CN101314607A - Method for recycling glyphosine from mother solution for preparing glyphosine - Google Patents
Method for recycling glyphosine from mother solution for preparing glyphosine Download PDFInfo
- Publication number
- CN101314607A CN101314607A CNA2008101244031A CN200810124403A CN101314607A CN 101314607 A CN101314607 A CN 101314607A CN A2008101244031 A CNA2008101244031 A CN A2008101244031A CN 200810124403 A CN200810124403 A CN 200810124403A CN 101314607 A CN101314607 A CN 101314607A
- Authority
- CN
- China
- Prior art keywords
- pmida98
- mother liquor
- glyphosine
- phosphonomethyl
- steps
- 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.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 9
- OXHDYFKENBXUEM-UHFFFAOYSA-N glyphosine Chemical compound OC(=O)CN(CP(O)(O)=O)CP(O)(O)=O OXHDYFKENBXUEM-UHFFFAOYSA-N 0.000 title 2
- 239000010413 mother solution Substances 0.000 title 1
- 238000004064 recycling Methods 0.000 title 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- 238000003795 desorption Methods 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims abstract description 12
- 238000004065 wastewater treatment Methods 0.000 claims abstract description 8
- 239000012266 salt solution Substances 0.000 claims abstract description 7
- 159000000000 sodium salts Chemical class 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 238000001179 sorption measurement Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000012452 mother liquor Substances 0.000 claims description 19
- 239000011347 resin Substances 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 8
- 238000010521 absorption reaction Methods 0.000 claims description 6
- 230000020477 pH reduction Effects 0.000 claims description 2
- 238000012856 packing Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 238000002203 pretreatment Methods 0.000 claims description 2
- 239000003957 anion exchange resin Substances 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 abstract description 3
- FDQQNNZKEJIHMS-UHFFFAOYSA-N 3,4,5-trimethylphenol Chemical compound CC1=CC(O)=CC(C)=C1C FDQQNNZKEJIHMS-UHFFFAOYSA-N 0.000 abstract 4
- 238000001914 filtration Methods 0.000 abstract 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 239000001117 sulphuric acid Substances 0.000 description 2
- 235000011149 sulphuric acid Nutrition 0.000 description 2
- 241000406668 Loxodonta cyclotis Species 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Abstract
A method for recovering N-(Phosphonomethyl) iminodiacetic acid from the mother liquid thereof comprises the steps as follows: fine-filtering the mother liquid to obtain a clear mother liquid; adsorbing at a flow rate of 2-12BV/h in an anion exchange resin adsorption column at 5-30 DEG C and subjecting the discharge water to the waste water treatment; desorbing with 3-8% sodium hydroxide solution as the desorption solution at a flow rate of 1-4BV/h at 25-50 DEG C to obtain a sodium salt solution of N-(Phosphonomethyl) iminodiacetic acid; and subjecting to acidization to obtain N-(Phosphonomethyl) iminodiacetic acid. The method carries out the recovery of N-(Phosphonomethyl) iminodiacetic acid from the mother liquid thereof before the waste water treatment, thereby reducing the resource consumption and improving the economic benefit on one hand, and reducing the difficulty and the cost of the waste water treatment on the other hand.
Description
Technical field
The present invention relates to the production method of pmida98, specifically, relate to the method that from the mother liquor of producing pmida98, reclaims pmida98.
Background technology
Pmida98 (N-(phosphonic acids methyl) imido oxalic acid) is produced in the mother liquor, except that the pmida98 that contains about 1.5%, also contains the hydrochloric acid, imido oxalic acid of higher concentration etc., produces at present and goes up the pmida98 mother liquor directly as wastewater treatment.Pmida98 did not both reclaim, and had wasted useful resources, had increased the intractability of waste water again.
Summary of the invention
The present invention adopts resin to reclaim the method for pmida98, be meant that specifically a kind of employing anionite-exchange resin adsorbs pmida98 under PH1-5,5-40 ℃, flow velocity 2-12BV/h condition, use sig water (is representative with the sodium hydroxide solution) to carry out desorption again, reclaim pmida98.
The objective of the invention is to be achieved through the following technical solutions:
A kind of method that from the mother liquor of producing pmida98, reclaims pmida98, it is made up of following steps:
Steps A: will produce the pmida98 mother liquor of pmida98, and, obtain clarified mother liquor through secondary filter;
Step B: the anionite-exchange resin of in adsorption column, packing into, after conventional pre-treatment, the pmida98 clarified mother liquor upper prop that steps A is obtained adsorbs, controlled temperature is 2-12BV/h at 5-30 ℃ with flow velocity, make solution stream through resin, pmida98 is adsorbed, and absorption effluent is gone wastewater treatment;
Step C: the sodium hydroxide solution of preparation 3-8% is a desorption liquid, and controlled temperature is to carry out desorption under the 1-4BV/h condition at 25-50 ℃ with flow velocity, and the desorption water outlet is the pmida98 sodium salt solution, through the recyclable pmida98 of acidification.
Adopt method of the present invention, after the pmida98 of pmida98 mother liquor is recycled earlier, carry out wastewater treatment again, can reduce the wasting of resources on the one hand, obtain economic benefit, also reduce the difficulty and the cost of wastewater treatment on the other hand.Improved the economic benefit of the integral body of pmida98 production.
Embodiment
The invention will be further described by the following examples.
Embodiment 1
Get the mother liquor 500ml that produces pmida98, the concentration of its pmida98 is 1.45%, through secondary filter, and regulates pH=1.5, gets the pmida98 clarified mother liquor; (the 335 type weak base anion-exchange resins of producing with the Shanghai China scientific and technological trading company of shake are example to get weak base anion-exchange resin; 335 type resins are the epoxy group(ing) skeleton) 10ml adorns post; after being processed into the OH type with dilute sulphuric acid, diluted sodium hydroxide solution successively; with above-mentioned pmida98 clarified mother liquor upper prop absorption; adsorption temp is 5 ℃; flow velocity 2BV/h, absorption effluent pmida98 concentration is 638mg/L, the rate of recovery 95.6%.Adsorbing saturated back is 50 ℃ with 8% sodium hydroxide solution in temperature, and flow velocity is to carry out desorption under the 1BV/h condition, obtains the pmida98 sodium salt solution, and pmida98 concentration is 23.0%, and desorption rate is 98.5%.The pmida98 sodium salt solution is added hydrochloric acid to pH1.5-2, be settled out pmida98, filter, drying gets white crystal shape pmida98 6.9 grams, and pmida98 content is 98.4%.
Embodiment 2
Get the mother liquor 200ml that produces pmida98, the concentration of its pmida98 is 1.45%, through secondary filter, and regulates pH=1.5, gets the pmida98 clarified mother liquor; Get strongly basic anion exchange resin (the 717 type anionite-exchange resin of producing with Danyang, Jiangsu Golden Elephant company are example) 10ml and adorn post, after being processed into the OH type with dilute sulphuric acid, diluted sodium hydroxide solution successively, with above-mentioned pmida98 clarified mother liquor upper prop absorption, adsorption temp is 30 ℃, flow velocity is 12BV/h, absorption effluent pmida98 concentration is 1682mg/L, the rate of recovery 88.4%.Adsorb saturated back with 3% sodium hydroxide solution 25 ℃ of temperature, carry out desorption under the flow velocity 4BV/h condition, obtain the pmida98 sodium salt solution, pmida98 concentration is 8.4%, desorption rate is 98.1%.The pmida98 sodium salt solution is added hydrochloric acid, be adjusted to pH 1.5-2, be settled out pmida98, filter, drying gets white crystal shape pmida98 2.5 grams, and pmida98 content is 98.1%.
Claims (1)
1. method that reclaims pmida98 from the mother liquor of producing pmida98 is characterized in that it is made up of following steps:
Steps A: will produce the pmida98 mother liquor of pmida98, and, obtain the pmida98 clarified mother liquor through secondary filter;
Step B: the anionite-exchange resin of in adsorption column, packing into, after conventional pre-treatment, the pmida98 clarified mother liquor upper prop that steps A is obtained adsorbs, controlled temperature is 2-12BV/h at 5-30 ℃ with flow velocity, make solution stream through resin, pmida98 is adsorbed, and absorption effluent is gone wastewater treatment;
Step C: the sodium hydroxide solution of preparation 3-8% is a desorption liquid, and controlled temperature is to carry out desorption under the 1-4BV/h condition at 25-50 ℃ with flow velocity, and the desorption water outlet is the pmida98 sodium salt solution, reclaims pmida98 through acidification.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101244031A CN101314607A (en) | 2008-07-01 | 2008-07-01 | Method for recycling glyphosine from mother solution for preparing glyphosine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101244031A CN101314607A (en) | 2008-07-01 | 2008-07-01 | Method for recycling glyphosine from mother solution for preparing glyphosine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101314607A true CN101314607A (en) | 2008-12-03 |
Family
ID=40105760
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008101244031A Pending CN101314607A (en) | 2008-07-01 | 2008-07-01 | Method for recycling glyphosine from mother solution for preparing glyphosine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101314607A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102674638A (en) * | 2010-10-18 | 2012-09-19 | 浙江拜克开普化工有限公司 | Device for recycling N-Phosphonomethyl aminodiacetic acid from waste water in N-Phosphonomethyl aminodiacetic acid production process |
-
2008
- 2008-07-01 CN CNA2008101244031A patent/CN101314607A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102674638A (en) * | 2010-10-18 | 2012-09-19 | 浙江拜克开普化工有限公司 | Device for recycling N-Phosphonomethyl aminodiacetic acid from waste water in N-Phosphonomethyl aminodiacetic acid production process |
| CN102674638B (en) * | 2010-10-18 | 2013-09-11 | 浙江拜克开普化工有限公司 | Device for recycling N-Phosphonomethyl aminodiacetic acid from waste water in N-Phosphonomethyl aminodiacetic acid production process |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20081203 |