CN103467312B - Bis-Tris synthesis method - Google Patents
Bis-Tris synthesis method Download PDFInfo
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- CN103467312B CN103467312B CN201310424640.0A CN201310424640A CN103467312B CN 103467312 B CN103467312 B CN 103467312B CN 201310424640 A CN201310424640 A CN 201310424640A CN 103467312 B CN103467312 B CN 103467312B
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Abstract
The invention provides a Bis-Tris synthesis method which comprises the steps of (1) preparing a solution from 5g of sodium hydrogen sulfite and 10ml of water, mixing the solution with 50ml of absolute ethyl alcohol, and introducing ethylene oxide gas into the mixed solution to obtain a saturated aqueous solution of ethylene oxide; (2) heating 100ml of the saturated solution to 30-35 DEG C, pouring 60g of Tris into the solution, after 2 hours of slow dissolution and clarification, mixing 20g of sodium hydroxide and 20ml of water, dropwise adding the mixture into the solution, controlling the pH value of the solution at 9.5-10.0, and keeping the reaction for 6-8 hours; (3) performing vacuum dehydration and hot filtration on the solution after the reaction in the step (2), adding absolute ethyl alcohol for dispersion, and cooling to precipitate a product. According to the method provided by the invention, Bis-Tris is synthesized by use of the saturated solution of ethylene oxide; the method is safe and reliable and realizes sufficient reaction and high product content.
Description
Technical field
The present invention relates to biological agent technical field, particularly the synthetic method of a kind of Bis-Tris.
Background technology
Bis-Tris two [three (methylol)] aminomethane by name, molecular formula is: C8H19NO5, white powder, main application: damping fluid, for detecting creatine kinase; Also for available protecting oxyphorase in lyophilize.
In the prior art, Bis-Tris is that when adopting Tris and oxyethane to synthesize, Ring oxidative ethane is very easy to blast in high-temperature reaction process, and this reactive mode also can bring the problem that reaction is incomplete, yield is low.Such as, epoxy chloropropane gas can reach the pressure of 141pka 30 DEG C time, and when adopting Ring oxidative ethane directly to synthesize when temperature of reaction is 85-90 DEG C, oxyethane is in high pressure conditions, and penetration power is very strong.
Summary of the invention
For solving problems of the prior art, the embodiment of the present invention provides the synthetic method of a kind of safe and reliable, Bis-Tris that sufficient reacting, product assay are high; The synthetic method of Bis-Tris of the present invention, by Ring oxidative ethane is passed in liquid aqueous solution, makes it to form oxyethane saturated solution, and then and Tris reaction formation the finished product.
The synthetic method of Bis-Tris of the present invention:
Step 1, get 5 grams of sodium bisulfites with 10 ml waters dilution after be mixed with sodium sulfite solution, then this sodium sulfite solution is mixed with 50 milliliters of dehydrated alcohols, again ethylene oxide gas is passed in this mixing solutions and make saturated aqueous solution of ethylene oxide, and make saturation ratio solution must not lower than 8%;
Step 2, to get in step 1 obtained oxyethane saturated solution 100 milliliters, be heated to 30-35 degree, then get Tris60 gram and pour in this oxyethane saturated solution, make it slowly clearly molten; React after 2 hours, instill in above-mentioned solution after getting 20 grams, sodium hydroxide and the mediation of 20 ml waters, the pH value of solution is controlled between 9.5-10.0 all the time, and terminates after sustained reaction 6-8 hour;
Step 3, by step 2 reaction terminate after solution carry out vacuum hydro-extraction, heat filtering after, add dehydrated alcohol and disperse, cooling wait for product separate out, the Bis-Tris of white powder can be obtained.
The synthetic method of Bis-Tris of the present invention, due to be adopt Ring oxidative ethane is passed in liquid aqueous solution form oxyethane saturated solution mode to synthesize Bis-Tris, so its reaction process avoids in prior art adopt the gas problem that directly synthesis meeting build-up of pressure is too high, synthetic method of the present invention is safe and reliable, sufficient reacting, and product assay is high.
Embodiment
For making the technical problem to be solved in the present invention, technical scheme and advantage clearly, be described in detail below in conjunction with specific embodiment.
The equipment facility that synthetic method uses of the Bis-Tris of the embodiment of the present invention comprises: there-necked flask, beaker, graduated cylinder, electric mixer; Desired raw material equipment comprises: oxyethane, sodium bisulfite, dehydrated alcohol, Tirs, sodium hydroxide, PH test paper; Wherein, Tirs is Tutofusin tris, and molecular formula is C4H11NO3, and relative molecular weight is 121.14; Ethylene oxide molecule formula is C2H4O.
The synthetic method of the Bis-Tris of the embodiment of the present invention is:
Step 1, get 5 grams of sodium bisulfites with 10 ml waters dilution after be mixed with sodium sulfite solution, put into 500 milliliters of there-necked flasks, then 50 milliliters of dehydrated alcohols are added in there-necked flask and mix, again ethylene oxide gas is passed in there-necked flask, alcoholic solution containing sodium bisulfite is fully absorbed and makes it to become saturated aqueous solution of ethylene oxide, and saturation ratio solution lower than 8%, generally must not be remained between 8%-20%;
Step 2, to get there-necked flask for subsequent use, gets oxyethane saturated solution 100 milliliters obtained in step 1 and put into this there-necked flask, be heated to 30-35 degree, then get 60 grams of Tris and pour in this oxyethane saturated solution, makes it slowly clearly molten; React after 2 hours, after getting 20 grams, sodium hydroxide and the mediation of 20 ml waters, instillation is equipped with in the there-necked flask of above-mentioned solution, and the pH value of solution is controlled between 9.5-10.0 all the time, and sustained reaction 6-8 hour;
Step 3, reaction in step 2 is terminated after solution carry out vacuum hydro-extraction, heat filtering after, add dehydrated alcohol and carry out disperseing, lower the temperature and wait for product precipitation, the Bis-Tris of white powder can be obtained.Obtained BIS-TRIS molecular formula is C8H19NO5, and relative molecular weight is 209.2.
The synthetic method of Bis-Tris of the present invention, due to be adopt Ring oxidative ethane is passed in liquid aqueous solution form oxyethane saturated solution mode to synthesize Bis-Tris, so its reaction process avoids in prior art adopt the gas problem that directly synthesis meeting build-up of pressure is too high, synthetic method of the present invention is safe and reliable, sufficient reacting, and product assay is high.
The above is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from principle of the present invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (1)
1. a synthetic method of Bis-Tris, is characterized in that, comprises the following steps:
Step 1, get 5 grams of sodium bisulfites with 10 ml waters dilution after be mixed with sodium sulfite solution, then this sodium sulfite solution is mixed with 50 milliliters of dehydrated alcohols, again ethylene oxide gas is passed in this mixing solutions and make saturated aqueous solution of ethylene oxide, and make the saturation concentration of saturated aqueous solution of ethylene oxide be 8% ~ 20%;
Step 2, to get in step 1 obtained oxyethane saturated solution 100 milliliters, be heated to 30-35 degree, then get Tris60 gram and pour in this oxyethane saturated solution, make it slowly clearly molten; React after 2 hours, instill in above-mentioned solution after getting 20 grams, sodium hydroxide and the mediation of 20 ml waters, the pH value of solution is controlled between 9.5-10.0 all the time, and terminates after sustained reaction 6-8 hour;
Step 3, by step 2 reaction terminate after solution carry out vacuum hydro-extraction, heat filtering after, add dehydrated alcohol and disperse, cooling wait for product separate out, the Bis-Tris of white powder can be obtained.
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| CN201310424640.0A CN103467312B (en) | 2013-09-18 | 2013-09-18 | Bis-Tris synthesis method |
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| CN201310424640.0A CN103467312B (en) | 2013-09-18 | 2013-09-18 | Bis-Tris synthesis method |
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| CN103467312B true CN103467312B (en) | 2015-07-15 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4781921A (en) * | 1986-10-06 | 1988-11-01 | The University Of Akron | Hydrogels of quadrol methacrylate polymers |
| CN101402576A (en) * | 2008-10-23 | 2009-04-08 | 浙江大学 | Method for producing bi(2-hydroxyethyl)imino-tri(hydroxymethyl)methyl hydride |
| CN101659621A (en) * | 2008-08-27 | 2010-03-03 | 苏州工业园区亚科化学试剂有限公司 | Method for preparing bi[tri(hydroxylmethyl)] aminomethane |
| CN101735077A (en) * | 2009-12-11 | 2010-06-16 | 广西壮族自治区化工研究院 | Production method and production equipment for synthesizing ethanolamine by ethylene oxide |
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2013
- 2013-09-18 CN CN201310424640.0A patent/CN103467312B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4781921A (en) * | 1986-10-06 | 1988-11-01 | The University Of Akron | Hydrogels of quadrol methacrylate polymers |
| CN101659621A (en) * | 2008-08-27 | 2010-03-03 | 苏州工业园区亚科化学试剂有限公司 | Method for preparing bi[tri(hydroxylmethyl)] aminomethane |
| CN101402576A (en) * | 2008-10-23 | 2009-04-08 | 浙江大学 | Method for producing bi(2-hydroxyethyl)imino-tri(hydroxymethyl)methyl hydride |
| CN101735077A (en) * | 2009-12-11 | 2010-06-16 | 广西壮族自治区化工研究院 | Production method and production equipment for synthesizing ethanolamine by ethylene oxide |
Non-Patent Citations (1)
| Title |
|---|
| 由含8%环氧乙烷水溶液合成乙醇胺的工艺研究;文民锦等;《石油化工高等学校学报》;19940319;第7卷(第1期);第16-17页 * |
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