CN101759578B - Method for recovering useful ingredients in waste glycin mother liquor - Google Patents
Method for recovering useful ingredients in waste glycin mother liquor Download PDFInfo
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- CN101759578B CN101759578B CN2009102510421A CN200910251042A CN101759578B CN 101759578 B CN101759578 B CN 101759578B CN 2009102510421 A CN2009102510421 A CN 2009102510421A CN 200910251042 A CN200910251042 A CN 200910251042A CN 101759578 B CN101759578 B CN 101759578B
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Abstract
The invention relates to a method for recovering useful ingredients in waste glycin mother liquor, which comprises the following steps: acidifying the waste glycin mother liquor; adding organic solvents to be fully mixed with the waste glycin mother liquor; carrying out the solid-liquid separation for the first time to obtain first filtrate and solid with the useful ingredients; dissolving the solid to separate different useful ingredients through concentration and crystallization; continuously adding organic solvents into the first filtrate to be fully mixed; carrying out the solid-liquid separation for the second time to obtain second filtrate and solid with the useful ingredients; dissolving the solid to separate different useful ingredients through concentration and crystallization; basifying the second filtrate; obtaining third filtrate and solid with the useful ingredients; dissolving the solid again to separate different useful ingredients through concentration and crystallization; and carrying out other steps. The invention can more sufficiently utilize the waste glycin mother liquor as resources, simplifies the subsequent separation and refining processes on the useful ingredients, lowers the process difficulty for treating residual liquid, can recover and reuse the used organic solvents, and greatly reduces the environment pollution by the waste glycin mother liquor.
Description
Technical field
The present invention relates to the processing of glycine waste mother liquid, belong to the chemical separation engineering field.
Background technology
Glycocoll has another name called Padil, is a kind of important fine-chemical intermediate, is widely used in industries such as agricultural chemicals, medicine, food, chemical fertilizer, feed.Since global herbicide glyphosate came out, glycocoll increased in the application of pesticide industry fast especially, and global glycocoll demand is estimated above 300,000 tons/year.Wherein, use hydroxyacetonitrile to belong to the initiative technology at home and abroad as the synthetic glycocoll of raw material.But; Since in process of production glycocoll the online always circulation of synthetic liquid and apply mechanically; Thereby cause various impurity enriched, mother liquor proportion and viscosity strengthen gradually, cause the content of glycocoll in sodium sulfate and bullion glycine crystallization difficulty, separating difficulty increasing, the product to reduce.Therefore, must be repeatedly circulating and applying mechanically the back glycin mother liquid and handle.Yet because glycin mother liquid is after repeatedly circulating and applying mechanically, its COD, colourity, viscosity etc. increase greatly, and intractability is also just quite big.So, present main processing way be repeatedly circulate and apply mechanically after glycin mother liquid treat as waste liquid, and many with spraying the treating method of burning.This not only causes the pollution to environment, and the useful components such as (for example, residue glycocoll and iminodiethanoic acid, vitriol) of remaining organism and salt in mother liquor has also been slatterned in vain." a kind of snow melting composition and the method for making thereof of utilizing glycine waste mother liquid to produce " of publication number CN1861731A; A kind of method of utilizing glycine waste mother liquid is provided; This method is reducing aspect environmental pollution, the recycling glycine waste mother liquid, truly have certain effect.Yet; This method is except that having separated the ammonia in the glycine waste mother liquid separately; In its snow melting composition, still comprise some organism and salt etc. and needn't be included in useful component wherein fully; Also be that its recycling is quite insufficient, still caused the waste of many useful components.
Summary of the invention
The objective of the invention is, a kind of method that reclaims useful component in the glycine waste mother liquid is provided, so that more fully it is carried out recycling.Recuperable useful component comprises glycocoll, iminodiethanoic acid, sodium sulfate etc.
For realizing said purpose, a kind of like this method that reclaims useful component in the glycine waste mother liquid is provided, this method comprises the steps:
1. in said waste liquor, add industrial acids commonly used, regulate its pH value to 0～3;
2. in above-mentioned waste liquor, add organic solvent, this volume of organic solvent is 0.5～4 times of above-mentioned waste liquor volume, reclaims solids component through the solid-liquid separation operation then;
3. in the liquid after above-mentioned solid-liquid separation operation, add industrial soda commonly used and regulate its pH value to 4～10, reclaim a solids component through the solid-liquid separation operation again;
4. 3. reclaim organic solvent in the liquid ingredient of the solid-liquid separation operation back gained the step through distillation or rectifying from the;
5. according to the 2., composition and content in the solid that 3. obtains in the step, through dissolving, concentrate, process for refining such as crystallization extracts glycocoll, iminodiethanoic acid and sodium sulfate technical-pure grade respectively.
Can find out that from scheme the inventive method is through glycine waste mother liquid being carried out the step of acidifying, organic solvent dissolution, alkalization (or adding further acidifying), come classification to reclaim useful component in the glycine waste mother liquid.Compared with prior art, the present invention has following advantage:
1. through handling, the contained useful component in the glycine waste mother liquid basically all is recovered, and also promptly can carry out recycling to glycine waste mother liquid more fully; Simultaneously, also simplified follow-up separation and treating process to useful component.
2. after fully extracting useful component among the present invention, salinity reduces greatly in the last raffinate, and then has reduced the technology difficulty of subsequent disposal raffinate.
3. the used organic solvent of the present invention can reclaim through simple relatively distillation or rectifying, also promptly can be recycled.
In a word, the present invention not only can greatly reduce the pollution of glycine waste mother liquid to environment, and utilization and improvement is with low cost.
Below in conjunction with embodiment the present invention is described further.
Embodiment
A kind of method that reclaims useful component in the glycine waste mother liquid is characterized in that this method comprises the steps:
1. in said waste liquor, add industrial acids commonly used, regulate its pH value to 0～3;
2. in above-mentioned waste liquor, add organic solvent, this volume of organic solvent is 0.5～4 times of above-mentioned waste liquor volume, reclaims solids component through the solid-liquid separation operation then;
3. in the liquid after above-mentioned solid-liquid separation operation, add industrial soda commonly used and regulate its pH value to 4～10, reclaim a solids component through the solid-liquid separation operation again;
4. 3. reclaim organic solvent in the liquid ingredient of the solid-liquid separation operation back gained the step through distillation or rectifying from the;
5. according to the 2., composition and content in the solid that 3. obtains in the step, through dissolving, concentrate, process for refining such as crystallization extracts glycocoll, iminodiethanoic acid and sodium sulfate technical-pure grade respectively.
Further say, step 1. described in industrial acids be the mixing acid of a kind of in the vitriol oil, concentrated nitric acid, SPA and the concentrated hydrochloric acid or two kinds.
Further say, step 2. in, organic solvent is the mixed solvent of a kind of in acetone, ether, methyl alcohol, ethanol, terepthaloyl moietie, sorbyl alcohol and the polyoxyethylene glycol or two kinds; Industrial soda is the mixed base of a kind of in sodium hydroxide, Pottasium Hydroxide, yellow soda ash, ammoniacal liquor and the liquefied ammonia or two kinds.
Say further that again adding organic solvent in step in 2. can be disposable adding; Also can be twice adding.
If the organic solvent of this step in 2. adds at twice, then promptly reclaiming solids component one time after adding organic solvent, thereby after 2. step finishes, obtaining two batches of solids components respectively each; Add for the first time volume of organic solvent and be 0.01～2 times of waste liquor volume, for the second time with the organic solvent that adds for the first time altogether after, its TV is 0.5～4 times of waste liquor volume.
The solid-liquid body lock out operation that it will be apparent to those skilled in the art that among the present invention to be mentioned can comprise: press filtration, suction filtration, centrifugal, gravity settling or normal pressure filter.During actually operating, solid-liquid separation efficiency should be suitable in each operation, and the product composition is not made significant difference.
The present invention has passed through verification experimental verification.Wherein, contained useful component of different solids and content, with the circulation of employing glycine waste mother liquid and apply mechanically degree and concrete technology relevant.The checking example sees the following form:
Annotate: go up in the table, " zero " expression is selected for use; Reclaim " % of total amount " in the hurdle and represent this recover materials shared per-cent in the solid amount behind the suction filtration several times.
Claims (2)
1. a method that reclaims useful component in the glycine waste mother liquid is characterized in that this method comprises the steps:
1. in said waste liquor, add industrial acids commonly used, regulate its pH value to 0～3;
2. in above-mentioned waste liquor, add organic solvent, this volume of organic solvent is 0.5～4 times of above-mentioned waste liquor volume, reclaims solids component through the solid-liquid separation operation then;
3. in the liquid after above-mentioned solid-liquid separation operation, add industrial soda commonly used and regulate its pH value to 4～10, reclaim a solids component through the solid-liquid separation operation again;
4. 3. reclaim said organic solvent in the liquid ingredient of the solid-liquid separation operation back gained the step through distillation or rectifying from the;
5. according to the 2., composition and content in the solid that 3. obtains in the step, through dissolving, concentrate, the crystalline process for refining extracts glycocoll, iminodiethanoic acid and sodium sulfate technical-pure grade respectively;
Step 1. described in industrial acids be the mixing acid of a kind of in the vitriol oil, concentrated nitric acid, SPA and the concentrated hydrochloric acid or two kinds;
Step 2. in, said organic solvent is the mixed solvent of a kind of in acetone, ether, methyl alcohol, ethanol, terepthaloyl moietie, sorbyl alcohol and the polyoxyethylene glycol or two kinds; Said industrial soda is a kind of in sodium hydroxide, Pottasium Hydroxide, yellow soda ash, ammoniacal liquor and the liquefied ammonia.
2. according to the method for useful component in the said recovery glycine waste mother liquid of claim 1, it is characterized in that, when step adds said organic solvent in 2., add at twice, and promptly reclaiming solids component one time after adding said organic solvent each; Add for the first time said volume of organic solvent and be 0.01～2 times of said waste liquor volume, for the second time with the said organic solvent that adds for the first time altogether after, its TV is 0.5～4 times of said waste liquor volume.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102510421A CN101759578B (en) | 2009-12-29 | 2009-12-29 | Method for recovering useful ingredients in waste glycin mother liquor |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102510421A CN101759578B (en) | 2009-12-29 | 2009-12-29 | Method for recovering useful ingredients in waste glycin mother liquor |
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| Publication Number | Publication Date |
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| CN101759578A CN101759578A (en) | 2010-06-30 |
| CN101759578B true CN101759578B (en) | 2012-08-22 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2009102510421A Expired - Fee Related CN101759578B (en) | 2009-12-29 | 2009-12-29 | Method for recovering useful ingredients in waste glycin mother liquor |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104744279B (en) * | 2015-04-03 | 2016-09-07 | 重庆紫光化工股份有限公司 | Remove the method for impurity in glycine crystallization mother liquid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5338530A (en) * | 1989-04-11 | 1994-08-16 | Hampshire Chemical Corp. | Recovery of glycine and Glauber's salt from waste crystal liquors |
| CN1861731A (en) * | 2005-05-11 | 2006-11-15 | 张天德 | Snow melting composition prepared from glycine waste mother liquid and preparation process thereof |
| CN1990460A (en) * | 2005-12-31 | 2007-07-04 | 重庆三峡英力化工有限公司 | Comprehensive treatment of glycine crystallization mother liquid |
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2009
- 2009-12-29 CN CN2009102510421A patent/CN101759578B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5338530A (en) * | 1989-04-11 | 1994-08-16 | Hampshire Chemical Corp. | Recovery of glycine and Glauber's salt from waste crystal liquors |
| CN1861731A (en) * | 2005-05-11 | 2006-11-15 | 张天德 | Snow melting composition prepared from glycine waste mother liquid and preparation process thereof |
| CN1990460A (en) * | 2005-12-31 | 2007-07-04 | 重庆三峡英力化工有限公司 | Comprehensive treatment of glycine crystallization mother liquid |
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| CN101759578A (en) | 2010-06-30 |
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Granted publication date: 20120822 Termination date: 20121229 |