CN204310861U - A kind of glyphosate mother solution catalytic oxidation treatment equipment - Google Patents
A kind of glyphosate mother solution catalytic oxidation treatment equipment Download PDFInfo
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- CN204310861U CN204310861U CN201420824153.3U CN201420824153U CN204310861U CN 204310861 U CN204310861 U CN 204310861U CN 201420824153 U CN201420824153 U CN 201420824153U CN 204310861 U CN204310861 U CN 204310861U
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Abstract
The utility model relates to a kind of glyphosate mother solution catalytic oxidation treatment equipment, mother liquor tank is connected with transferpump, be connected with ram pump again after transferpump is connected with static mixer, the tubular heat exchange of plural serial stage is established after ram pump, be provided with Multi-stage sleeve interchanger after tubular heat exchange, double-tube heat exchanger is connected with middle pressure interchanger, and middle pressure interchanger is connected with serpentine reactor, serpentine reactor via line pipeline is connected with double-tube heat exchanger, forms loop.Solve glyphosate mother solution oxidizing reaction incomplete, oxidizing reaction temperature, pressure are high, and danger is comparatively large, reacts realistic problems such as equipment corrosion are larger.After adding homogeneous catalyst, speed of reaction improves greatly, and oxidizing reaction is complete, and apparatus system temperature, pressure reduces, and equipment corrosion improving situation, for glyphosate mother solution ECO process provides a kind of more perfect, reliable technique newly.
Description
Technical field
The utility model relates to a kind of glyphosate mother solution oxide treatment, object be in order to solve glyphosate mother solution oxidizing reaction not exclusively, not high, the equipment of total phosphorus transformation efficiency, COD transformation efficiency dangerous high, run in the problems such as seriously corroded, running cost are high.
Background technology
Glyphosate is a kind of inner sucting conduction type, chronic, efficient, low toxicity, wide spectrum, steriland herbicide, is developed at first by About Monsanto Chemicals, and existing more than 40 years produce, use history.The former powder of glyphosate is the tasteless solid of non-volatile white, about 230 DEG C fusings also with decomposing, being insoluble to common organic solvents, can generating salt, sell after being often mixed with the preparation such as ammonium salt, isopropyl amine salt as terminal agricultural chemicals with inorganic (organic) alkali.Be combined with the metal ion such as iron, aluminium and lose activity very soon after glyphosate buries, seed hiding in soil and soil microorganisms are had no adverse effects.
A large amount of phosphorus-containing wastewaters (hereinafter referred to as " glyphosate mother solution ") can be produced in glyphosate production process, domestic method for processing mother solution of glyphosate configures 10% gyphosate solution sale for adding glyphosate technicals before, but be weakly alkaline due to gyphosate solution and contain impurity and a large amount of salinity (sodium-chlor), life-time service can cause salting of soil, the problem such as harden, the Ministry of Agriculture in 2009, the Ministry of Industry and Information Technology combines No. 1158th, issue bulletin, forbid on December 31st, 2009 produce afterwards active constituent content lower than 30% gyphosate solution, this means that the gyphosate solution of tradition 10% exits China market at this point.Therefore how processing glyphosate mother solution to reach environmental emission standard is the emphasis problem that glyphosate production enterprise must will solve at once, Tai Sheng company takes ECO treating glyphosate mother liquor by oxidation method to achieve significant effect, the total phosphorus of glyphosate mother solution after High Temperature High Pressure oxide treatment in mother liquor is converted into inorganic phosphorus, oxidation solution enters extraction and raffinate after inorganic phosphorus taking-up is entered reverse osmosis membrane interception again, the phosphorous dope tackled out returns ECO system oxide treatment once again, and light liquid (dephosphorization 99%) is sent into MVR system and steamed salt (sodium-chlor) process.
The defect that the method occurs in actual production process, ECO oxide treatment total phosphorus transformation efficiency is on the low side is about about 89%, unconverted phosphorus needs to send ECO process again after reverse osmosis membrane interception, and can not continuity primary treatment put in place, another membrane cartridge consuming cost is higher; COD transformation efficiency is also on the low side, is about about 75%; ECO oxidizing reaction High Temperature High Pressure, have certain risk and equipment corrosion, service life of equipment is shorter.
Current ECO plant running major defect:
Current ECO plant running technology controlling and process index general data:
| Operation item | Technic index | Unit | Operation item | Technic index | Unit |
| System air input | 500 | m 3/h | System pressure | 75-80 | Kilogram |
| Mother liquor amount | 3.33 | m 3/h | System temperature | 250-255 | ℃ |
Summary of the invention
The purpose of this utility model is to provide a kind of glyphosate mother solution catalytic oxidation treatment equipment, mother liquor tank is connected with transferpump, be connected with ram pump again after transferpump is connected with static mixer, the tubular heat exchange of plural serial stage is established after ram pump, be provided with Multi-stage sleeve interchanger after tubular heat exchange, double-tube heat exchanger is connected with middle pressure interchanger, and middle pressure interchanger is connected with serpentine reactor, serpentine reactor via line pipeline is connected with double-tube heat exchanger, forms loop.
Described tubular heat exchange be 1 and more than, further preferably tubular heat exchange is 2, described double-tube heat exchanger be 2 and more than, preferably double-tube heat exchanger is 5 further.
Described tubular heat exchange is arranged with gas-liquid separator, and gas-liquid separator is connected with extraction kettle through transferpump, and gas-liquid separator is also connected with device for absorbing tail gas.
Be connected with volume pump after described mother liquor tank is connected with transferpump, volume pump is connected with catalyzer storage tanks again, and catalyzer storage tanks is connected with catalyzer configured slot.
As follows to glyphosate mother solution catalytic oxidation process for treating according to aforesaid device, the catalyzer copper nitrate trihydrate solution configured and glyphosate mother solution are pumped into static mixer through transferpump, oxidation system is entered with ram pump after mixing, this oxidation system is the circulation loop of tubular heat exchange-double-tube heat exchanger-middle pressure interchanger-coil heat exchanger-double-tube heat exchanger-tubular heat exchange, at the temperature controlling this oxidation system is 210 ± 5 DEG C, pressure is under 4MPa, oxidation solution after oxidation is entered gas-liquid separator from tubular heat exchange, gas after separation is qualified discharge after device for absorbing tail gas process, after being separated, inorganic phosphorus is through extraction, product sodium phosphate salt is obtained after crystallisation by cooling, raffinate send MVR system to steam salt.
Copper nitrate trihydrate solution described in above-mentioned processing step can also replace with cupric nitrate and aluminum oxide mixing suspension or copper sulfate.
In ECO oxide treatment glyphosate mother solution process, in mother liquor, add a small amount of homogeneous catalyst solution and after mixing, enter ECO system, mother liquor increasing temperature and pressure in system makes homogeneous catalyst catalysis mother liquor oxidizing reaction rate, until organism and COD complete oxidation in mother liquor, in oxidation solution, total phosphorus transformation efficiency reaches more than 99%, COD transformation efficiency reaches more than 95%, oxidation solution can directly remain after extractive crystallization raffinate enter MVR system carry out desalination (sodium-chlor) process, do not need to tackle through film again.Due to catalyst action, ECO oxidation system pressure, temperature reduce, and System risk is reduced; Oxidizing reaction is mainly metal ion and organism in catalyzer and occurs to ionize exchange interaction, can greatly reduce the corrodibility to system.
In above-mentioned technique
1, homogeneous catalyst type selecting:
Catalyst grade cupric nitrate, three water (also claiming Gerhardite):
English name: Copper nitrate, trihydrate
Molecular formula: Cu (NO3) 23H2O
Molecular weight: 241.6
Proterties: cupric nitrate has three water, six water, nine water, three kinds of hydrates, and three water things are mazarine styloid, relative density 2.05, fusing point 114.5 DEG C.Heating cupric nitrate decomposes in 170 DEG C subsalt Cu (NO3) 2l Cu (OH) 2 generating indissoluble, continues heating and then changes cupric oxide into.Soluble in water and ethanol, its aqueous solution in acid, the easy moisture absorption.Cupric nitrate is strong oxidizer, heats, rubs or clashes into together with charcoal end, sulphur or other combustiblesubstance, can cause burning and blast.
Purposes: cupric nitrate is used as catalyzer, oxygenant, fluorescent material activator and photovaristor material etc.
Packaging: mould outer volume bag packaging in 25 kilograms, or by customer requirement.
| Technical indicator (HG/T3-931-76) | Catalyst grade | Technical grade |
| Content Cu (NO3) 23H2O% | ≥99.0 | ≥98.0 |
| Water-insoluble % | ≤0.005 | ≤0.1 |
| Muriate (Cl) % | ≤0.005 | ≤0.1 |
| Vitriol (SO4) % | ≤0.02 | ≤0.03-0.05 |
| Iron (Fe) % | ≤0.01 | --- |
| Hydrogen sulfide is throw out (vitriol) % not | ≤0.1 | ≤0.2 |
| Outward appearance | Blue xln | Blue xln |
2, homogeneous catalyst configuration: according to cupric nitrate, three water: pure water=1:0.3-0.8 proportional arrangement aqueous catalyst solution.
3, catalyzer adds: the catalyst solution configured squeezes into hold-up vessel, to squeeze into after mother liquor transferpump in mother liquor pipeline through self-priming volume pump again, catalyst solution: mother liquor=1-1.5:10000, make it fully to mix with mother liquor through static mixer, enter ECO system inlets ram pump, enter ECO device through ram pump.
4, ECO system process controls: system temperature vertex controls at 210 DEG C ± 5 DEG C, system pressure 40 kilograms.
Following and the beneficial effect of unique advantage of the present invention:
1, enter oxidation solution after homogeneous catalyst completes katalysis in this process treatment process finally to enter in Product mix sodium phosphate, do not affect quality product.
2, increase catalyzer configuration dnockout static mixing system in the present invention program, increase plant area little, input cost is little, and increase at former ECO system front end, ECO system ontology need not make change.
3, increasing device technique controls simple, and human users's difficulty is little.
4, this invention makes the Hazard Factor that in ECO plant running, High Temperature High Pressure may be brought greatly reduce.
5, this invention improves the rate of oxidation of total phosphorus and COD in glyphosate mother solution, directly eliminates raffinate liquid film treatment process and drops into, further ensure that the reliability that mother liquid disposal environment protection standard is discharged.
6, this invention can effectively reduce ECO system running pressure and temperature, provides new lectotype selection direction, greatly save new device equipment investment for second phase enlarging ECO new device.
7, this invention reduces greatly for new device equipment material requirements of type selecting, greatly saves new device equipment investment.
Accompanying drawing explanation
Fig. 1 is glyphosate mother solution catalytic oxidation treatment equipment, wherein 1. mother liquor tanks, 2. transferpump, 3. static mixer, 4. ram pump, 5-1,2. tubular heat exchange, 6-1,-2 ,-3 ,-4,-5. double-tube heat exchangers, press interchanger 7., 8. coil heat exchanger, 9. gas-liquid separator, 10. extraction kettle, 11. device for absorbing tail gas, 12. volume pumps, 13. catalyzer storage tankss, 14. catalyzer configured slots.
Embodiment
Embodiment 1
A kind of glyphosate mother solution catalytic oxidation treatment equipment, mother liquor tank 1 is connected with transferpump 2, transferpump 2 is connected with ram pump 4 after being connected with static mixer 3 again, 2 grades of tubular heat exchanges of connecting 5 are established after ram pump 4, the double-tube heat exchanger 6 of 5 grades of series connection is provided with after tubular heat exchange 5, double-tube heat exchanger 6 is connected with serpentine reactor 8 after being connected with middle pressure interchanger 7 again, and serpentine reactor 8 via line pipeline is connected with last step double-tube heat exchanger 6, forms loop.
First step tubular heat exchange 5 is arranged with gas-liquid separator 9, and gas-liquid separator 9 is connected with extraction kettle 10 through transferpump, and gas-liquid separator 9 is also connected with device for absorbing tail gas 11.
Mother liquor tank 1 is connected with volume pump 12 after being connected with transferpump 2 again, and volume pump 12 is connected with catalyzer storage tanks 13, and catalyzer storage tanks 13 is connected with catalyzer configured slot 14.
The utility model utilizes Gerhardite to have strong catalytic feature, Gerhardite starts to decompose at 170 DEG C, its cupric ion can reduce organophosphorus and macromole COD just point reactive behavior energy, improve its oxidizing reaction rate, under the condition of temperature and pressure far below ECO plant running state of art, make phosphorus in mother liquor, COD is converted into small molecules inorganic phosphorus and micro-molecular gas, gas is qualified discharge after the process of ammonia nitrogen absorption unit, inorganic phosphorus goes out product mixed phosphate sodium salt (being not less than the Sodium phosphate dibasic of 90%) through extraction process crystallisation by cooling, MVR operation of sending raffinate continues to do steams salt (sodium-chlor) process.
A kind of glyphosate mother solution catalytic oxidation process for treating, the catalyzer copper nitrate trihydrate solution configured and glyphosate mother solution are pumped into static mixer through transferpump, oxidation system is entered with ram pump after mixing, this oxidation system is the circulation loop of tubular heat exchange-double-tube heat exchanger-middle pressure interchanger-coil heat exchanger-double-tube heat exchanger-tubular heat exchange, at the temperature controlling this oxidation system is 210 ± 5 DEG C, pressure is under 4MPa, oxidation solution after oxidation is entered gas-liquid separator from tubular heat exchange, gas after separation is qualified discharge after device for absorbing tail gas process, after being separated, inorganic phosphorus is through extraction, product sodium phosphate salt is obtained after crystallisation by cooling, raffinate send MVR system to steam salt.
In described copper nitrate trihydrate solution, the mass ratio of copper nitrate trihydrate and water is 1:0.5; The mass ratio of copper nitrate trihydrate solution and mother liquor is 1:10000.
Described copper nitrate trihydrate solution can also replace with cupric nitrate and aluminum oxide mixing suspension or copper sulfate.
Through inspection, obtain Sodium phosphate dibasic target level of product quality in product as follows:
| Interventions Requested | Assay |
| Sodium phosphate dibasic (Na2HPO4.12H2O meter) | 90.03％ |
| Moisture | 63.27％ |
| Water-insoluble | 0.06％ |
| PH value (1% aqueous solution) | 9.18 |
| Muriate | ≤0.05 |
| Iron level | ≤0.0020 |
| Outward appearance | White granular is containing wet crystal |
Embodiment 2
All processing steps of the present embodiment are as embodiment 1, and only catalyzer is copper sulfate solution.The quality standard of the product obtained is:
| Interventions Requested | Assay |
| Sodium phosphate dibasic (Na2HPO4.12H2O meter) | 91.08％ |
| Moisture | 62.53％ |
| Water-insoluble | 0.06％ |
| PH value (1% aqueous solution) | 9.1 |
| Muriate | ≤0.05 |
| Iron level | ≤0.0020 |
| Outward appearance | White granular is containing wet crystal |
Embodiment 3
All processing steps of the present embodiment are as embodiment 1, and only catalyzer is cupric nitrate and aluminum oxide mixing suspension.The quality standard of the product obtained is:
| Interventions Requested | Assay |
| Sodium phosphate dibasic (Na2HPO4.12H2O meter) | 92.02％ |
| Moisture | 60.53％ |
| Water-insoluble | 0.05％ |
| PH value (1% aqueous solution) | 9.12 |
| Muriate | ≤0.05 |
| Iron level | ≤0.0020 |
| Outward appearance | White granular is containing wet crystal |
Claims (5)
1. a glyphosate mother solution catalytic oxidation treatment equipment, it is characterized in that: mother liquor tank (1) is connected with transferpump (2), transferpump (2) is connected with ram pump (4) after being connected with static mixer (3) again, the tubular heat exchange (5) of plural serial stage is established after ram pump (4), Multi-stage sleeve interchanger (6) is provided with after tubular heat exchange (5), double-tube heat exchanger (6) is connected with middle pressure interchanger (7), middle pressure interchanger (7) is connected with serpentine reactor (8), serpentine reactor (8) via line pipeline is connected with double-tube heat exchanger (6), form loop.
2. equipment according to claim 1, is characterized in that: described tubular heat exchange (5) be 1 and more than, described double-tube heat exchanger (6) be 2 and more than.
3. equipment according to claim 1, is characterized in that: described tubular heat exchange (5) is 2, and described double-tube heat exchanger (6) is 5.
4. equipment according to claim 1, it is characterized in that: tubular heat exchange (5) is arranged with gas-liquid separator (9), gas-liquid separator (9) is connected with extraction kettle (10) through transferpump, and gas-liquid separator (9) is also connected with device for absorbing tail gas (11).
5. equipment according to claim 1, it is characterized in that: mother liquor tank (1) is connected with volume pump (12) after being connected with transferpump (2) again, volume pump (12) is connected with catalyzer storage tanks (13), and catalyzer storage tanks (13) is connected with catalyzer configured slot (14).
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| Application Number | Priority Date | Filing Date | Title |
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| CN201420824153.3U CN204310861U (en) | 2014-12-23 | 2014-12-23 | A kind of glyphosate mother solution catalytic oxidation treatment equipment |
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| CN201420824153.3U CN204310861U (en) | 2014-12-23 | 2014-12-23 | A kind of glyphosate mother solution catalytic oxidation treatment equipment |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104556343A (en) * | 2014-12-23 | 2015-04-29 | 湖北泰盛化工有限公司 | Glyphosate mother liquor catalytic oxidation treatment equipment and process |
| CN104828798A (en) * | 2015-05-20 | 2015-08-12 | 湖北泰盛化工有限公司 | Device and method for extracting sodium dihydrogen phosphate dihydrate by using crude brine in glyphosate production process through glycine method |
| CN106816489A (en) * | 2017-02-28 | 2017-06-09 | 安徽拓吉泰新型陶瓷科技有限公司 | A kind of light sensitive resistance ceramics and preparation method thereof |
-
2014
- 2014-12-23 CN CN201420824153.3U patent/CN204310861U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104556343A (en) * | 2014-12-23 | 2015-04-29 | 湖北泰盛化工有限公司 | Glyphosate mother liquor catalytic oxidation treatment equipment and process |
| CN104828798A (en) * | 2015-05-20 | 2015-08-12 | 湖北泰盛化工有限公司 | Device and method for extracting sodium dihydrogen phosphate dihydrate by using crude brine in glyphosate production process through glycine method |
| CN106816489A (en) * | 2017-02-28 | 2017-06-09 | 安徽拓吉泰新型陶瓷科技有限公司 | A kind of light sensitive resistance ceramics and preparation method thereof |
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