CN103420789A - Method for processing triethylamine method glycine circulating mother liquid according to membrane separation technology - Google Patents
Method for processing triethylamine method glycine circulating mother liquid according to membrane separation technology Download PDFInfo
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- CN103420789A CN103420789A CN2013103919386A CN201310391938A CN103420789A CN 103420789 A CN103420789 A CN 103420789A CN 2013103919386 A CN2013103919386 A CN 2013103919386A CN 201310391938 A CN201310391938 A CN 201310391938A CN 103420789 A CN103420789 A CN 103420789A
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- glycine
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- triethylamine
- circulating mother
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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
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/582—Recycling of unreacted starting or intermediate materials
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Abstract
The invention provides a method for processing triethylamine method glycine circulating mother liquid according to the membrane separation technology. Through the trapping performance and the charge performance of a nanofiltration membrane, separation of colored by-products generated in the reaction process of triethylamine hydrochloride, glycine and the mother liquid is achieved. Through the separation of the nanofiltration membrane, most of the triethylamine hydrochloride, most of the glycine and part of urotropine in the glycine reaction circulating mother liquid permeate the nanofiltration membrane to enter nanofiltration percolate, and most of the colored by-products and part of the urotropine are trapped into trapped liquid. The nanofiltration percolate returns to a glycine synthesis system to be recycled.
Description
Technical field:
The present invention relates to a kind of production technique of triethylamine set process glycine, belong to chemical production technical field.
Background technology:
It is raw material (or take ammonium chloroacetate as raw material) that the triethylamine set process glycine be take Mono Chloro Acetic Acid and ammonia, and the methyl alcohol (or methanol aqueous solution) of take is solvent, under the effect of catalyzer urotropine, take triethylamine as acid binding agent, and reaction directly obtains the glycine solid phase prod.Utilize calcium oxide to reclaim the acid binding agent triethylamine and recycle, obtain calcium chloride solution simultaneously.Calcium chloride solution after treatment, can be produced the calcium chloride product.Calcium chloride solution also can with strong sulfuric acid response, obtain calcium sulfate precipitation and hydrogen chloride gas (processing other products or recovery obtain the hydrochloric acid that purity is high).The circulating mother liquor that contains methyl alcohol, urotropine and triethylamine hydrochloride, after participating in the certain number of times of circulating reaction, due to the increase of the impurity such as by product, its colour changed into yellow, the building-up reactions that can not continue again to participate in glycine.The treatment process of prior art is as follows:
At first evaporation concentration reclaims the most of methyl alcohol in mother liquor.Then add a certain amount of water (0.5-3 that the volume that adds water is residue mother liquor volume doubly) in remaining circulating mother liquor, then add calcium hydroxide (or calcium oxide) reaction, then methyl alcohol and the triethylamine in solution reclaimed in rectifying.Remaining liquid obtains the chemical fertilizer raw material product after concentrate drying, for the production of chemical fertilizer.
Above method is due to needs through Distillation recovery methyl alcohol, and steam consumption is higher.Reclaimed in addition the remaining liquid of triethylamine, the calcium chloride concentration contained is higher, and the chemical fertilizer raw material quality product be processed into is subject to the impact of calcium chloride, and the nitrogen content of fertilizer is on the low side, affects the use of product.
Also having a kind of method, is exactly to lead to ammonia in circulating mother liquor, after recovery triethylamine wherein, is reprocessed into chemical fertilizer raw material.The shortcoming of this method is high with the cost of ammonia, and the yield of recovery triethylamine is low.
Nanofiltration (NF) is a kind of new membrane isolation technique grown up over nearly 20 years, and nanofiltration membrane is the composite charged film that has nanometer micropore, based on its screening principle, is applicable to molecular weight is separated between the daltonian organic molecule of 80-1000; Based on its electrocharge effect, be applicable to separating univalent ion and polyvalent ion and neutral substance.
Summary of the invention:
The invention provides a kind of method of utilizing Nanofiltration Membrane Separation Technology to process triethylamine set process glycine circulating mother liquor.Utilize dam performance and the charge of nanofiltration membrane separation, realized separating of the coloured by product that produces in reaction process in triethylamine hydrochloride, glycine and mother liquor.The present invention implements by following concrete scheme:
Step 1, at first glycine reactant methyl alcohol for circulating mother liquor (or methanol wash liquid of washing glycine product) is diluted to original volume 2-6 doubly.
Step 2, to select the molecular weight that nanofiltration membrane is held back be the daltonian nanofiltration equipment of 80--300, working pressure 1.5-4.0Mpa, and 20 ℃ of service temperatures--40 ℃.
Separation by nanofiltration membrane, most of triethylamine hydrochloride in the glycine reactant circulating mother liquor and glycine, part urotropine see through nanofiltration membrane and enter into nanofiltration through the liquid the inside, and most coloured by products and part urotropine are trapped the liquid the inside of damming.
Step 3, nanofiltration turn back to glycine synthetic system the inside through liquid and recycle.
Step 4, nanofiltration trapped fluid adopt following methods to process:
At first the methyl alcohol in the Distillation recovery trapped fluid then adds a certain amount of water in solution, and methyl alcohol is reclaimed in rectifying.
Add calcium oxide in the remaining aqueous solution, by the Distillation recovery triethylamine.Remaining liquid obtains the chemical fertilizer raw material product through super-dry.Also can add the vitriol oil through in reclaiming the remaining solution that contains calcium chloride of triethylamine above, obtain calcium sulfate precipitation.The liquid that filters out calcium sulfate precipitation obtains the chemical fertilizer raw material product through super-dry.
Reclaim the aqueous solution of methyl alcohol, also can adopt the method for logical ammonia to process.Reclaim triethylamine after logical ammonia, remaining liquid obtains the chemical fertilizer raw material product after super-dry.
The nanofiltration trapped fluid also can adopt following methods to process:
By the methyl alcohol in the Distillation recovery trapped fluid, remaining material convection drying obtains the chemical fertilizer raw material product.
Embodiment:
Get 10L glycine methanol loop mother liquor, add 40L methyl alcohol, use nanofiltration experiment equipment to carry out concentrating and separating.Nanofiltration equipment is selected the DK--2540 model of AM General company, and molecular weight cut-off is the daltonian nanofiltration membrane of 100--300, working pressure 1.8-2.4Mpa; Service temperature 20--40 ℃; Dam liquid while being concentrated into volume 8L when nanofiltration, stop concentrating;
The 42L nanofiltration turns back in the glycine reactant system and recycles through liquid;
Get 4L nanofiltration trapped fluid, methanol solution 3.5L is reclaimed in evaporation, and remaining solution obtains chemical fertilizer raw material product 456 grams through super-dry.
Claims (4)
1. a method of utilizing Nanofiltration Membrane Separation Technology to process triethylamine set process glycine circulating mother liquor.It is characterized in that the method comprises following steps:
Step 1, glycine reactant methyl alcohol for circulating mother liquor (or methanol wash liquid of washing glycine product) is diluted to original volume 2-6 doubly.
Step 2, to select the molecular weight that nanofiltration membrane is held back be the daltonian nanofiltration equipment of 80--300, working pressure 1.5-4.0Mpa, and 20 ℃ of service temperatures--40 ℃.Separation by nanofiltration membrane, most of triethylamine hydrochloride in the glycine reactant circulating mother liquor and glycine, part urotropine see through nanofiltration membrane and enter into nanofiltration through the liquid the inside, and most coloured by products and part urotropine are trapped the liquid the inside of damming.
Step 3, nanofiltration turn back to glycine synthetic system the inside through liquid and recycle.
Step 4, nanofiltration trapped fluid be the methyl alcohol in the Distillation recovery trapped fluid at first, then in solution, adds a certain amount of water, and methyl alcohol is reclaimed in rectifying.Add calcium oxide in the remaining aqueous solution, by the Distillation recovery triethylamine.Remaining liquid obtains the chemical fertilizer raw material product through super-dry.Also can add the vitriol oil through in reclaiming the remaining solution that contains calcium chloride of triethylamine above, obtain calcium sulfate precipitation.The liquid that filters out calcium sulfate precipitation obtains the chemical fertilizer raw material product through super-dry.
2. the method for claim 1, is characterized in that by the glycine reactant 2-6 that for circulating mother liquor, methyl alcohol (or methanol wash liquid of washing glycine product) is diluted to original volume doubly.
3. the method for claim 1, is characterized in that selecting the molecular weight that nanofiltration membrane is held back is the daltonian nanofiltration equipment of 80--300, working pressure 1.5-4.0Mpa, and 20 ℃ of service temperatures--40 ℃.
4. the method for claim 1, is characterized in that nanofiltration sees through liquid and turns back to glycine synthetic system the inside and recycle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2013103919386A CN103420789A (en) | 2013-09-03 | 2013-09-03 | Method for processing triethylamine method glycine circulating mother liquid according to membrane separation technology |
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| CN2013103919386A CN103420789A (en) | 2013-09-03 | 2013-09-03 | Method for processing triethylamine method glycine circulating mother liquid according to membrane separation technology |
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| CN103420789A true CN103420789A (en) | 2013-12-04 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109136298A (en) * | 2018-08-10 | 2019-01-04 | 浙江正硕生物科技有限公司 | A kind of preparation method of D- amino acid |
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2013
- 2013-09-03 CN CN2013103919386A patent/CN103420789A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109136298A (en) * | 2018-08-10 | 2019-01-04 | 浙江正硕生物科技有限公司 | A kind of preparation method of D- amino acid |
| CN109136298B (en) * | 2018-08-10 | 2021-09-10 | 浙江正硕生物科技有限公司 | Preparation method of D-amino acid |
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| C06 | Publication | ||
| PB01 | Publication | ||
| DD01 | Delivery of document by public notice |
Addressee: Liu Changfei Document name: Notification of Passing Preliminary Examination of the Application for Invention Addressee: Liu Changfei Document name: Notification of Passing Examination on Formalities |
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| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20131204 |