CN101100437A - Method for preparing high-purity beta-alanine - Google Patents
Method for preparing high-purity beta-alanine Download PDFInfo
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- CN101100437A CN101100437A CNA2007100966661A CN200710096666A CN101100437A CN 101100437 A CN101100437 A CN 101100437A CN A2007100966661 A CNA2007100966661 A CN A2007100966661A CN 200710096666 A CN200710096666 A CN 200710096666A CN 101100437 A CN101100437 A CN 101100437A
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Abstract
Production of high-purity beta-lactamin is carried out by adding industrial beta-lactamin into deionized water, dissolving in proportion of deionized water: industrial beta-lactamin=2.0-50.0:1 mol, adding into activated carbon, de-coloring, electro-dialyzing, removing purities, filtering, ultra-filtering to remove endotoxin, inverse penetrating, first concentrating, re-evaporating, concentrating to obtain glue, adding into absolute methanol or ethanol, cooling, crystallizing, centrifugal filtering to obtain filter cake and crystallizing mother liquor, heating and drying to obtain refined final product. It costs low and can be used for industrial production.
Description
Technical field
The invention belongs to the biochemical engineering field, relate to a kind of preparation method of high-purity beta-alanine.
Technical background
Beta-alanine (English name Beta-Alanine) has another name called β-An Jibingsuan, and structural formula is H
2NCH
2CH
2COOH.Found in the degraded product of uridylic by Ross and Monroe in 1972.It is a kind of amino acid of nonprotein, is the unique β type amino acid of occurring in nature.Beta-alanine is a kind of important biochemical raw material, has very in fields such as medicine, feed and food and uses widely.
Beta-alanine mainly adopts chemical synthesis production at present, as (1) vinylformic acid that U.S.2376334 and BP561013 reported or acrylate and ammoniacal liquor, and the method for pressurized, heated reaction; (2) vinyl cyanide that U.S.2335997 and U.S.2377401 reported and ammoniacal liquor, pressurized, heated reaction, the method for hydrolysis then, the Beta-alanine of two kinds of method preparations all contains a large amount of impurity salts, as ammonium salt, Ba-Ba-L-Ala or NaCl etc., need carry out purifying.Method for the Beta-alanine purifying that contains impurity has following several:
(1) separating out alcohol method: as U.S.3,932,501 and JP74,29,170 disclosed methods of carrying out recrystallization with alcoholic solvent;
(2) ion exchange method: Khim-Farm, zh., 4 (2), 27,1970; The Hunan chemical industry, 2,60,1989 disclosed ion exchange methods;
(3) JP81,118, the 047 disclosed electroosmose processs that carry out with ion-exchange membrane.
All there is obvious defects in the technology of the disclosed purifying Beta-alanine of above document, and as complex operation, expense is higher, and yield is no more than 80% usually.Must find a kind of new easy to operately, purification process cheaply is to satisfy industrial demand for this reason.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of high-purity beta-alanine of easy to operate, low-cost purifying.
The preparation method of a kind of high-purity beta-alanine provided by the invention, it may further comprise the steps:
A kind of preparation method of high-purity beta-alanine is characterized in that the step of this method is as follows:
To dissolve in the technical grade Beta-alanine adding deionized water, wherein the proportioning (weight) of deionized water and technical grade Beta-alanine is: H
2O: H
2N CH
2CH
2COO H=(2.0-50.0): 1;
Add activated carbon decolorizing;
Solution after the decolouring is carried out electrodialysis removal of impurities and filtration, remove the foreign ion that exists in solution, and remove the mechanical impurity in the solution, and remove intracellular toxin in the solution with ultrafiltration;
Make solution tentatively concentrate revaporization and be concentrated into colloid, add anhydrous methanol or ethanol through reverse osmosis, crystallisation by cooling, centrifuging obtains filter cake and crystalline mother solution; Filter cake is carried out heat drying, obtain purified Beta-alanine crystal.
In the preparation method of a kind of high-purity beta-alanine provided by the invention, reactor in the whole process of production and mass transport pipeline are in the sealed state.
Adopt the present invention to avoid using a large amount of methyl alcohol or alcoholic acid defective in the separating out alcohol method, saved raw-material expense, reduced the consumption that the methyl alcohol or the required energy of ethanol are reclaimed in distillation.And, little to the pollution of environment in process of production, less to operator's health hazard ratio.
Produce Beta-alanine with ion exchange method and compare,, reduced the consumption of acid-base reagent owing to cancelled the use of ion exchange resin.
The present invention has simplified the production stage of Beta-alanine, and prevents that crystalline mother solution from contacting with extraneous, has avoided introduced contaminants to enter the situation that crystalline mother solution reduces quality product, makes the quality of Beta-alanine be greatly enhanced, product transmittance 〉=99%.
Description of drawings
Fig. 1 is the Production Flow Chart synoptic diagram of Beta-alanine purifying among the present invention.
As shown in Figure 1, in Beta-alanine production method provided by the invention, it may further comprise the steps:
To dissolve in the technical grade Beta-alanine adding deionized water, the consumption of deionized water is industry The 2-50 of level Beta-alanine doubly. Be 50-80 ℃ in solution temperature, the time is that 0.5-1.5 is little The time condition under, the technical grade Beta-alanine is dissolved in deionized water. Simultaneously, at β-third ammonia In the deionized water solution of acid, add active carbon and decolour, the amount that adds active carbon is 0.01-1% (weight ratio) is namely take the solution weight ratio of Beta-alanine and deionized water as 0.01-1% adds active carbon.
Adopt bag filter, to filtering through de-inking solution, in bag filter, adopt With filter bag in pore size be the 0.5-0.1 micron, exist in solution in order to remove Mechanical admixture, and the employing hyperfiltration process is removed the endotoxin in the solution.
Adopt electrodialysis methods commonly known in the art, remove and be present in the technical grade Beta-alanine With the foreign ion in the deionized water solution, and remove the salinity that exists in solution.
After solution was tentatively concentrated through counter-infiltration commonly known in the art, evaporation and concentration extremely again Add methyl alcohol behind the colloid, crystallisation by cooling, centrifugal acquisition filter cake, its crystallization temperature is 55-20 ℃, Crystallization time is 1.5-4.5 hour.
Adopt continuous tray drier that filter cake is carried out drying, its heating-up temperature is 50-70 ℃, Obtain refining Beta-alanine crystal.
Below describe by specific embodiment.
Embodiment 1
To dissolve 70 ℃ of solvent temperatures, dissolution time 1.5 hours in technical grade Beta-alanine 100 gram addings 200 ml deionized water.The activated carbon decolorizing of adding 0.2% in solution filters the solution through decolouring, and the filter paper pore size is 0.5 micron, removes the mechanical impurity in the solution.Adopt electrodialytic method to remove foreign ion in the above-mentioned solution again.Adopt hyperfiltration process to remove intracellular toxin in the solution then.The solution of handling tentatively concentrates through reverse osmosis and adds anhydrous methanol after revaporization is concentrated into colloid, sends into the crystallizing pan crystallisation by cooling then, 20 ℃ of Tcs, and crystallization time 4 hours obtains filter cake after centrifugal.Filter cake adopts continuous tray drier heat drying after using anhydrous methanol drip washing, and about 60 ℃ of drying temperature obtains purified Beta-alanine crystal.
Embodiment 2
To dissolve 60 ℃ of solvent temperatures, dissolution time 1 hour in technical grade Beta-alanine 100 gram addings 500 ml deionized water.The activated carbon decolorizing of adding 0.1% in solution filters the solution through decolouring, and the filter paper pore size is 0.2 micron, removes the mechanical impurity in the solution.Adopt electrodialytic method to remove foreign ion in the above-mentioned solution again.Adopt hyperfiltration process (0.1 micron of filter membrane filter opening diameter) to remove the intracellular toxin in the solution then.The solution of handling tentatively concentrates through reverse osmosis and sends into the crystallizing pan crystallisation by cooling after adding anhydrous methanol after revaporization is concentrated into colloid, 25 ℃ of Tcs, and crystallization time 4.5 hours obtains filter cake after centrifugal.Filter cake adopts continuous tray drier heat drying after using anhydrous methanol drip washing, and about 70 ℃ of drying temperature obtains purified Beta-alanine crystal.
Embodiment 3
To dissolve 55 ℃ of solvent temperatures, dissolution time 1.5 hours in technical grade Beta-alanine 100 gram addings 1000 ml deionized water.The activated carbon decolorizing of adding 0.05% in solution filters the solution through decolouring, and the filter paper pore size is 0.5 micron, removes the mechanical impurity in the solution.Adopt electrodialytic method to remove foreign ion in the above-mentioned solution again.Adopt hyperfiltration process to remove intracellular toxin in the solution then.The solution of handling tentatively concentrates through reverse osmosis and sends into the crystallizing pan crystallisation by cooling after adding anhydrous methanol after revaporization is concentrated into colloid, 20 ℃ of Tcs, and crystallization time 4 hours obtains filter cake after centrifugal.Filter cake adopts continuous tray drier heat drying after using anhydrous methanol drip washing, and about 65 ℃ of drying temperature obtains purified beta Alanine crystal.
Embodiment 4
To dissolve 75 ℃ of solvent temperatures, dissolution time 1.5 hours in technical grade Beta-alanine 100 gram addings 2500 ml deionized water.The activated carbon decolorizing of adding 0.2% in solution filters the solution through decolouring, and the filter paper pore size is 0.5 micron, removes the mechanical impurity in the solution.Adopt electrodialytic method to remove foreign ion in the above-mentioned solution again.Adopt hyperfiltration process to remove intracellular toxin in the solution then.The solution of handling tentatively concentrates through reverse osmosis and sends into the crystallizing pan crystallisation by cooling after adding anhydrous methanol after revaporization is concentrated into colloid, 20 ℃ of Tcs, and crystallization time 3.5 hours obtains filter cake after centrifugal.Filter cake adopts continuous tray drier heat drying after using anhydrous methanol drip washing, and about 60 ℃ of drying temperature obtains purified Beta-alanine crystal.
Embodiment 5
To dissolve in technical grade Beta-alanine 100 gram addings 4000 ml deionized water, 50 ℃ of solvent temperatures, dissolution time 0.5 hour, the activated carbon decolorizing of adding 0.05% in solution, solution through decolouring is filtered, the filter paper pore size is 0.5 micron, removes the mechanical impurity in the solution.Adopt electrodialytic method to remove foreign ion in the above-mentioned solution again.Adopt hyperfiltration process to remove intracellular toxin in the solution then.The solution of handling tentatively concentrates through reverse osmosis and sends into the crystallizing pan crystallisation by cooling after adding anhydrous methanol after revaporization is concentrated into colloid, 30 ℃ of Tcs, and crystallization time 4.5 hours obtains filter cake after centrifugal.Filter cake adopts continuous tray drier heat drying after using anhydrous methanol drip washing, and about 68 ℃ of drying temperature obtains purified Beta-alanine crystal.
Embodiment 6
To dissolve 53 ℃ of solvent temperatures, dissolution time 0.5 hour in technical grade Beta-alanine 100 gram addings 5000 ml deionized water.The activated carbon decolorizing of adding 0.08% in solution filters the solution through decolouring, and the filter paper pore size is 0.2 micron, removes the mechanical impurity in the solution.Adopt electrodialytic method to remove foreign ion in the above-mentioned solution again.Adopt hyperfiltration process to remove intracellular toxin in the solution then.The solution of handling tentatively concentrates through reverse osmosis and sends into the crystallizing pan crystallisation by cooling after adding anhydrous methanol after revaporization is concentrated into colloid, 20 ℃ of Tcs, and crystallization time 4 hours obtains filter cake after centrifugal.Filter cake adopts continuous tray drier heat drying after using anhydrous methanol drip washing, and about 70 ℃ of drying temperature obtains purified Beta-alanine crystal.
Technical scheme disclosed according to the present invention and embodiment can find that the said method of the present invention is easy and simple to handle, and the product purity height satisfies the high-end requirement of pharmacy corporation.
Claims (8)
1, a kind of preparation method of high-purity beta-alanine is characterized in that the step of this method is as follows:
To dissolve in the technical grade Beta-alanine adding deionized water, wherein the proportioning (weight) of deionized water and technical grade Beta-alanine is: H
2O: H
2NCH
2CH
2COOH=(2.0-50.0): 1;
Add activated carbon decolorizing;
Solution after the decolouring is carried out electrodialysis removal of impurities and filtration, remove the foreign ion that exists in solution, and remove the mechanical impurity in the solution, and remove intracellular toxin in the solution with ultrafiltration;
Make solution tentatively concentrate revaporization and be concentrated into colloid, add anhydrous methanol or ethanol through reverse osmosis, crystallisation by cooling, centrifuging obtains filter cake and crystalline mother solution; Filter cake is carried out heat drying, obtain purified Beta-alanine crystal.
2, the preparation method of high-purity beta-alanine according to claim 1 is characterized in that: it is 0.5-1.5 hour that the described solution that makes technical grade Beta-alanine and deionized water carries out the dissolved time, and its solvent temperature is 50-80 ℃.
3, the preparation method of high-purity beta-alanine according to claim 1, it is characterized in that: when decolouring, be that 0.01-1% adds gac with the solution weight ratio of Beta-alanine and deionized water for the solution of technical grade Beta-alanine and deionized water.
4, the preparation method of high-purity beta-alanine according to claim 1, it is characterized in that: adopt deep bed filter, to filtering through de-inking solution, pore size in the filter bag that adopts in deep bed filter is the 0.5-0.1 micron, and the employing hyperfiltration process is removed the intracellular toxin in the solution.
5, the preparation method of high-purity beta-alanine according to claim 1 is characterized in that: adopt electrodialytic method to remove the foreign ion that is present in technical grade and the deionized water solution, and remove the salinity that is present in the crystalline mother solution.
6, the preparation method of high-purity beta-alanine according to claim 1 is characterized in that: when making through the solution crystallisation by cooling behind the reverse osmosis reconcentration, its Tc is 55-20 ℃, and crystallization time is 1.5-4.5 hour.
7, the preparation method of high-purity beta-alanine according to claim 1 is characterized in that: adopt continuous tray drier that filter cake is carried out heat drying, its Heating temperature is 50-70 ℃.
8, the preparation method of high-purity beta-alanine according to claim 1 is characterized in that: reactor in the production process and mass transport pipeline are in the sealed state.
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| CN2007100966661A CN101100437B (en) | 2007-08-15 | 2007-08-15 | Method for preparing high-purity beta-alanine |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104313071A (en) * | 2014-10-17 | 2015-01-28 | 湖南宝利士生物技术有限公司 | Biosynthetic method of high purity L-alpha-amino acid |
| CN106631851A (en) * | 2016-09-23 | 2017-05-10 | 精晶药业股份有限公司 | L-alanine refining method |
| CN106831466A (en) * | 2016-12-28 | 2017-06-13 | 安徽省虹升生物股份有限公司 | A kind of conventional storage method of beta Alanine |
| CN109776344A (en) * | 2017-11-13 | 2019-05-21 | 秦皇岛华恒生物工程有限公司 | A method of l-Alanine and lactic acid are separated using electrodialysis |
| CN110305028A (en) * | 2019-06-21 | 2019-10-08 | 湖北泰盛化工有限公司 | A kind of device and technique of alcohol phase method washing glycine crude product |
| CN114014771A (en) * | 2021-06-30 | 2022-02-08 | 安徽华恒生物科技股份有限公司 | Ultrahigh-purity amino acid, and preparation method and application thereof |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3105092A (en) * | 1959-09-25 | 1963-09-24 | Union Carbide Corp | Purification of beta-alanine |
| GB1502365A (en) * | 1974-10-24 | 1978-03-01 | Grace W R & Co | Process for recovering glycine and beta-alanine |
| CN1285730C (en) * | 2003-12-10 | 2006-11-22 | 浙江工业大学 | Biology method for synthesizing beta alanine |
| CN1884565B (en) * | 2006-05-29 | 2011-05-04 | 安徽华恒生物工程有限公司 | Process for producing D-alanine using microbe |
-
2007
- 2007-08-15 CN CN2007100966661A patent/CN101100437B/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104313071A (en) * | 2014-10-17 | 2015-01-28 | 湖南宝利士生物技术有限公司 | Biosynthetic method of high purity L-alpha-amino acid |
| CN106631851A (en) * | 2016-09-23 | 2017-05-10 | 精晶药业股份有限公司 | L-alanine refining method |
| CN106831466A (en) * | 2016-12-28 | 2017-06-13 | 安徽省虹升生物股份有限公司 | A kind of conventional storage method of beta Alanine |
| CN106831466B (en) * | 2016-12-28 | 2018-05-22 | 安徽省虹升生物股份有限公司 | A kind of conventional storage method of Beta-alanine |
| CN109776344A (en) * | 2017-11-13 | 2019-05-21 | 秦皇岛华恒生物工程有限公司 | A method of l-Alanine and lactic acid are separated using electrodialysis |
| CN109776344B (en) * | 2017-11-13 | 2022-01-18 | 秦皇岛华恒生物工程有限公司 | Method for separating L-alanine and lactic acid by electrodialysis |
| CN110305028A (en) * | 2019-06-21 | 2019-10-08 | 湖北泰盛化工有限公司 | A kind of device and technique of alcohol phase method washing glycine crude product |
| CN110305028B (en) * | 2019-06-21 | 2022-04-08 | 湖北泰盛化工有限公司 | Device and process for washing glycine crude product by alcohol phase method |
| CN114014771A (en) * | 2021-06-30 | 2022-02-08 | 安徽华恒生物科技股份有限公司 | Ultrahigh-purity amino acid, and preparation method and application thereof |
| CN114014771B (en) * | 2021-06-30 | 2023-12-12 | 安徽华恒生物科技股份有限公司 | Ultra-high purity amino acid, preparation method and application thereof |
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