CN102627601B - Production technology of inositol nicotinate - Google Patents
Production technology of inositol nicotinate Download PDFInfo
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- CN102627601B CN102627601B CN201210079112.1A CN201210079112A CN102627601B CN 102627601 B CN102627601 B CN 102627601B CN 201210079112 A CN201210079112 A CN 201210079112A CN 102627601 B CN102627601 B CN 102627601B
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Abstract
The invention discloses a production technology of inositol nicotinate, and changes the recovery method of pyridine to alkali ion layering method. By using the principle of like polarity ion effect, the invention employs sodium hydroxide to dissociate salified pyridine, and subjects a mixture of pyridine and water to effective layering, thus achieving the purpose of pyridine recovery. Changing dichlorobenzene extraction method to alkali ion layering method reduces the unit consumption of pyridine by 91.5%, and nonuse of dichlorobenzene any more reduces dichlorobenzene consumption to zero, thus effectively reducing production cost, realizing energy saving, emission lowering and consumption reduction, as well as ecological environment protection.
Description
Technical field
The present invention relates to medicine and foodstuff production raw material field, more particularly, relate to a kind of Inositol Nicotinate new process of production.
Background technology
Inositol Nicotinate is a kind of peripheral vasodilation agent of gentleness, has the cholesterol of reduction and the effect of expansion peripheral vessel, is adjuvant drug and the nourishment food additive of hypercholesterolemia and atherosclerosis.Inositol Nicotinate is hydrolyzed to nicotinic acid and inositol in vivo gradually, therefore have the two the pharmacological action of nicotinic acid and inositol.Inositol Nicotinate tool effect for reducing fat, its vasorelaxation action relaxes compared with nicotinic acid and lasting, the side effect such as do not take the flush after nicotinic acid and have a stomach upset.Inositol Nicotinate optionally makes diseased region and is subject to the vasodilation of the sensitive part of cold stimulation, to the dilating effect of normal blood vessels a little less than.In addition and have effects such as thrombus, anti-freezing, anti-fatty liveranti-fatty liver, reduction capillary fragility.Inositol Nicotinate has very important significance to human body, and therefore, this product is widely used at medicine, food and cosmetic field, and market demand is quite large, and a whole world year current needs amount can reach 600 tons of left and right.
Producing Inositol Nicotinate will be with a large amount of pyridines as solvent (produces one ton of Inositol Nicotinate will with 3 tons of pyridines as solvent) when carrying out chlorination reaction.What traditional technology adopted when pyridine reclaims is dichlorobenzene extraction process.Dichlorobenzene extraction ratio juris is: application pyridine is dissolved in the physical properties of dichlorobenzene, and the pyridine extraction in the mixture of pyridine and water is dissolved in after dichlorobenzene, and pyridine is separated with water, and then by distillation method, pyridine and dichlorobenzene is carried out to Separation and Recovery.Due to solubleness partition ratio, there is 30% pyridine nearly from water, not extract, cause having 30% pyridine to be nearly discharged as waste water.Because dichlorobenzene boiling point is higher, reclaiming dichlorobenzene also will have 15% consumption again.Therefore, one ton of Inositol Nicotinate of every production consumes pyridine up to 0.94 ton, consumes dichlorobenzene up to 0.15 ton.This not only causes a large amount of wastes in starting material and energy man-hour, and severe contamination environment.
The production technique raw materials consumption traditional due to Inositol Nicotinate is large, environmental pollution is serious, the production cycle is long, can not adapt to socio-economic development requirement.
Summary of the invention
Technical problem to be solved by this invention is, overcomes the deficiencies in the prior art, and a kind of Inositol Nicotinate production technique is provided.
Inositol Nicotinate production technique of the present invention, according to following step, carry out:
1, chlorination reaction: moisture content is no more than to 0.5% pyridine 100kg, add in dry 1000L enamel reactor, then add phosphorus oxychloride 107kg, after stirring well, under cooling conditions, add gradually nicotinic acid 150kg, add post-heating and be warming up to 65-75 ℃, insulation reaction 0.8-1.2 hour;
2, esterification: slowly add inositol under cooling conditions, add inositol post-heating and be warming up to 80-90 ℃, react approximately 1 hour;
3, rejection filter wash water: reactant is stirred with tap water, carry out rejection filter after cooling, gained rejection filter thing washs to throwing away liquid non-pyridine bitter taste by hot purified water, filter cake is dried and obtained Inositol Nicotinate crude product;
4, decolorizing and refining: Inositol Nicotinate crude product is dissolved in to DMF, and with activated carbon decolorizing, the product drying after decolouring obtains Inositol Nicotinate finished product;
5, reclaim pyridine:
1., mother liquor that rejection filter wash water step is thrown away collects in retort, every crowd of mother liquor 900～1000L, hydro-oxidation sodium (sheet alkali), is adjusted to 9～10 by pH, air distillation is to till the fraction non-pyridine taste steaming;
2., cut proceeds to free tank, adds sheet alkali 150～175kg, opens and stirs 0.5-1 hour, more standing 1～1.5 hour, and oil reservoir is isolated and delivered to rectifying post, the above-mentioned steps that water layer is joined to lower batch of mother liquor is used in 1.;
3., slightly heating up in a steamer in the oil reservoir suction rectifying tank of gained, air distillation, reflux and control 200 1 300L/hr, separate and be controlled at 30-40L/hr, when rising to 110～112 ℃, tower top temperature starts to collect positive component, positive component check pyridine moisture content≤0.40%, can be used pyridinium crosslink chlorination reaction step.
Traditional technology adopts dichlorobenzene extraction process when reclaiming pyridine, causes one ton of Inositol Nicotinate pyridine unit consumption of every production up to 0.94 ton, and dichlorobenzene consumption is up to 0.15 ton.
The present invention is the principle of application same sex ionic effect, uses sodium hydroxide that the pyridine of salify is free out, and the mixture of pyridine and water is carried out to effective layering, thereby reach the object that reclaims pyridine.The innovative point key of this patent invention is to change dichlorobenzene extraction process into basic ion top and bottom process; thereby make pyridine unit consumption reduce by 91.5%; do not re-use dichlorobenzene; make the consumption of dichlorobenzene reduce to zero; thereby effectively reduced production cost; realize energy-saving and emission-reduction consumption reduction, protected ecotope.
Apply the raw material consumption contrast of this process and application traditional technology: unit: kg
| Material name | Application traditional technology unit consumption | Application invention technique unit consumption | Average reduction consumes |
| Inositol | 0.2660 | 0.2520 | 5.3％ |
| Nicotinic acid | 1.1093 | 1.0939 | 1.4％ |
| Phosphorus oxychloride | 0.7965 | 0.7830 | 1.7％ |
| Pyridine | 0.9400 | 0.0860 | 91.5％ |
| Dichlorobenzene | 0.1500 | 0 | 100％ |
| Sheet alkali | 0 | 1.1160 | - |
Embodiment
Below the present invention is described further.
Inositol Nicotinate production technique of the present invention, according to following step, carry out:
1, chlorination reaction: moisture content is no more than to 0.5% pyridine 100kg, add in dry 1000L enamel reactor, then add phosphorus oxychloride 107kg, after stirring well, under cooling conditions, add gradually nicotinic acid 150kg, add post-heating and be warming up to 65-75 ℃, insulation reaction 0.8-1.2 hour;
2, esterification: slowly add inositol under cooling conditions, add inositol post-heating and be warming up to 80-90 ℃, react approximately 1 hour;
3, rejection filter wash water: reactant is stirred with tap water, carry out rejection filter after cooling, gained rejection filter thing washs to throwing away liquid non-pyridine bitter taste by hot purified water, filter cake is dried and obtained Inositol Nicotinate crude product;
4, decolorizing and refining: Inositol Nicotinate crude product is dissolved in to DMF, and with activated carbon decolorizing, the product drying after decolouring obtains Inositol Nicotinate finished product;
5, reclaim pyridine:
1., mother liquor that rejection filter wash water step is thrown away collects in retort, every crowd of mother liquor 900～1000L, hydro-oxidation sodium (sheet alkali), is adjusted to 9～10 by pH, air distillation is to till the fraction non-pyridine taste steaming;
2., cut proceeds to free tank, adds sheet alkali 150～175kg, opens and stirs 0.5-1 hour, more standing 1～1.5 hour, and oil reservoir is isolated and delivered to rectifying post, the above-mentioned steps that water layer is joined to lower batch of mother liquor is used in 1.;
3., slightly heating up in a steamer in the oil reservoir suction rectifying tank of gained, air distillation, reflux and control 200-300L/hr, separate and be controlled at 30-40L/hr, when rising to 110～112 ℃, tower top temperature starts to collect positive component, positive component check pyridine moisture content≤0.40%, can be used pyridinium crosslink chlorination reaction step.
Embodiment recited above is described the preferred embodiment for the present invention; not the spirit and scope of the present invention are limited; do not departing under the prerequisite of design philosophy of the present invention; various distortion and improvement that in this area, common engineering technical personnel make technical scheme of the present invention, all should belong to protection scope of the present invention.
Claims (1)
1. an Inositol Nicotinate production technique, is characterized in that, according to following step, carries out:
1) chlorination reaction: moisture content is no more than to 0.5% pyridine 100kg, add in dry 1000L enamel reactor, then add phosphorus oxychloride 107kg, after stirring well, under cooling conditions, add gradually nicotinic acid 150kg, add post-heating and be warming up to 65-75 ℃, insulation reaction 0.8-1.2 hour;
2) esterification: slowly add inositol 35kg under cooling conditions, add inositol post-heating and be warming up to 80-90 ℃, react 1 hour;
3) rejection filter wash water: reactant is stirred with tap water, carry out rejection filter after cooling, gained rejection filter thing washs to throwing away liquid non-pyridine bitter taste by hot purified water, filter cake is dried and obtained Inositol Nicotinate crude product;
4) decolorizing and refining: Inositol Nicotinate crude product is dissolved in to dimethyl formamide, and with activated carbon decolorizing, the product drying after decolouring obtains Inositol Nicotinate finished product;
5) reclaim pyridine:
1., mother liquor that rejection filter wash water step is thrown away collects in retort, every crowd of mother liquor 900～1000L, adds sodium hydroxide, and pH is adjusted to 9～10, air distillation is to till the fraction non-pyridine taste steaming;
2., cut proceeds to free tank, adds sheet alkali 150～175kg, opens and stirs 0.5-1 hour, more standing 1～1.5 hour, and oil reservoir is separated and delivered to rectifying post, the above-mentioned steps that water layer is joined to lower batch of mother liquor is used in 1.;
3., slightly heating up in a steamer in the oil reservoir suction rectifying tank of gained, air distillation, reflux and control 200-300L/hr, separate and be controlled at 30-40L/hr, when rising to 110～112 ℃, tower top temperature starts to collect positive component, positive component check pyridine moisture≤0.40%, can be used pyridinium crosslink chlorination reaction step.
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| CN201210079112.1A CN102627601B (en) | 2012-03-23 | 2012-03-23 | Production technology of inositol nicotinate |
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| CN102627601B true CN102627601B (en) | 2014-02-12 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104799302A (en) * | 2014-01-25 | 2015-07-29 | 天津中瑞药业股份有限公司 | Inositol nicotinate nutrition fortification capsule preparation metho |
| CN105153025A (en) * | 2015-09-23 | 2015-12-16 | 潍坊盛瑜药业有限公司 | Inositol nicotinate polymorph A and preparing method thereof |
| CN107879973A (en) * | 2017-11-09 | 2018-04-06 | 华中药业股份有限公司 | A kind of process for purification of mannityl nicotinate |
| CN109438335A (en) * | 2018-12-22 | 2019-03-08 | 华中药业股份有限公司 | A kind of refining methd of Inositol Nicotinate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0431197A1 (en) * | 1989-06-28 | 1991-06-12 | MITSUI TOATSU CHEMICALS, Inc. | Myoinositol derivative and method of production thereof, and phosphorylating agent and its use |
| CN1546676A (en) * | 2003-11-28 | 2004-11-17 | 华南理工大学 | Preparation method of inositol nicotinate by enzyme method |
| CN102249994A (en) * | 2011-05-10 | 2011-11-23 | 浙江爱迪亚营养科技开发有限公司 | Preparation method of nicotinic acid |
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2012
- 2012-03-23 CN CN201210079112.1A patent/CN102627601B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0431197A1 (en) * | 1989-06-28 | 1991-06-12 | MITSUI TOATSU CHEMICALS, Inc. | Myoinositol derivative and method of production thereof, and phosphorylating agent and its use |
| CN1546676A (en) * | 2003-11-28 | 2004-11-17 | 华南理工大学 | Preparation method of inositol nicotinate by enzyme method |
| CN102249994A (en) * | 2011-05-10 | 2011-11-23 | 浙江爱迪亚营养科技开发有限公司 | Preparation method of nicotinic acid |
Non-Patent Citations (4)
| Title |
|---|
| "有机介质中脂肪酶催化肌醇烟酸酯的合成";罗志刚 等;《食品与生物技术学报》;20060131;第25卷(第1期);第45-49页 * |
| "烟酸肌醇酯的合成";梁峰 等;《烟酸肌醇酯的合成》;20010630;第30卷(第3期);第19-20页 * |
| 梁峰 等."烟酸肌醇酯的合成".《烟酸肌醇酯的合成》.2001,第30卷(第3期),第19-20页. |
| 罗志刚 等."有机介质中脂肪酶催化肌醇烟酸酯的合成".《食品与生物技术学报》.2006,第25卷(第1期),第45-49页. |
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Address after: 300000, Tianjin, Wuqing Chengguan Road, east side of the ring road Patentee after: Medicine company limited company of Tianjin China and Sweden Address before: 300000, Tianjin, Wuqing Chengguan Road, east side of the ring road Patentee before: Tianjin Zhongrui Pharmaceutical Co., Ltd. |