CN102766159A - Treatment method of glyphosate alkaline mother solution - Google Patents
Treatment method of glyphosate alkaline mother solution Download PDFInfo
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- CN102766159A CN102766159A CN2012102221230A CN201210222123A CN102766159A CN 102766159 A CN102766159 A CN 102766159A CN 2012102221230 A CN2012102221230 A CN 2012102221230A CN 201210222123 A CN201210222123 A CN 201210222123A CN 102766159 A CN102766159 A CN 102766159A
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- solution
- glyphosate
- mother liquor
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- sodium
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- 239000005562 Glyphosate Substances 0.000 title claims abstract description 53
- XDDAORKBJWWYJS-UHFFFAOYSA-N glyphosate Chemical compound OC(=O)CNCP(O)(O)=O XDDAORKBJWWYJS-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 229940097068 glyphosate Drugs 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000010413 mother solution Substances 0.000 title abstract description 10
- 239000000243 solution Substances 0.000 claims abstract description 112
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 42
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 32
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 27
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims abstract description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000011780 sodium chloride Substances 0.000 claims abstract description 13
- 239000012528 membrane Substances 0.000 claims abstract description 10
- 239000012047 saturated solution Substances 0.000 claims abstract description 9
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 9
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 4
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims description 52
- 239000012452 mother liquor Substances 0.000 claims description 40
- 150000003839 salts Chemical class 0.000 claims description 29
- 235000009508 confectionery Nutrition 0.000 claims description 26
- 229910000073 phosphorus hydride Inorganic materials 0.000 claims description 26
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 16
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 238000003672 processing method Methods 0.000 claims description 9
- 238000005070 sampling Methods 0.000 claims description 8
- 235000017550 sodium carbonate Nutrition 0.000 claims description 8
- 238000004458 analytical method Methods 0.000 claims description 6
- 230000003750 conditioning effect Effects 0.000 claims description 6
- 235000013905 glycine and its sodium salt Nutrition 0.000 claims description 6
- NBZBKCUXIYYUSX-UHFFFAOYSA-N iminodiacetic acid Chemical compound OC(=O)CNCC(O)=O NBZBKCUXIYYUSX-UHFFFAOYSA-N 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 6
- 238000007254 oxidation reaction Methods 0.000 claims description 6
- 159000000000 sodium salts Chemical class 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000005373 pervaporation Methods 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 4
- CZHYKKAKFWLGJO-UHFFFAOYSA-N dimethyl phosphite Chemical compound COP([O-])OC CZHYKKAKFWLGJO-UHFFFAOYSA-N 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000006386 neutralization reaction Methods 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 239000002699 waste material Substances 0.000 abstract description 3
- OXHDYFKENBXUEM-UHFFFAOYSA-N glyphosine Chemical compound OC(=O)CN(CP(O)(O)=O)CP(O)(O)=O OXHDYFKENBXUEM-UHFFFAOYSA-N 0.000 abstract 5
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 abstract 1
- 239000004471 Glycine Substances 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 229910001379 sodium hypophosphite Inorganic materials 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- NCPXQVVMIXIKTN-UHFFFAOYSA-N trisodium;phosphite Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])[O-] NCPXQVVMIXIKTN-UHFFFAOYSA-N 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
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- Agricultural Chemicals And Associated Chemicals (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a treatment method of a glyphosate alkaline mother solution, which comprises the following steps that: a hydrochloric acid is added to the mother solution to adjust the pH of the solution to 1-5 to obtain a solution A; the solution A is subjected to membrane separation to obtain a solution B and a sodium chloride solution, and the sodium chloride solution is evaporated to obtain a saturated solution; and the saturated sodium chloride solution is subjected to the Hou soda process to obtain sodium carbonate to be recycled. The treatment method is characterized in that the solution B is concentrated to make the concentration of a solute in the solution B increase to 3-10 times, i.e. a solution C, and then the appropriate amount of glycine and formaldehyde is added to the solution C, so that glyphosate and phosphorous acid in the solution C are reacted completely to obtain glyphosine and the original glyphosine in the solution C; and the glyphosine is neutralized, leached and dried and the like to obtain a glyphosine solid to be recycled. The treatment method has the advantages that the glyphosate, the glyphosine, sodium hypophosphite and the sodium chloride in the glyphosate alkaline mother solution are fully recycled, the waste is reduced, the pollution is reduced, and the utilization rate of the alkaline mother solution is improved.
Description
Technical field
The present invention relates to a kind of treatment process of glyphosate mother solution, specifically, relate to a kind of treatment process of glyphosate alkaline mother liquor.
Background technology
Utilize the dimethylphosphite method to produce in the Glyphosate 62 IPA Salt process, one ton of Glyphosate 62 IPA Salt of every production probably has six tons of glyphosate mother solutions and produces.Usually contain the Glyphosate 62 IPA Salt of 0.8%-1%, the sodium phosphite that increases sweet phosphine, 2%-3% of 3%-4%, the glycocoll of 0.15%-0.3%, the by product of 1.5%-2%, the sodium-chlor of 10%-14%, sodium hydroxide and the water of 2.5%-3.5% in the glyphosate mother solution.Be that it is concentrated back desalination (or concentrating behind the membrane sepn) to method for processing mother solution of glyphosate at present; Be mixed with 30% gyphosate solution then; The gyphosate solution of preparation 30% need consume a large amount of former powder of high-quality Glyphosate 62 IPA Salt (producing aqua inferior with the former powder of high-quality); And a large amount of sodium phosphite in this aqua, increase sweet phosphine and be not used, contaminate environment not only after the discharging, but also cause waste.In addition, this aqua life-time service makes and is prone to cause soil compaction.Therefore, need a kind of new technical scheme to solve above-mentioned technical problem.
Summary of the invention
The treatment process that the purpose of this invention is to provide a kind of glyphosate mother solution, this method not only can make full use of the sodium phosphite in the alkali liquor, increase sweet phosphine but also can fully recycle.
The technical scheme that the present invention solves the problems of the technologies described above employing is:
Glyphosate alkaline mother liquor processing method, said glyphosate alkaline mother liquor are the alkaline mother liquors of being produced mother liquor remainder in adding alkali and behind the recovery triethylamine wherein of Glyphosate 62 IPA Salt by the dimethylphosphite method; Its treatment process is: get solution A toward the interior adding of this alkaline mother liquor hydrochloric acid conditioning solution pH value to 1-5; Solution A gets solution B and sodium chloride solution through membrane sepn, and said sodium chloride solution makes saturated solution through pervaporation, and saturated nacl aqueous solution makes yellow soda ash through Hou's process for soda production and is recovered utilization; Said solution B makes the concentration of the interior solute of solution B increase to 3-10 doubly through concentrating; Ie in solution C; Then the solution C sampling analysis is gone out the content of each material in the solution C, in solution C, add an amount of glycocoll and formaldehyde, make that Glyphosate 62 IPA Salt and the phosphorous acid in the solution C reacts completely according to analytical data; Increasing of promptly obtaining originally in sweet phosphine and the solution C increases sweet phosphine, obtains increasing sweet phosphine solid through neutralization, suction filtration and drying step and is recovered utilization.
Said solution A is separated out fully through being evaporated to sodium-chlor, crosses then and filters sodium-chlor and solution C, and said sodium-chlor is processed saturated solution and is recovered utilization after Hou's process for soda production gets yellow soda ash.
In the gained solution C, add an amount of iminodiethanoic acid one sodium salt and formaldehyde according to analytical data, make that the phosphorous acid in the solution C reacts completely, make pmida98, said pmida98 makes Glyphosate 62 IPA Salt through oxidation and is recovered utilization.
To said pmida98 be converted into behind the Glyphosate 62 IPA Salt remaining mother liquor carry out sampling analysis, add an amount of formaldehyde and phosphorous acid according to analytical results in the remaining mother liquor and make the Glyphosate 62 IPA Salt in the mother liquor react completely, make and increase sweet phosphine and be recovered utilization.
Also can add an amount of solution C, formaldehyde in the mother liquor of above-mentioned remainder according to analytical results and make that Glyphosate 62 IPA Salt and formolite reaction in the mother liquor of above-mentioned remainder are complete, make and increase sweet phosphine and be recovered utilization.
Said solution B must increase sweet phosphine and solution D behind the secondary membrane sepn; Said solution D is after concentrating; The solution D sampling analysis is gone out the content of each material in the solution D, in solution D, add an amount of iminodiethanoic acid one sodium salt and formaldehyde according to analytical data then, make that the phosphorous acid in the solution D reacts completely; Make pmida98, said pmida98 makes Glyphosate 62 IPA Salt through oxidation and is recovered utilization.
The aperture of said secondary film is less than the molecular diameter that increases sweet phosphine, greater than the molecular diameter of Glyphosate 62 IPA Salt.
Advantage of the present invention is: can be to the Glyphosate 62 IPA Salt in the glyphosate alkaline mother liquor, increase sweet phosphine, sodium phosphite, sodium-chlor and fully recycle, cut the waste, and reduce and pollute, improve the utilization ratio of alkaline mother liquor.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Glyphosate alkaline mother liquor described in following examples is an alkaline mother liquor of being produced mother liquor remainder in adding alkali and behind the recovery triethylamine wherein of Glyphosate 62 IPA Salt by the dimethylphosphite method, and its gross weight is 2Kg.PH value is 12 in this alkaline mother liquor of sampling and measuring, wherein contain 0.8% Glyphosate 62 IPA Salt, 3% increase sweet phosphine, 3% sodium phosphite, 0.3% glycocoll, 14% sodium-chlor, 2.5% sodium hydroxide, other is a water.
Embodiment 1
Get solution A toward the interior hydrochloric acid conditioning solution pH value that adds of above-mentioned alkaline mother liquor to 1-5, at this moment, the sodium phosphite in the solution A is converted into phosphorous acid, sodium hydroxide is converted into sodium-chlor; Solution A gets solution B and sodium chloride solution through membrane sepn, and sodium chloride solution makes saturated solution through pervaporation, and saturated nacl aqueous solution makes yellow soda ash through Hou's process for soda production and is recovered utilization; Solution B makes the concentration of the interior solute of solution B increase to 10 times through concentrating; Ie in solution C; Then toward glycocoll 8.5 grams of the interior adding 98% of solution C and 37% formaldehyde 38.6 grams; Make Glyphosate 62 IPA Salt and phosphorous acid in the solution C react completely, increasing of promptly obtaining originally in sweet phosphine and the solution C increases sweet phosphine, obtains 95% the sweet phosphine solid 98 that increases through neutralization, suction filtration and drying step and restrains and be recovered utilization.Glyphosate 62 IPA Salt, phosphorous acid and formaldehyde in the solution C is synthetic at this moment increases sweet phosphine, and its reaction equation is following:
React incomplete phosphorous acid and increase sweet phosphine and react completely until phosphorous acid with glycocoll and formaldehyde are synthetic again, reaction equation is following:
Embodiment 2
Get solution A toward the interior hydrochloric acid conditioning solution pH value that adds of above-mentioned alkaline mother liquor to 1-5, at this moment, the sodium phosphite in the solution A is converted into phosphorous acid, sodium hydroxide is converted into sodium-chlor; Solution A gets solution B and sodium chloride solution through membrane sepn, and sodium chloride solution makes saturated solution through pervaporation, and saturated nacl aqueous solution makes yellow soda ash through Hou's process for soda production and is recovered utilization; Solution B makes the concentration of the interior solute of solution B increase to 6 times through concentrating; Ie in solution C; In solution C, add folding hundred iminodiethanoic acid one sodium salt, 64 grams and 37% formaldehyde, 45 grams then; Make the phosphorous acid in the solution C react completely, make pmida98, said pmida98 makes Glyphosate 62 IPA Salt through oxidation and is recovered utilization.
The reaction equation that makes pmida98 is following:
To pmida98 be converted into behind the Glyphosate 62 IPA Salt remaining mother liquor carry out sampling and testing, toward mother liquor in, can add an amount of formaldehyde and phosphorous acid or solution C and formaldehyde according to test, make the interior Glyphosate 62 IPA Salt of mother liquor react completely, make and increase sweet phosphine and be recovered utilization.
Embodiment 3
Get solution A toward the interior hydrochloric acid conditioning solution pH value that adds of above-mentioned alkaline mother liquor to 1-5, at this moment, the sodium phosphite in the solution A is converted into phosphorous acid, sodium hydroxide is converted into sodium-chlor; Solution A is separated out fully through being evaporated to sodium-chlor, crosses then and filters sodium-chlor and solution C, and said sodium-chlor is processed saturated solution and is recovered utilization after Hou's process for soda production gets yellow soda ash.
The treating processes embodiment 1 of solution C or embodiment 2.
Embodiment 4
Get solution A toward the interior hydrochloric acid conditioning solution pH value that adds of alkaline mother liquor to 1-5, at this moment, the sodium phosphite in the solution A is converted into phosphorous acid, sodium hydroxide is converted into sodium-chlor; Solution A gets solution B and sodium chloride solution through membrane sepn, and sodium chloride solution makes saturated solution through pervaporation, and saturated nacl aqueous solution makes yellow soda ash through Hou's process for soda production and is recovered utilization; Solution B must increase sweet phosphine and solution D behind the secondary membrane sepn; Solution D makes the concentration of the interior solute of solution D increase to 8 times through concentrating; Add folding hundred iminodiethanoic acid one sodium salt, 64 grams and 37% formaldehyde, 45 grams; Make the phosphorous acid in the solution D react completely, make pmida98, said pmida98 makes Glyphosate 62 IPA Salt through oxidation and is recovered utilization.
Claims (7)
1. glyphosate alkaline mother liquor processing method, said glyphosate alkaline mother liquor be produce Glyphosate 62 IPA Salt by the dimethylphosphite method mother liquor in adding alkali with the triethylamine that reclaims wherein after remaining alkaline mother liquor; Its treatment process is: get solution A toward the interior adding of this alkaline mother liquor hydrochloric acid conditioning solution pH value to 1-5; Solution A gets solution B and sodium chloride solution through membrane sepn, and said sodium chloride solution makes saturated solution through pervaporation, and saturated nacl aqueous solution makes yellow soda ash through Hou's process for soda production and is recovered utilization; It is characterized in that: said solution B makes the concentration of the interior solute of solution B increase to 3-10 doubly through concentrating; Ie in solution C; Then the solution C sampling analysis is gone out the content of each material in the solution C, in solution C, add an amount of glycocoll and formaldehyde, make that Glyphosate 62 IPA Salt and the phosphorous acid in the solution C reacts completely according to analytical data; Increasing of promptly obtaining originally in sweet phosphine and the solution C increases sweet phosphine, obtains increasing sweet phosphine solid through neutralization, suction filtration and drying step and is recovered utilization.
2. glyphosate alkaline mother liquor processing method according to claim 1; It is characterized in that: said solution A is separated out fully through being evaporated to sodium-chlor; Cross then and filter sodium-chlor and solution C, said sodium-chlor is processed saturated solution and is recovered utilization after Hou's process for soda production gets yellow soda ash.
3. glyphosate alkaline mother liquor processing method according to claim 1 and 2; It is characterized in that: in the gained solution C, add an amount of iminodiethanoic acid one sodium salt and formaldehyde according to analytical data; Make the phosphorous acid in the solution C react completely; Make pmida98, said pmida98 makes Glyphosate 62 IPA Salt through oxidation and is recovered utilization.
4. glyphosate alkaline mother liquor processing method according to claim 3; It is characterized in that: to said pmida98 be converted into behind the Glyphosate 62 IPA Salt remaining mother liquor carry out sampling analysis; Add an amount of formaldehyde and phosphorous acid according to analytical results in the remaining mother liquor and make the Glyphosate 62 IPA Salt in the mother liquor react completely, make and increase sweet phosphine and be recovered utilization.
5. glyphosate alkaline mother liquor processing method according to claim 4 is characterized in that: also can add an amount of solution C, formaldehyde in the remaining mother liquor according to analytical results and make the Glyphosate 62 IPA Salt in the mother liquor react completely, make and increase sweet phosphine and be recovered utilization.
6. glyphosate alkaline mother liquor processing method according to claim 1; It is characterized in that: said solution B must increase sweet phosphine and solution D behind the secondary membrane sepn, and said solution D goes out the content of each material in the solution D to the solution D sampling analysis after concentrating; In solution D, add an amount of iminodiethanoic acid one sodium salt and formaldehyde according to analytical data then; Make the phosphorous acid in the solution D react completely, make pmida98, said pmida98 makes Glyphosate 62 IPA Salt through oxidation and is recovered utilization.
7. glyphosate alkaline mother liquor processing method according to claim 6 is characterized in that: the aperture of said secondary film is less than the molecular diameter that increases sweet phosphine, greater than the molecular diameter of Glyphosate 62 IPA Salt.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210222123.0A CN102766159B (en) | 2012-06-18 | 2012-06-18 | Glyphosate alkaline mother liquor processing method |
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| CN201210222123.0A CN102766159B (en) | 2012-06-18 | 2012-06-18 | Glyphosate alkaline mother liquor processing method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105801426A (en) * | 2016-03-19 | 2016-07-27 | 安徽东至广信农化有限公司 | Method for recovering and treating triethylamine tail gas in glyphosate production |
| CN112062141A (en) * | 2020-08-25 | 2020-12-11 | 合众思(北京)环境工程有限公司 | Process for producing sodium chloride and phosphate from sodium hypochlorite wastewater |
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| CN105801426A (en) * | 2016-03-19 | 2016-07-27 | 安徽东至广信农化有限公司 | Method for recovering and treating triethylamine tail gas in glyphosate production |
| CN112062141A (en) * | 2020-08-25 | 2020-12-11 | 合众思(北京)环境工程有限公司 | Process for producing sodium chloride and phosphate from sodium hypochlorite wastewater |
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