastewater flow rate is relatively big, to Phosphorus From Wastewater, salt, water resource recovery again
Utilize, it is achieved the production of by-product industrialization, economic benefit can be significantly improved, it is achieved industrialization produces.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of side based on glyphosate mother solution preparing phosphoric acid disodium hydrogen
Method.
The present invention can be achieved through the following technical solutions:
A kind of method based on glyphosate mother solution preparing phosphoric acid disodium hydrogen, described step is:
(1) glyphosate mother solution is adjusted pH value to after 10-11, enters MVR vaporizer, beforehand control temperature at 70-80 DEG C,
Latter stage, temperature controlled at 85-95 DEG C, and vacuum degree control is at-0.08MPa；
(2) when the enrichment of glyphosate mother solution is at 30-60%, in material is transferred completely into crystallization kettle, normal pressure knot is carried out
Crystalline substance, controls crystallization temperature and is 0-10 DEG C, and the time is 1-3h；
(3) after material crystallizes, carry out solid-liquid separation, isolate sodium chloride crude product, after desalinization of soil by flooding or leaching equipment clean, reach industry
Product salt standard；
(4), after the evaporation residual liquid of the liquid material in step 3 and step 1 being mixed, carry out in transferring to catalytic degradation tower
Normal pressure is degraded, and controls degradation temperature and is 120-150 DEG C, and the time is 5-8h；
(5) after having degraded, therefrom extracting sodium chloride, disodium hydrogen phosphate, tertiary sodium phosphate, the waste water after degraded drops through heat exchange
To room temperature, carrying out crystallisation by cooling operation in transferring to extraction tank, the extract after crystallization is through being pumped into two-in-one press filter
Filter；
(6) the solid spout bag after twice washing after filtering takes on sells, and filtrate carries out membrane filtration, it is ensured that waste water
Effluent quality is preferable, it is ensured that subsequent treatment energy qualified discharge.
Further, the catalytic degradation tower described in step 4 is electrocatalytic oxidation degradation tower.
The invention have the benefit that 1) utilize MVR vaporizer to concentrate, it can be ensured that the purity of product；2) utilize
Electro-catalytic oxidation technology carries out catalytic degradation to glyphosate waste water, therefrom can extract sodium chloride, disodium hydrogen phosphate, tricresyl phosphate
Sodium, as side-product, cost-effective, resource also recoverable；3) two-in-one Filter Press separation and recovery is utilized effectively to become
Point.
Detailed description of the invention:
By embodiment, the detailed description of the invention of the present invention is made an explanation below.
Embodiment
A kind of method based on glyphosate mother solution preparing phosphoric acid disodium hydrogen, described step is: (1) glyphosate mother solution is through adjusting
Joint pH value, to after 10, enters MVR vaporizer, and beforehand control temperature is at 75 DEG C, and latter stage, temperature controlled at 90 DEG C, vacuum degree control
At-0.08MPa；(2) when the enrichment of glyphosate mother solution is 50%, in material is transferred completely into crystallization kettle, normal pressure knot is carried out
Crystalline substance, controlling crystallization temperature is 5 DEG C, and the time is 1h；(3) after material crystallizes, carry out solid-liquid separation, isolate sodium chloride crude product, warp
Nacl product standard is reached after desalinization of soil by flooding or leaching equipment clean；(4) the evaporation residual liquid of the liquid material in step 3 and step 1 is mixed
After, carry out normal pressure degraded in transferring to electrocatalytic oxidation degradation tower, controlling degradation temperature is 130 DEG C, and the time is 5h；(5) degraded
After completing, therefrom extracting sodium chloride, disodium hydrogen phosphate, tertiary sodium phosphate, the waste water after degraded, after room temperature is down in heat exchange, is transferred to
Carrying out crystallisation by cooling operation in extraction tank, the extract after crystallization is through being pumped into two-in-one Filter Press；(6) after filtering
Solid spout bag after twice washing takes on sells, and filtrate carries out membrane filtration, it is ensured that the effluent quality of waste water is preferable, it is ensured that after
Continuous process can qualified discharge.
The invention have the benefit that 1) utilize MVR vaporizer to concentrate, it can be ensured that the purity of product；2) utilize
Electro-catalytic oxidation technology carries out catalytic degradation to glyphosate waste water, therefrom can extract sodium chloride, disodium hydrogen phosphate, tricresyl phosphate
Sodium, as side-product, cost-effective, resource also recoverable；3) two-in-one Filter Press separation and recovery is utilized effectively to become
Point.
Claims (2)
1. a method based on glyphosate mother solution preparing phosphoric acid disodium hydrogen, it is characterised in that described step is:
(1) glyphosate mother solution through pH value regulate after, enter MVR vaporizer, beforehand control temperature at 70-80 DEG C, temperature control in latter stage
System is at 85-95 DEG C, and vacuum degree control is at-0.08MPa；
(2) when the enrichment of glyphosate mother solution is at 30-60%, in material is transferred completely into crystallization kettle, normal pressure crystallization is carried out,
Controlling crystallization temperature and be 0-10 DEG C, the time is 1-3h；
(3) after material crystallizes, carry out solid-liquid separation, isolate sodium chloride crude product, after desalinization of soil by flooding or leaching equipment clean, reach Nacl produce
Product standard；
(4), after being mixed by the evaporation residual liquid of the liquid material in step 3 and step 1, in transferring to catalytic degradation tower, normal pressure is carried out
Degraded, controls degradation temperature and is 120-150 DEG C, and the time is 5-8h；
(5) after having degraded, therefrom extracting sodium chloride, disodium hydrogen phosphate, tertiary sodium phosphate, the waste water after degraded is down to room through heat exchange
Wen Hou, carries out crystallisation by cooling operation in transferring to extraction tank, and the extract after crystallization is through being pumped into two-in-one Filter Press；
(6) the solid spout bag after twice washing after filtering takes on sells, and filtrate carries out membrane filtration, it is ensured that the water outlet of waste water
Water quality is preferable, it is ensured that subsequent treatment energy qualified discharge.
A kind of method based on glyphosate mother solution preparing phosphoric acid disodium hydrogen the most according to claim 1, it is characterised in that step
Catalytic degradation tower described in rapid 4 is electrocatalytic oxidation degradation tower.
Priority Applications (1)
| 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 |
Applications Claiming Priority (1)
| 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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106044731A true CN106044731A (en) | 2016-10-26 |
| CN106044731B CN106044731B (en) | 2018-10-23 |
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| Application Number | Title | Priority Date | Filing Date |
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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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Cited By (2)
| 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 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103012474A (en) * | 2012-12-31 | 2013-04-03 | 浙江金帆达生化股份有限公司 | Cyclic 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 |
| CN104310692A (en) * | 2014-11-14 | 2015-01-28 | 许昌东方化工有限公司 | Method for treating glyphosate mother liquid |
| CN104944398A (en) * | 2015-06-29 | 2015-09-30 | 江西金龙化工有限公司 | Method for recycling glyphosate mother solution |
-
2016
- 2016-08-13 CN CN201610665750.XA patent/CN106044731B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103012474A (en) * | 2012-12-31 | 2013-04-03 | 浙江金帆达生化股份有限公司 | Cyclic 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 |
| CN104310692A (en) * | 2014-11-14 | 2015-01-28 | 许昌东方化工有限公司 | Method for treating glyphosate mother liquid |
| CN104944398A (en) * | 2015-06-29 | 2015-09-30 | 江西金龙化工有限公司 | Method for recycling glyphosate mother solution |
Cited By (2)
| 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 |
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| Publication number | Publication date |
|---|---|
| CN106044731B (en) | 2018-10-23 |
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