CN109232409A - A kind of technique of niacinamide usp concentrated acid crystallization production niacin - Google Patents
A kind of technique of niacinamide usp concentrated acid crystallization production niacin Download PDFInfo
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- CN109232409A CN109232409A CN201811241965.4A CN201811241965A CN109232409A CN 109232409 A CN109232409 A CN 109232409A CN 201811241965 A CN201811241965 A CN 201811241965A CN 109232409 A CN109232409 A CN 109232409A
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- niacin
- reaction kettle
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D213/78—Carbon atoms having three bonds to hetero atoms, with at the most one bond to halogen, e.g. ester or nitrile radicals
- C07D213/79—Acids; Esters
- C07D213/80—Acids; Esters in position 3
Abstract
The present invention provides a kind of technique of niacinamide usp concentrated acid crystallization production niacin, is related to niacin production preparation field, comprising the following steps: niacin amine aqueous solution and a phegma, secondary returning flow liquid are put into reaction kettle, in T1At a temperature of carry out heating stirring, while aqueous slkali reflux is added dropwise, stops stirring after 80-100min, T is cooled to the speed of 5 DEG C/min2；After 2-3h, the mixture in reaction kettle is depressurized and is filtered, be separated by solid-liquid separation, it is a phegma that liquid portion, which is back in reaction kettle, and solid portion is collected, and after washing 2-3 times, stirring is dried to obtain crystal crude product；After crystal crude product and dehydrated alcohol heating stirring solution, cooling recrystallization, after 4-5h, filtration washing, liquid portion are back in reaction kettle as secondary returning flow liquid again, collect solid, drying is stirred, until moisture less than 2.0%, obtains niacin finished product, the present invention effectively improves the purity of product niacin, reduces production cost.
Description
Technical field
The present invention relates to niacin to produce preparation field, and in particular to a kind of technique of niacinamide usp concentrated acid crystallization production niacin.
Background technique
Niacinamide usp and niacin are B family vitamin substance, are necessary chemical substances in organism, and niacinamide usp and niacin are equal
For white crystalline powder, make mainly as food additives, feed addictive, cosmetic additive agent in daily life, but
It is that niacinamide usp than niacin is more soluble in water, it is not easy to maintain, therefore with the continuous development of China's economic level, for the need of niacin
The amount of asking sharply increases.
Currently, predominantly staying in the synthesis technologies such as nitric acid oxidation method, ammonia oxidation for the preparation of niacin, all have
To product niacin purity it is low, consumption of raw materials is big the problems such as.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides the techniques that a kind of niacinamide usp concentrated acid crystallizes production niacin, effectively
The purity of product niacin is improved, production cost is reduced.
(2) technical solution
In order to achieve the above object, the present invention is achieved by the following technical programs:
A kind of technique of niacinamide usp concentrated acid crystallization production niacin, comprising the following steps:
(1) niacin amine aqueous solution and a phegma, secondary returning flow liquid are put into reaction kettle, in T1At a temperature of heat up
Stirring, while aqueous slkali reflux is added dropwise, stop stirring after 80-100min, T is cooled to the speed of 5 DEG C/min2；
(2) after 2-3h, the mixture in reaction kettle is depressurized and is filtered, be separated by solid-liquid separation, liquid portion is back to reaction kettle
In be a phegma, solid portion is collected, washing 2-3 time after, stir be dried to obtain crystal crude product；
(3) by after crystal crude product and dehydrated alcohol heating stirring solution, cooling recrystallization, after 4-5h, filtration washing again,
Liquid portion is back in reaction kettle as secondary returning flow liquid, collection solid, stirring drying, until moisture less than 2.0%, obtains cigarette
Sour finished product.
Preferably, T described in step (1)1Temperature is 80-90 DEG C.
Preferably, the T2Temperature is 15-18 DEG C.
Preferably, aqueous slkali described in step (1) is the sodium hydroxide solution of 4mol/L.
Preferably, the mass ratio of aqueous slkali additional amount described in step (1) and the niacin amine aqueous solution additional amount is 1:18-
22。
Preferably, stirring drying described in step (2) and step (3), mixing speed 50-60r/min, drying be
Cold air drying.
(3) beneficial effect
The present invention provides the techniques that a kind of niacinamide usp concentrated acid crystallizes production niacin, have the advantages that
Firstly, mixing it with the ethyl alcohol in a phegma and secondary returning flow liquid by the way that aqueous slkali is added, in niacinamide usp
While forming alkaline environment in solution, using alcohol reflux, help niacinamide usp that can decomposite stable niacin.
Secondly, making full use of raw material during niacinamide usp prepares niacin, stock utilization is effectively improved, is reduced
Production cost.
Finally, carrying out secondary recrystallization using dehydrated alcohol, product purity is improved, and stir at low speed cold air drying, prevented
Only there is the phenomenon that crystallizing and drying is long placed in agglomeration.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is the present invention one
Divide embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making
Every other embodiment obtained, shall fall within the protection scope of the present invention under the premise of creative work.
Embodiment 1:
A kind of technique of niacinamide usp concentrated acid crystallization production niacin, comprising the following steps:
(4) niacin amine aqueous solution and a phegma, secondary returning flow liquid are put into reaction kettle, are risen at a temperature of 80 DEG C
Temperature stirring, while the sodium hydroxide solution of 4mol/L is added dropwise while flowing back, aqueous slkali additional amount and the niacin amine aqueous solution are added
The mass ratio of amount is 1:18, stops stirring after 100min, is cooled to 18 DEG C with the speed of 5 DEG C/min；
(5) after 2h, the mixture in reaction kettle is depressurized and is filtered, be separated by solid-liquid separation, liquid portion is back in reaction kettle
For a phegma, solid portion is collected, after washing 3 times, it is thick to obtain crystallization for cold air drying under the mixing speed of 50r/min
Product；
(6) by after crystal crude product and dehydrated alcohol heating stirring solution, cooling recrystallization, after 4h, filtration washing again, liquid
Body portion is back in reaction kettle as secondary returning flow liquid, collects solid, the cold air drying under the mixing speed of 60r/min, until
Moisture obtains niacin finished product less than 2.0%.
Embodiment 2:
A kind of technique of niacinamide usp concentrated acid crystallization production niacin, comprising the following steps:
(1) niacin amine aqueous solution and a phegma, secondary returning flow liquid are put into reaction kettle, are risen at a temperature of 90 DEG C
Temperature stirring, while the sodium hydroxide solution of 4mol/L is added dropwise while flowing back, aqueous slkali additional amount and the niacin amine aqueous solution are added
The mass ratio of amount is 1:22, stops stirring after 80min, is cooled to 15 DEG C with the speed of 5 DEG C/min；
(2) after 3h, the mixture in reaction kettle is depressurized and is filtered, be separated by solid-liquid separation, liquid portion is back in reaction kettle
For a phegma, solid portion is collected, after washing 2 times, it is thick to obtain crystallization for cold air drying under the mixing speed of 60r/min
Product；
(3) by after crystal crude product and dehydrated alcohol heating stirring solution, cooling recrystallization, after 5h, filtration washing again, liquid
Body portion is back in reaction kettle as secondary returning flow liquid, collects solid, the cold air drying under the mixing speed of 50r/min, until
Moisture obtains niacin finished product less than 2.0%.
Embodiment 3:
A kind of technique of niacinamide usp concentrated acid crystallization production niacin, comprising the following steps:
(1) niacin amine aqueous solution and a phegma, secondary returning flow liquid are put into reaction kettle, are risen at a temperature of 85 DEG C
Temperature stirring, while the sodium hydroxide solution of 4mol/L is added dropwise while flowing back, aqueous slkali additional amount and the niacin amine aqueous solution are added
The mass ratio of amount is 1:20, stops stirring after 90min, is cooled to 16 DEG C with the speed of 5 DEG C/min；
(2) after 2.5h, the mixture in reaction kettle is depressurized and is filtered, be separated by solid-liquid separation, liquid portion is back to reaction kettle
In be a phegma, solid portion is collected, washing 3 times after, cold air drying is crystallized under the mixing speed of 55r/min
Crude product；
(7) by after crystal crude product and dehydrated alcohol heating stirring solution, cooling recrystallization, after 4.5h, filtration washing again,
Liquid portion is back in reaction kettle as secondary returning flow liquid, collects solid, the cold air drying under the mixing speed of 55r/min, directly
To moisture less than 2.0%, niacin finished product is obtained.
Embodiment 4:
A kind of technique of niacinamide usp concentrated acid crystallization production niacin, comprising the following steps:
(1) niacin amine aqueous solution and a phegma, secondary returning flow liquid are put into reaction kettle, are risen at a temperature of 88 DEG C
Temperature stirring, while the sodium hydroxide solution of 4mol/L is added dropwise while flowing back, aqueous slkali additional amount and the niacin amine aqueous solution are added
The mass ratio of amount is 1:21, stops stirring after 85min, is cooled to 16 DEG C with the speed of 5 DEG C/min；
(2) after 2.7h, the mixture in reaction kettle is depressurized and is filtered, be separated by solid-liquid separation, liquid portion is back to reaction kettle
In be a phegma, solid portion is collected, washing 2 times after, cold air drying is crystallized under the mixing speed of 53r/min
Crude product；
(3) by after crystal crude product and dehydrated alcohol heating stirring solution, cooling recrystallization, after 4.2h, filtration washing again,
Liquid portion is back in reaction kettle as secondary returning flow liquid, collects solid, the cold air drying under the mixing speed of 57r/min, directly
To moisture less than 2.0%, niacin finished product is obtained.
Embodiment 5:
A kind of technique of niacinamide usp concentrated acid crystallization production niacin, comprising the following steps:
(1) niacin amine aqueous solution and a phegma, secondary returning flow liquid are put into reaction kettle, are risen at a temperature of 82 DEG C
Temperature stirring, while the sodium hydroxide solution of 4mol/L is added dropwise while flowing back, aqueous slkali additional amount and the niacin amine aqueous solution are added
The mass ratio of amount is 1:21, stops stirring after 95min, is cooled to 16 DEG C with the speed of 5 DEG C/min；
(2) after 2h, the mixture in reaction kettle is depressurized and is filtered, be separated by solid-liquid separation, liquid portion is back in reaction kettle
For a phegma, solid portion is collected, after washing 2 times, it is thick to obtain crystallization for cold air drying under the mixing speed of 51r/min
Product；
(4) by after crystal crude product and dehydrated alcohol heating stirring solution, cooling recrystallization, after 4.6h, filtration washing again,
Liquid portion is back in reaction kettle as secondary returning flow liquid, collects solid, the cold air drying under the mixing speed of 53r/min, directly
To moisture less than 2.0%, niacin finished product is obtained.
Beneficial effect in order to further illustrate the present invention, the niacin system for selecting 1-54 of the embodiment of the present invention to be prepared
Product test its grain size and purity, and result are recorded in following table.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.In the absence of more restrictions, including the element that sentence "including a ..." limits, it is not excluded that
There is also other identical elements in the process, method, article or apparatus that includes the element.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations, although with reference to the foregoing embodiments
Invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features；And these modification or
Replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (6)
1. a kind of technique of niacinamide usp concentrated acid crystallization production niacin, which comprises the following steps:
(1) niacin amine aqueous solution and a phegma, secondary returning flow liquid are put into reaction kettle, in T1At a temperature of carry out heating stirring,
Aqueous slkali reflux is added dropwise simultaneously, stops stirring after 80-100min, T is cooled to the speed of 5 DEG C/min2；
(2) after 2-3h, the mixture in reaction kettle is depressurized and is filtered, be separated by solid-liquid separation, liquid portion is back in reaction kettle is
Phegma, solid portion is collected, and after washing 2-3 times, stirring is dried to obtain crystal crude product；
(3) by after crystal crude product and dehydrated alcohol heating stirring solution, cooling recrystallization, after 4-5h, filtration washing again, liquid
Be partly refluxed in reaction kettle as secondary returning flow liquid, collect solid, stir drying, until moisture less than 2.0%, obtain niacin at
Product.
2. the technique of niacinamide usp concentrated acid crystallization production niacin as described in claim 1, which is characterized in that T described in step (1)1
Temperature is 80-90 DEG C.
3. the technique of niacinamide usp concentrated acid crystallization production niacin as described in claim 1, which is characterized in that the T2Temperature is
15-18℃。
4. the technique of niacinamide usp concentrated acid crystallization production niacin as described in claim 1, which is characterized in that described in step (1)
Aqueous slkali is the sodium hydroxide solution of 4mol/L.
5. the technique of niacinamide usp concentrated acid crystallization production niacin as described in claim 1, which is characterized in that described in step (1)
The mass ratio of aqueous slkali additional amount and the niacin amine aqueous solution additional amount is 1:18-22.
6. the technique of niacinamide usp concentrated acid crystallization production niacin as described in claim 1, which is characterized in that step (2) and step
(3) the stirring drying described in, mixing speed 50-60r/min, dry is cold air drying.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811241965.4A CN109232409A (en) | 2018-10-24 | 2018-10-24 | A kind of technique of niacinamide usp concentrated acid crystallization production niacin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811241965.4A CN109232409A (en) | 2018-10-24 | 2018-10-24 | A kind of technique of niacinamide usp concentrated acid crystallization production niacin |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101597258A (en) * | 2009-04-29 | 2009-12-09 | 南通醋酸化工股份有限公司 | The technology of 3-cyanopyridine synthesizing niacinamide and co-producing niacin by hydrolyzing |
| CN104557685A (en) * | 2014-12-18 | 2015-04-29 | 天津汉德威药业有限公司 | Method for producing nicotinic acid by using nicotinamide mother solution |
| CN107382844A (en) * | 2017-08-28 | 2017-11-24 | 天津科技大学 | A kind of method that nicotinic acid is produced using niacinamide usp as raw material |
-
2018
- 2018-10-24 CN CN201811241965.4A patent/CN109232409A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101597258A (en) * | 2009-04-29 | 2009-12-09 | 南通醋酸化工股份有限公司 | The technology of 3-cyanopyridine synthesizing niacinamide and co-producing niacin by hydrolyzing |
| CN104557685A (en) * | 2014-12-18 | 2015-04-29 | 天津汉德威药业有限公司 | Method for producing nicotinic acid by using nicotinamide mother solution |
| CN107382844A (en) * | 2017-08-28 | 2017-11-24 | 天津科技大学 | A kind of method that nicotinic acid is produced using niacinamide usp as raw material |
Non-Patent Citations (2)
| Title |
|---|
| 何树华等: "《基础化学实验》", 31 May 2017, 西南交通大学出版社 * |
| 陈少萍等: "《口腔临床药物手册》", 31 December 2005, 华南理工大学出版 * |
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Application publication date: 20190118 |