CN105037217B - Preparation method for biological buffer agent - Google Patents
Preparation method for biological buffer agent Download PDFInfo
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- CN105037217B CN105037217B CN201510338904.XA CN201510338904A CN105037217B CN 105037217 B CN105037217 B CN 105037217B CN 201510338904 A CN201510338904 A CN 201510338904A CN 105037217 B CN105037217 B CN 105037217B
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Abstract
The invention discloses a preparation method for a biological buffer agent which has a general reaction formula shown in the description. In the general reaction formula, n is equal to 1, 2, 3, or 4, and M is K or Na. The synthesis process of the biological buffer agent has the main advantages of being low in solvent consumption, little in sewage, high in reaction efficiency, and easy for industrialization; in the synthesis process, raw materials are simple and easy to obtain; compared with the conventional preparation method that diethanol amine and butene sodium sulfonate or chloroethanesulfonic acid are taken as raw materials for reaction, the preparation method provided by the invention achieves a breakthrough in the synthesis process, that is, a compound III is obtained through reaction between ethylene epoxide and sulfamate, so that the reaction yield and efficiency are greatly improved, and the problem of low reaction yield and efficiency in the prior art is solved.
Description
Technical field
The invention belongs to technical field of fine, and in particular to a kind of preparation method of biological buffer, mainly with
Oxirane substitutes the synthetic route of diethanolamine, can more effectively be prepared and purify.
Background technology
In biological study, cell medium, interstice and the biomacromolecule for studying Object of Development will be to train
Nutrient solution is nutrient source.When there is chemical reaction, these materials to culture medium in [H+] have certain requirement, need more steady
Determine the applicable biological buffer of pH value.Except pKa value should properly in addition to, generally also require biological buffer have chemical inertness,
It is soluble in water and the characteristics of be seldom dissolved in organic solvent, the impact of temperature and little salt effect, and also to be readily synthesized.Amino sulphur
Acid type double ion biological buffer can meet as above most of requirement, obtain more application in the world, but with regard to hydroxyl
Saying, traditional synthetic route is with diethanolamine and butylene sodium sulfonate or chloroethyl sodium sulfonate as reaction to ethyl sulfamate
Thing, than relatively low only 60% or so, than relatively low, raw material is also more expensive, and not only high energy consumption is also brought greatly for production efficiency for its reaction yield
The emission problem of amount sewage.
The content of the invention
Goal of the invention：Against the deficiencies in the prior art, such as traditional synthetic route is to be with diethanolamine to the present invention
Reactant, its reaction yield than relatively low, only 60% or so, than relatively low, not only high energy consumption also brings large amount of sewage to production efficiency
Emission problem, so improve on this basis, the invention provides a kind of preparation method of biological buffer.The conjunction of the present invention
High in reaction yield into technique major embodiment, quantity of solvent is few, and sewage is few, and production efficiency is high, and raw material is simple and easy to get, easy industry
Change.
Technical scheme：In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is：The invention provides one
The preparation method of biological buffer is planted, its reaction expression is as follows：
In formula, n=1-4, M are K or Na,
Specifically include following steps：
1) compound I is added to after reaction bulb, then plus compound I 5%～80% mass water and stir；
2) reactant liquor is warming up to into 0～90 DEG C；
3) compound II is dropped in reactant liquor；
4) post processing, filters, and filter cake carries out recrystallization to obtain pure target product.
Further, the step 2) and step 3) reaction temperature be 0～90 DEG C, the step 2) response time be
0.5-2 hours.
Further, the mol ratio of the compound I and II is 1:2-1:3.
Further, the compound II replaces with expoxy propane.
Beneficial effect：Compared with prior art, the present invention has following characteristic and advantage：The synthesis technique master of the present invention
It is embodied in reaction yield high, quantity of solvent is few, and sewage is few, production efficiency is high, and raw material is simple and easy to get, easy industrialization.The present invention
Traditional synthetic route using diethanolamine as reactant is broken through, reaction is substantially increased with oxirane as an alternative
Yield and efficiency.Traditional synthetic method yield only has 60% or so, and the inventive method yield can reach more than 90%.
Specific embodiment
Below by specific embodiment, the present invention is further described, it is noted that for the ordinary skill of this area
For personnel, under the premise without departing from the principles of the invention, some modifications and improvement can also be made, these also should be regarded as belonging to
Protection scope of the present invention.
Embodiment 1：
When compound III isI.e. as n=2, when M is Na, the conjunction of its biological buffer
It is as follows into reaction expression：
The preparation method of the biological buffer, specifically includes following steps：
1) compound I is added to after reaction bulb, then plus compound I 80% mass water and stir；
2) reactant liquor ice bath is cooled down into 0 DEG C or so；Response time is 2 hours；
3) compound II is dropped in reactant liquor；
4) post processing, filters, and filter cake carries out recrystallization to obtain pure target product N, N- (2- ethoxys) -2- amino second
Sodium sulfonate (BES sodium salts).
| Compound I | Compound II | H2O | Compound III | |
| M (quality) | 500g | 299.2g | 400g | 711g |
| N (molal weight) | 3.40mol | 6.80mol | 80%mH2O/mI | 3.025mol |
| Y% (yield) | 89.0% |
Wherein, mH2O/mIFor water and the mass ratio of compound I.
Embodiment 2：
When compound III isI.e. as n=1, when M is Na, the conjunction of its biological buffer
It is as follows into reaction expression：
The preparation method of the biological buffer, specifically includes following steps：
1) compound I is added to after reaction bulb, then plus compound I 80% mass water and stir；
2) reactant liquor ice bath is cooled down into 0 DEG C or so；Response time is 2 hours；
3) compound II is dropped in reactant liquor；
4) post processing, filters, and filter cake carries out recrystallization to obtain pure target product N, N- (2- ethoxys) -2- amino first
Sodium sulfonate.
| Compound I | Compound II | H2O | Compound III | |
| M (quality) | 500g | 330.9g | 400g | 723g |
| N (molal weight) | 3.76mol | 7.52mol | 80%mH2O/mI | 3.27mol |
| Y% (yield) | 87.0% |
Wherein, mH2O/mIFor water and the mass ratio of compound I.
Embodiment 3：
When compound III isI.e. as n=3, when M is Na, the synthesis of its biological buffer
Reaction expression is as follows：
The preparation method of the biological buffer, specifically includes following steps：
1) compound I is added to after reaction bulb, then plus compound I 5% mass water and stir；
2) reactant liquor is warming up to into 90 DEG C；Response time is 0.5 hour；
3) compound II is dropped in reactant liquor；
4) post processing, filters, and filter cake carries out recrystallization to obtain pure target product N, N- (2- ethoxys) -2- aminopropans
Sodium sulfonate.
| Compound I | Compound II | H2O | Compound III | |
| M (quality) | 500g | 415.2g | 25g | 704.4g |
| N (molal weight) | 3.145mol | 9.435mol | 5%mH2O/mI | 2.829mol |
| Y% (yield) | 90.0% |
Wherein, mH2O/mIFor water and the mass ratio of compound I.
Embodiment 4：
When compound III isI.e. as n=3, when M is K, the synthesis of its biological buffer
Reaction expression is as follows：
The preparation method of the biological buffer, specifically includes following steps：
1) compound I is added to after reaction bulb, then plus compound I 40% mass water and stir；
2) reactant liquor is warming up to into 45 DEG C；Response time is 1 hour；
3) compound II is dropped in reactant liquor；
4) filter, filter cake carries out recrystallization (cooling crystallize) to obtain pure target product N, N- (2- ethoxys) -2- ammonia
Base propane sulfonic acid potassium.
| Compound I | Compound II | H2O | Compound III |
| M (quality) | 500g | 248.6g | 25g | 659g |
| N (molal weight) | 2.825mol | 5.65mol | 5%mH2O/mI | 2.488mol |
| Y% (yield) | 88.1% |
Wherein, mH2O/mIFor water and the mass ratio of compound I.
Embodiment 5：
When compound III isI.e. as n=4, when M is Na, its biological buffer
Synthetic reaction formula is as follows：
The preparation method of the biological buffer, specifically includes following steps：
1) compound I is added to after reaction bulb, then plus compound I 80% mass water and stir；
2) reactant liquor ice bath is cooled down into 0 DEG C or so；Response time is 2 hours；
3) compound II is dropped in reactant liquor；
4) post processing, filters, and filter cake carries out recrystallization to obtain pure target product N, N- (2- ethoxys) -2- amino fourths
Sodium sulfonate.
| Compound I | Compound II | H2O | Compound III | |
| M (quality) | 500g | 252g | 400g | 671g |
| N (molal weight) | 2.86mol | 5.72mol | 80%mH2O/mI | 2.55mol |
| Y% (yield) | 89.0% |
Wherein, mH2O/mIFor water and the mass ratio of compound I.
Embodiment 6：
The product I II N of example 1, N- (2- ethoxys) -2-aminoethyl sulfonic acid sodium (i.e. BES sodium salts) 100g are dissolved in
In the water of 300ml, by strong-acid ion exchange resin removing sodium ion, methanol crystallization is added after eluent concentration, separate out white
Solid product N, N- (2- ethoxys) -2-aminoethyl sulfonic acid, as product BES, yield is 80% or so.
Embodiment 7：
Reactant oxirane is substituted for into expoxy propane, i.e., when synthetic isWhen, its life
The synthetic reaction formula of thing buffer agent is as follows：
The preparation method of the biological buffer, specifically includes following steps：
1) compound I is added to after reaction bulb, then plus compound I 80% mass water and stir；
2) reactant liquor ice bath is cooled down into 0 DEG C or so；Response time is 2 hours；
3) compound II is dropped in reactant liquor；
4) post processing, filters, and filter cake carries out recrystallization to obtain pure target product N, N- (2-2- hydroxypropyls) -2- ammonia
Base ethyl sulfonic acid sodium (BES sodium salts).
| Compound I | Compound II | H2O | Compound III | |
| M (quality) | 500g | 394.4g | 400g | 778g |
| N (molal weight) | 3.40mol | 6.80mol | 80%mH2O/mI | 2.958mol |
| Y% (yield) | 87.0% |
Wherein, mH2O/mIFor water and the mass ratio of compound I.
The preferred embodiment of the invention is above are only, the present invention is not restricted to.For those skilled in the art comes
Say, the change or variation of other multi-forms can also be made on the basis of the above description.There is no need to all
Embodiment illustrating.And thus scheme it is extended obvious change or change still in the present invention protection
Within the scope of.
Claims (2)
1. a kind of preparation method of biological buffer, it is characterised in that its reaction expression is as follows：
In formula, n=1-4, M are K or Na；
A kind of preparation method of described biological buffer, comprises the following steps：
1) compound I is added to after reaction bulb, then plus compound I 5%～80% mass water and stir；
2) reactant liquor is warming up to into 0～90 DEG C；
3) compound II is dropped in reactant liquor；
4) post processing, filters, and filter cake carries out recrystallization to obtain pure target product；
The step 3) reaction temperature be 0～90 DEG C, the step 2) response time be 0.5-2 hours；
The mol ratio of the compound I and II is 1:2-1:3.
2. the preparation method of a kind of biological buffer described in claim 1, it is characterised in that the compound II replaces with ring
Ethylene Oxide.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2388816A (en) * | 1942-06-25 | 1945-11-13 | Eastman Kodak Co | Photographic developer |
| CN101161632A (en) * | 2006-10-10 | 2008-04-16 | 中科院嘉兴中心应用化学分中心 | Preparation method of polyhydric alcohol amine |
| CN103382170A (en) * | 2012-10-25 | 2013-11-06 | 潜江永安药业股份有限公司 | Preparation method for taurine |
| CN103665291A (en) * | 2013-11-29 | 2014-03-26 | 陕西科技大学 | Zwitterionic hydrophilic chain extender and preparation method thereof |
| CN103665292A (en) * | 2013-11-29 | 2014-03-26 | 陕西科技大学 | Sulfonic acid type water-based polyurethane chain extender and preparation method thereof |
-
2015
- 2015-06-17 CN CN201510338904.XA patent/CN105037217B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2388816A (en) * | 1942-06-25 | 1945-11-13 | Eastman Kodak Co | Photographic developer |
| CN101161632A (en) * | 2006-10-10 | 2008-04-16 | 中科院嘉兴中心应用化学分中心 | Preparation method of polyhydric alcohol amine |
| CN103382170A (en) * | 2012-10-25 | 2013-11-06 | 潜江永安药业股份有限公司 | Preparation method for taurine |
| CN103665291A (en) * | 2013-11-29 | 2014-03-26 | 陕西科技大学 | Zwitterionic hydrophilic chain extender and preparation method thereof |
| CN103665292A (en) * | 2013-11-29 | 2014-03-26 | 陕西科技大学 | Sulfonic acid type water-based polyurethane chain extender and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| N,N-二（2-羟乙基）-2-氨基乙磺酸钠的合成研究;宋文生等;《化学研究与应用》;20110430;第23卷(第4期);第470-474页 * |
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