CN103804368A - Recovery method of thiamine nitrate in thiamine nitrate mother liquor - Google Patents
Recovery method of thiamine nitrate in thiamine nitrate mother liquor Download PDFInfo
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- CN103804368A CN103804368A CN201210440970.4A CN201210440970A CN103804368A CN 103804368 A CN103804368 A CN 103804368A CN 201210440970 A CN201210440970 A CN 201210440970A CN 103804368 A CN103804368 A CN 103804368A
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- C07D415/00—Heterocyclic compounds containing the thiamine skeleton
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Abstract
The invention discloses a recovery method of thiamine nitrate in a thiamine nitrate mother liquor. The recovery method comprises following steps: 1) pure water and hydrogen peroxide are added into thiothiamine for mixing, and an obtained mixture is subjected to oxidation decolouring so as to obtain a thiamine sulfate solution; 2) an ammonium nitrate solution is added into the thiamine sulfate solution for salt conversing processing so as to obtain a nitrate sulfate thiamine solution, and ammonium hydroxide is added into the nitrate sulfate thiamine solution for neutralization so as to obtain a nitric acid sulfuric acid solution; 3) the nitric acid sulfuric acid solution is filtered so as to obtain thiamine nitrate and a mother liquor containing ammonium sulfate and ammonium nitrate; 4) calcium nitrate is added into the mother liquor containing ammonium sulfate and ammonium nitrate so as to change ammonium sulfate into ammonium nitrate, and obtain calcium sulfate precipitate and a ammonium nitrate solution; 5) the ammonium nitrate solution is subjected to concentration and decolouring; and 6) the concentrated ammonium nitrate solution is added into the thiamine sulfate solution for salt conversing processing, and then ammonium hydroxide is added for neutralization so as to obtain thiamine nitrate.
Description
[technical field]
The present invention relates to a kind of recovery process, especially relate to the recovery method of thiamine mononitrate in a kind of thiamine mononitrate mother liquor.
[background technology]
Existing thiamine mononitrate preparation technology is that thiothiamine turns salt through peroxy-nitric acid ammonium after oxidation, then neutralizes with ammoniacal liquor, separates and obtains thiamine mononitrate, and the ammonium sulfate containing in mother liquor and ammonium nitrate enter after Sewage treatment systems is processed and discharges.There are the following problems for former technique: the one, and liquid containing ammonium sulfate and ammonium nitrate in mother liquor, content reaches respectively 8% and 4%, due to containing high salinity, need to, by just entering biochemical treatment system after dilution, increase the volumetric loading of biochemical treatment system; The 2nd, in mother liquor, contain a certain amount of thiamine mononitrate, run off with mother liquor, do not reclaim.Defect in above-mentioned technique, causes thiamine mononitrate preparation technology's yield not high, is therefore necessary to improve.
[summary of the invention]
The technical problem that the present invention solves is to provide the recovery method of thiamine mononitrate in a kind of thiamine mononitrate mother liquor, become add nitrocalcite that ammonium sulfate is turned to salt in mother liquor into ammonium nitrate, generate sulfate precipitate calcium simultaneously, then filtration obtains the solution that contains ammonium nitrate and thiamine mononitrate, then add a small amount of volatile salt to regulate pH value, remove excessive calcium ion, then carry out filtering and concentrating and obtain sell ammonium concentrated solution, after processing, activated carbon decolorizing is back in sulfuric acid thiamine solution again, for again turning after salt with the ammonia neutralization thiamine mononitrate of getting back with sulfuric acid thiamine solution.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: the recovery method of thiamine mononitrate in a kind of thiamine mononitrate mother liquor, comprises following step:
1) after adding pure water and hydrogen peroxide to mix, after being oxidized and decolouring, obtain sulfuric acid thiamine solution in thiothiamine;
2) in sulfuric acid thiamine solution, add ammonium nitrate solution to turn salt and process to obtain nitric acid-sulfuric acid thiamine solution, then in nitric acid-sulfuric acid thiamine solution, add ammoniacal liquor to neutralize to obtain nitric acid-sulfuric acid solution;
3) mother liquor that nitric acid-sulfuric acid solution filter is obtained to thiamine mononitrate and contain ammonium sulfate and sell ammonium;
4) in the mother liquor that contains ammonium sulfate and sell ammonium, add nitrocalcite that ammonium sulfate is turned to salt and become ammonium nitrate, generate calcium sulfate precipitation and sell ammonium solution;
5) by concentrated ammonium nitrate solution decolouring;
6) ammonium nitrate solution after concentrated is again added in sulfuric acid thiamine solution and turns salt processing, then add the ammonia neutralization thiamine mononitrate of getting back.
After above-mentioned steps four, in sell ammonium solution, add volatile salt, obtain precipitation of calcium carbonate, after filtering, remove calcium carbonate in solution, then solution filter is obtained to comparatively pure ammonium nitrate solution.
Further, in sell ammonium solution, adding the pH value of volatile salt adjustment pin acid ammonium solution is 6.5-7.5.
In above-mentioned steps two and step 5, the concentration of described ammonium nitrate solution is 40%-50%.
The present invention's beneficial effect is compared with prior art:
1, realized the recycling of ammonium salt in mother liquor, by-product calcium sulfate can increase benefit simultaneously;
2, effectively realize the recycle of mother liquor, alleviated the load of sewage disposal;
3, effectively reclaimed the sulfuric acid thiamine in mother liquor, realized and improve yield 1%.
[accompanying drawing explanation]
Accompanying drawing described herein is to be used to provide a further understanding of the present invention, forms the application's a part, but do not form inappropriate limitation of the present invention, in the accompanying drawings:
Fig. 1 is principle schematic of the present invention.
[embodiment]
Below in conjunction with accompanying drawing 1, embodiments of the invention are described.
A recovery method for thiamine mononitrate in thiamine mononitrate mother liquor,
Embodiment mono-:
1) get 93.0 grams of thiothiamines (kilogram or rise or milliliter the unification of unit before and after noting), after adding 200 grams of pure water and 105 grams of hydrogen peroxide to mix, after being oxidized and decolouring, obtain 498 grams of sulfuric acid thiamine solution that concentration is 22.83%;
2) in sulfuric acid thiamine solution, adding 125 grams of concentration is that 40% ammonium nitrate solution turns salt and processes to such an extent that 623 grams of concentration are 18.96% nitric acid-sulfuric acid thiamine solution, then in nitric acid-sulfuric acid thiamine solution, adds 50.0 grams of ammoniacal liquor to neutralize to obtain 673 grams of nitric acid-sulfuric acid solution;
3) nitric acid-sulfuric acid solution filter is obtained to 96.7 grams of solid nitric acid thiamines and 550 grams of mother liquors that contain ammonium sulfate and sell ammonium.And in mother liquor, contain a small amount of thiamine mononitrate;
4) in the mother liquor that contains ammonium sulfate and sell ammonium, add 65.2 grams of nitrocalcite that ammonium sulfate is turned to salt and become 43.62g ammonium nitrate, generate 46.91 grams of calcium sulfate precipitations and 568.11 grams of sell ammonium solution;
5) in sell ammonium solution, adding the pH value of 0.26 gram of volatile salt adjustment pin acid ammonium solution is 6.5, obtains 0.27 gram of precipitation of calcium carbonate, after filtering, removes calcium carbonate in solution, and then solution filter being obtained to comparatively pure concentration is 10.85% ammonium nitrate solution.
6) by concentrated comparatively pure ammonium nitrate solution decolouring;
7) be that 40.23% ammonium nitrate solution again adds in 597.6 grams of sulfuric acid thiamine solution and turns salt processing by the concentration after concentrated, then add the ammonia neutralization thiamine mononitrate of getting back.
Embodiment bis-:
1) get 93.0 grams of thiothiamines (or rising or milliliter the unification of unit before and after noting), after adding 200.0 grams of pure water and 105.0 grams of hydrogen peroxide to mix, after being oxidized and decolouring, obtain 498 grams of sulfuric acid thiamine solution that concentration is 22.83%;
2) in sulfuric acid thiamine solution, adding 100 grams of concentration is that 50% ammonium nitrate solution turns salt and processes to such an extent that 598 grams of concentration are 19.75% nitric acid-sulfuric acid thiamine solution, then in nitric acid-sulfuric acid thiamine solution, adds 50.0 grams of ammoniacal liquor to neutralize to obtain 648 grams of nitric acid-sulfuric acid solution;
3) nitric acid-sulfuric acid solution filter is obtained to 96.8 grams of solid nitric acid thiamines and 550 grams of mother liquors that contain ammonium sulfate and sell ammonium.And in mother liquor, contain a small amount of thiamine mononitrate;
4) in the mother liquor that contains ammonium sulfate and sell ammonium, add 65.2 grams of nitrocalcite that ammonium sulfate is turned to salt and become 43.62 grams of ammonium nitrate, generate 46.91 grams of calcium sulfate precipitations and 568.11 grams of sell ammonium solution;
5) in sell ammonium solution, adding the pH value of 1.52 grams of volatile salts adjustment pin acid ammonium solution is 7.5, obtains 0.28 gram of precipitation of calcium carbonate, after filtering, removes calcium carbonate in solution, and then solution filter being obtained to comparatively pure concentration is 10.82% ammonium nitrate solution.
6) by concentrated comparatively pure ammonium nitrate solution decolouring;
7) be that 42.15% ammonium nitrate solution again adds in 597.6 grams of sulfuric acid thiamine solution and turns salt processing by the concentration after concentrated, then add the ammonia neutralization thiamine mononitrate of getting back.
The above is only in order to convenient explanation the present invention, and not departing from the spiritual category of the present invention's creation, that is familiar with that those skilled in the art of this technology does various simple in a disguised form still belongs to protection scope of the present invention with modification.
Claims (4)
1. a recovery method for thiamine mononitrate in thiamine mononitrate mother liquor, is characterized in that comprising following step:
1) after adding pure water and hydrogen peroxide to mix, after being oxidized and decolouring, obtain sulfuric acid thiamine solution in thiothiamine;
2) in sulfuric acid thiamine solution, add ammonium nitrate solution to turn salt and process to obtain nitric acid-sulfuric acid thiamine solution, then in nitric acid-sulfuric acid thiamine solution, add ammoniacal liquor to neutralize to obtain nitric acid-sulfuric acid solution;
3) mother liquor that nitric acid-sulfuric acid solution filter is obtained to thiamine mononitrate and contain ammonium sulfate and sell ammonium;
4) in the mother liquor that contains ammonium sulfate and sell ammonium, add nitrocalcite that ammonium sulfate is turned to salt and become ammonium nitrate, generate calcium sulfate precipitation and sell ammonium solution;
5) by concentrated ammonium nitrate solution decolouring;
6) ammonium nitrate solution after concentrated is again added in sulfuric acid thiamine solution and turns salt processing, then add the ammonia neutralization thiamine mononitrate of getting back.
2. the recovery method of thiamine mononitrate in thiamine mononitrate mother liquor according to claim 1, it is characterized in that: after above-mentioned steps four, in sell ammonium solution, add volatile salt, obtain precipitation of calcium carbonate, after filtering, remove calcium carbonate in solution, then solution filter is obtained to comparatively pure ammonium nitrate solution.
3. the recovery method of thiamine mononitrate in thiamine mononitrate mother liquor according to claim 2, is characterized in that: the pH value that adds volatile salt adjustment pin acid ammonium solution in sell ammonium solution is 6.5-7.5.
4. according to the recovery method of thiamine mononitrate in the thiamine mononitrate mother liquor described in claim 1,2 or 3, it is characterized in that: in above-mentioned steps two and step 5, the concentration of described ammonium nitrate solution is 40%-50%.
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| CN201210440970.4A CN103804368A (en) | 2012-11-07 | 2012-11-07 | Recovery method of thiamine nitrate in thiamine nitrate mother liquor |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105384735A (en) * | 2015-10-19 | 2016-03-09 | 天津大学 | Preparation method for bulk crystal product of thiamine nitrate |
| CN106588907A (en) * | 2016-11-07 | 2017-04-26 | 华中药业股份有限公司 | Crystallization method of thiamine mononitrate |
| CN107903254A (en) * | 2017-10-10 | 2018-04-13 | 江苏兄弟维生素有限公司 | A kind of thiamine mononitrate new technique for synthesizing |
| CN107903255A (en) * | 2017-10-10 | 2018-04-13 | 江苏兄弟维生素有限公司 | A kind of new synthesis mode of thiamine mononitrate |
| CN109942568A (en) * | 2019-04-03 | 2019-06-28 | 赤峰制药股份有限公司 | A kind of thiamine mononitrate preparation method |
| CN112851659A (en) * | 2020-12-31 | 2021-05-28 | 江苏兄弟维生素有限公司 | Preparation method of thiamine oxidation liquid and thiamine nitrate preparation method applying same |
| CN114180599A (en) * | 2021-12-23 | 2022-03-15 | 江苏兄弟维生素有限公司 | Process for recovering ammonium nitrate from thiamine nitrate mother liquor and application thereof |
| CN114181203A (en) * | 2021-12-24 | 2022-03-15 | 江苏兄弟维生素有限公司 | Preparation method of thiamine hydrochloride, application and vitamin B1 |
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| CN1459449A (en) * | 2002-05-22 | 2003-12-03 | 东北制药总厂 | New method of preparing ritamin B1 hydrochloride using thiohydrothiamine |
| JP2007023001A (en) * | 2005-07-21 | 2007-02-01 | Daiichi Sankyo Healthcare Co Ltd | Method for stabilizing thiamine compounds |
| CN101638409A (en) * | 2009-08-24 | 2010-02-03 | 江西天新药业有限公司 | Preparation method of 4-methyl-3-[(2- methyl-4-amido-5- purimidyl) methyl]-5-(2-hydroxide ethide) thiazole onium nitrate |
| CN101955307A (en) * | 2010-10-27 | 2011-01-26 | 同济大学 | Method for treating vitamin B1 production waste water |
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- 2012-11-07 CN CN201210440970.4A patent/CN103804368A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1459449A (en) * | 2002-05-22 | 2003-12-03 | 东北制药总厂 | New method of preparing ritamin B1 hydrochloride using thiohydrothiamine |
| JP2007023001A (en) * | 2005-07-21 | 2007-02-01 | Daiichi Sankyo Healthcare Co Ltd | Method for stabilizing thiamine compounds |
| CN101638409A (en) * | 2009-08-24 | 2010-02-03 | 江西天新药业有限公司 | Preparation method of 4-methyl-3-[(2- methyl-4-amido-5- purimidyl) methyl]-5-(2-hydroxide ethide) thiazole onium nitrate |
| CN101955307A (en) * | 2010-10-27 | 2011-01-26 | 同济大学 | Method for treating vitamin B1 production waste water |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105384735A (en) * | 2015-10-19 | 2016-03-09 | 天津大学 | Preparation method for bulk crystal product of thiamine nitrate |
| CN105384735B (en) * | 2015-10-19 | 2018-12-28 | 天津大学 | A kind of preparation method of thiamine mononitrate bulk crystals product |
| CN106588907A (en) * | 2016-11-07 | 2017-04-26 | 华中药业股份有限公司 | Crystallization method of thiamine mononitrate |
| CN107903254A (en) * | 2017-10-10 | 2018-04-13 | 江苏兄弟维生素有限公司 | A kind of thiamine mononitrate new technique for synthesizing |
| CN107903255A (en) * | 2017-10-10 | 2018-04-13 | 江苏兄弟维生素有限公司 | A kind of new synthesis mode of thiamine mononitrate |
| CN109942568A (en) * | 2019-04-03 | 2019-06-28 | 赤峰制药股份有限公司 | A kind of thiamine mononitrate preparation method |
| CN112851659A (en) * | 2020-12-31 | 2021-05-28 | 江苏兄弟维生素有限公司 | Preparation method of thiamine oxidation liquid and thiamine nitrate preparation method applying same |
| CN114180599A (en) * | 2021-12-23 | 2022-03-15 | 江苏兄弟维生素有限公司 | Process for recovering ammonium nitrate from thiamine nitrate mother liquor and application thereof |
| CN114181203A (en) * | 2021-12-24 | 2022-03-15 | 江苏兄弟维生素有限公司 | Preparation method of thiamine hydrochloride, application and vitamin B1 |
| CN114181203B (en) * | 2021-12-24 | 2023-08-18 | 江苏兄弟维生素有限公司 | Preparation method of thiamine hydrochloride, application and vitamin B1 |
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Application publication date: 20140521 |