CN103408603A - Chemical preparation method of D-ribose - Google Patents
Chemical preparation method of D-ribose Download PDFInfo
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- CN103408603A CN103408603A CN2013103715533A CN201310371553A CN103408603A CN 103408603 A CN103408603 A CN 103408603A CN 2013103715533 A CN2013103715533 A CN 2013103715533A CN 201310371553 A CN201310371553 A CN 201310371553A CN 103408603 A CN103408603 A CN 103408603A
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Abstract
The invention provides a chemical preparation method of D-ribose. The chemical preparation method mainly comprises the following steps of carrying out D-arabinose isomerization reaction, purification and impurity removal, chromatographic separation as well as concentration and crystallization to obtain a D-ribose crystal, wherein the mass percentage of the D-ribose is over 98.6%. The chemical preparation method has the beneficial effects that a small amount of carbohydrate-used activated carbon for decoloration and a small amount of hydrochloric acid and sodium hydroxide for impurity removal are only consumed in the whole technical process, and no wastes are generated in other links, so that the sanitary production is realized, no environment pollution is caused, meanwhile, the production cost is reduced, the basis is provided for the industrial production, and the heavy demand on the aspects such as medicines, chemical industry and the like can be met.
Description
Technical field
The invention belongs to the functional sugar production field, be specifically related to a kind of chemical preparation process of D-ribose.
Background technology
D-ribose is the monose that contains five carbon atoms, is epochmaking aldopentose, and large form mainly with piperylene or glucosides exists in vivo.D-ribose is genetic material--the important composition material of Yeast Nucleic Acid in organism, is in hub site in nucleosides material, protein, metabolism of fat, has important physiological function and wide application prospect.D-ribose is the important intermediate of many nucleic acid drugs, and nucleic acid drug is the important means of mankind nowadays treatment virus, tumour, acquired immune deficiency syndrome (AIDS).In prior art, not yet find to prepare by chemical process the patent documentation of D-ribose.Traditional production method adopts microbe fermentation method to prepare D-ribose mostly, method is to utilize a kind of bacterial classification (for example subtilis), in the fermention medium that contains the substrate that the mixing sugar source such as amylum hydrolysate of the sugar forms, carry out aerobic fermentation, then from tunning, collecting the D-ribose clear liquid.But in fermented liquid, the removal of thalline and residual solid substance will obtain the clear liquid of D-ribose with a series of processing such as flocculation, centrifugal, filtrations, has increased the production technique cost, and the thalline after fermentation is difficult to process, and brings immense pressure to environmental protection.
Summary of the invention
The object of the present invention is to provide a kind of chemical preparation process of producing D-ribose, the above defect existed to overcome prior art.
The chemical preparation process of D-ribose of the present invention mainly comprises the following steps:
(1) D-R isomerization reaction: take a certain amount of D-R, add water and be mixed with the solution that mass concentration is 10%-30%, 0.5%-1.2% according to the D-R quality adds isomery agent ammonium molybdate, regulate the pH value between 2.5-4.8, control temperature at 80 ℃-130 ℃, reaction times 1-3 hour, obtain isomery liquid;
(2) purification and impurity removal: the 1-5% by isomery liquid amount of dry matter adds gac, insulation decolouring, filtration under 60-80 ℃, through negative resin and the purification of positive resin, remove isomery agent and the impurity in reaction solution again, obtain the D-ribose scavenging solution, in the scavenging solution dry, the D-ribose mass content is 20-40%;
(3) chromatographic separation: utilize simulated moving bed technology that the D-ribose scavenging solution is carried out to chromatographic separation, obtain D-ribose purification liquid, collecting D-ribose quality percentage composition in purification liquid dry is to be not less than 75% part, by D-ribose quality percentage composition in purification liquid dry, be that Partial purification liquid below 75% returns to chromatographic fractionation system again and continues to separate, continue to collect D-ribose quality percentage composition in purification liquid dry and be not less than 75% purification liquid;
(4) condensing crystal: the quality percentage composition that chromatographic separation is obtained is that D-ribose liquid vacuum concentration more than 75% is to being more than 98.5% without moisture or mass percentage concentration; In the time of 75 ℃, to concentrated solution, add dehydrated alcohol, the dosage of dehydrated alcohol is 2-5 times of concentrated solution volume; Stir cooling, be cooled to sub-zero zero according to the speed of 0.5 ℃ of-5 ℃/h, now crystallization goes out a large amount of white crystals, and centrifugation obtains the D-ribose crystal, and wherein D-ribose quality percentage composition is more than 98.6%.
Positively effect of the present invention is: a small amount of hydrochloric acid and sodium hydroxide when whole technological process only consumes minute quantity craboraffin and purification and impurity removal when decolouring, all the other links are all without generation of waste materials, realized cleaner production, do not cause environmental pollution, reduced simultaneously production cost, for suitability for industrialized production provides foundation, can meet the heavy demand of the aspects such as medicine, chemical industry.
Embodiment
Embodiment 1
(1) D-R isomerization reaction: take the 500g D-R, add water 1200 grams, be mixed with mass percentage concentration and be 30% solution, according to 1.2% of D-R quality, add isomery agent ammonium molybdate 6 grams, regulate pH value to 4.8, control temperature at 130 ℃, in 3 hours reaction times, obtain isomery liquid;
(2) purification and impurity removal: add gac 18 grams by 5% of isomery liquid amount of dry matter, insulation is 40 minutes under 80 ℃, decolouring, filtration, treat that temperature is down to below 40 ℃, through D301 resin and the purification of 001 * 7 resin, remove isomery agent and the impurity in reaction solution again, obtain the D-ribose scavenging solution, in the scavenging solution dry, the D-ribose mass content is 21.8%;
(3) chromatographic separation: utilize simulated moving bed technology that the D-ribose scavenging solution is carried out to chromatographic separation, obtain D-ribose purification liquid.D-ribose quality percentage composition in purification liquid dry is not less than to 75% purification liquid collection, by D-ribose quality percentage composition in purification liquid dry, be that purification liquid below 75% returns to chromatographic fractionation system again and continues to separate, continue to collect D-ribose quality percentage composition in purification liquid dry and be not less than 75% purification liquid;
(4) condensing crystal: the quality percentage composition that chromatographic separation is obtained is 88% D-ribose liquid vacuum concentration to without moisture.In the time of 75 ℃, to concentrated solution, add dehydrated alcohol 300ml, stir cooling, according to the speed of 5 ℃ ∕ h, be cooled to-5 ℃, now crystallization goes out a large amount of white crystals, and centrifugation obtains the D-ribose crystal, and wherein D-ribose quality percentage composition is 98.6%.
Embodiment 2
(1) D-R isomerization reaction: take the 800g D-R, add water 7200 grams, be mixed with mass concentration and be 10% solution, according to 0.5% of D-R quality, add isomery agent ammonium molybdate 6 grams, regulate pH value to 2.5, control temperature at 80 ℃, in 1 hour reaction times, obtain isomery liquid;
(2) purification and impurity removal: add gac 7.2 grams by 1% of isomery liquid amount of dry matter, insulation is 30 minutes under 75 ℃, decolouring, filtration, treat that temperature is down to below 40 ℃, through D202 resin and the purification of 001 * 4 resin, remove isomery agent and the impurity in reaction solution again, obtain the D-ribose scavenging solution, in the scavenging solution dry, D-ribose quality percentage composition is 36.2%;
(3) chromatographic separation: utilize simulated moving bed technology that the D-ribose scavenging solution is carried out to chromatographic separation, obtain D-ribose purification liquid.D-ribose quality percentage composition in purification liquid dry is not less than to 75% purification liquid collection, by D-ribose quality percentage composition in purification liquid dry, be that purification liquid below 75% returns to chromatographic fractionation system again and continues to separate, continue to collect D-ribose quality percentage composition in purification liquid dry and be not less than 75% purification liquid;
(4) condensing crystal: the quality percentage composition that chromatographic separation is obtained is that 90% D-ribose liquid vacuum concentration to mass percentage concentration is more than 98.5%.In the time of 75 ℃, to concentrated solution, add dehydrated alcohol 1200ml, stir cooling, according to the speed of 1 ℃ ∕ h, be cooled to-5 ℃, now crystallization goes out a large amount of white crystals, and centrifugation obtains the D-ribose crystal, and wherein D-ribose quality percentage composition is 99.2%.
Embodiment 3
(1) D-R isomerization reaction: take the 5000g D-R, add water 23000 grams, be mixed with mass percentage concentration and be 18% solution, according to 0.6% of D-R quality, add isomery agent ammonium molybdate 30 grams, regulate pH value to 3.14, control temperature at 120 ℃, in 2 hours reaction times, obtain isomery liquid;
(2) purification and impurity removal: add gac 136.8 grams by 3.3% of isomery liquid amount of dry matter, insulation is 40 minutes under 75 ℃, decolouring, filtration, treat that temperature is down to below 40 ℃, through D311 resin and the purification of D001 resin, remove isomery agent and the impurity in reaction solution again, obtain the D-ribose scavenging solution, in the scavenging solution dry, D-ribose quality percentage composition is 35.6%;
(3) chromatographic separation: utilize simulated moving bed technology that the D-ribose scavenging solution is carried out to chromatographic separation, obtain D-ribose purification liquid.D-ribose quality percentage composition in purification liquid dry is not less than to 75% purification liquid collection, by D-ribose quality percentage composition in purification liquid dry, be that purification liquid below 75% returns to chromatographic fractionation system again and continues to separate, continue to collect D-ribose quality percentage composition in purification liquid dry and be not less than 75% purification liquid;
(4) condensing crystal: the quality percentage composition that chromatographic separation is obtained is 92% D-ribose liquid vacuum concentration to without moisture.In the time of 75 ℃, to concentrated solution, add dehydrated alcohol 400ml, stir cooling, according to the speed of 0.5 ℃ ∕ h, be cooled to-5 ℃, now crystallization goes out a large amount of white crystals, and centrifugation obtains the D-ribose crystal, and wherein D-ribose quality percentage composition is 99.3%.
Claims (1)
1. a chemical preparation process of producing D-ribose, is characterized in that, mainly comprises the following steps:
(1) D-R isomerization reaction: take a certain amount of D-R, add water and be mixed with the solution that mass concentration is 10%-30%, 0.5%-1.2% according to the D-R quality adds isomery agent ammonium molybdate, regulate the pH value between 2.5-4.8, control temperature at 80 ℃-130 ℃, reaction times 1-3 hour, obtain isomery liquid;
(2) purification and impurity removal: the 1-5% by isomery liquid amount of dry matter adds gac, insulation decolouring, filtration under 60-80 ℃, through negative resin and the purification of positive resin, remove isomery agent and the impurity in reaction solution again, obtain the D-ribose scavenging solution, in the scavenging solution dry, the D-ribose mass content is 20-40%;
(3) chromatographic separation: utilize simulated moving bed technology that the D-ribose scavenging solution is carried out to chromatographic separation, obtain D-ribose purification liquid, collecting D-ribose quality percentage composition in purification liquid dry is to be not less than 75% part, by D-ribose quality percentage composition in purification liquid dry, be that Partial purification liquid below 75% returns to chromatographic fractionation system again and continues to separate, continue to collect D-ribose quality percentage composition in purification liquid dry and be not less than 75% purification liquid;
(4) condensing crystal: the quality percentage composition that chromatographic separation is obtained is that D-ribose liquid vacuum concentration more than 75% is to being more than 98.5% without moisture or mass percentage concentration; In the time of 75 ℃, to concentrated solution, add dehydrated alcohol, the dosage of dehydrated alcohol is 2-5 times of concentrated solution volume; Stir cooling, be cooled to sub-zero zero according to the speed of 0.5 ℃ of-5 ℃/h, now crystallization goes out a large amount of white crystals, and centrifugation obtains the D-ribose crystal, and wherein D-ribose quality percentage composition is more than 98.6%.
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| CN2013103715533A CN103408603A (en) | 2013-08-23 | 2013-08-23 | Chemical preparation method of D-ribose |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103665055A (en) * | 2013-12-23 | 2014-03-26 | 江西苏克尔新材料有限公司 | Method for purifying 2-deoxy-L-ribose |
| CN104447888A (en) * | 2014-12-04 | 2015-03-25 | 山东福田药业有限公司 | Preparation method and application of allulose |
| CN109232676A (en) * | 2018-11-16 | 2019-01-18 | 山东福田药业有限公司 | A kind of separation method of L- ribose |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4602086A (en) * | 1983-10-13 | 1986-07-22 | Tokyo Tanabe Company, Limited | Method of producing solution containing D-ribose |
| JPS61212592A (en) * | 1985-03-19 | 1986-09-20 | Tokyo Tanabe Co Ltd | Production of d-ribose |
| CN101450956A (en) * | 2007-12-07 | 2009-06-10 | 山东福田药业有限公司 | Method for improving ribose purity |
| CN101891773A (en) * | 2010-07-15 | 2010-11-24 | 山东福田药业有限公司 | Process for preparing L-ribose |
-
2013
- 2013-08-23 CN CN2013103715533A patent/CN103408603A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4602086A (en) * | 1983-10-13 | 1986-07-22 | Tokyo Tanabe Company, Limited | Method of producing solution containing D-ribose |
| JPS61212592A (en) * | 1985-03-19 | 1986-09-20 | Tokyo Tanabe Co Ltd | Production of d-ribose |
| CN101450956A (en) * | 2007-12-07 | 2009-06-10 | 山东福田药业有限公司 | Method for improving ribose purity |
| CN101891773A (en) * | 2010-07-15 | 2010-11-24 | 山东福田药业有限公司 | Process for preparing L-ribose |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103665055A (en) * | 2013-12-23 | 2014-03-26 | 江西苏克尔新材料有限公司 | Method for purifying 2-deoxy-L-ribose |
| CN104447888A (en) * | 2014-12-04 | 2015-03-25 | 山东福田药业有限公司 | Preparation method and application of allulose |
| CN109232676A (en) * | 2018-11-16 | 2019-01-18 | 山东福田药业有限公司 | A kind of separation method of L- ribose |
| CN109232676B (en) * | 2018-11-16 | 2021-08-03 | 山东福田药业有限公司 | Separation method of L-ribose |
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Effective date of registration: 20151012 Address after: 266031, 1001/1002 building, 177 Shandong Road, Sifang Road, Sifang, Shandong, Qingdao Applicant after: Shandong Futaste Technology Group Co., Ltd. Address before: 251200 Yucheng, Shandong, South Ring Road, No. 666, No. Applicant before: Shandong Futian Medicine Industry Co., Ltd. |
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Application publication date: 20131127 |