CN109232406A - A method of niacin is produced by raw material of niacinamide usp - Google Patents
A method of niacin is produced by raw material of niacinamide usp Download PDFInfo
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- CN109232406A CN109232406A CN201811102605.6A CN201811102605A CN109232406A CN 109232406 A CN109232406 A CN 109232406A CN 201811102605 A CN201811102605 A CN 201811102605A CN 109232406 A CN109232406 A CN 109232406A
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- niacin
- raw material
- filtrate
- hydrochloric acid
- solution
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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
-
- 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
- C07D213/803—Processes of preparation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pyridine Compounds (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The present invention discloses a kind of method for producing niacin as raw material using niacinamide usp, this method is specifically included that put into niacin amine aqueous solution in stirring container and is stirred uniformly, hydrochloric acid solution is uniformly added into niacin amine aqueous solution again and is acidified, acidization stirs heating under the revolving speed of 400~600r/min, it is uniformly heating to 50~65 DEG C, it detects the pH of reaction solution and is adjusted to 3.5~6 by continuing dropwise addition hydrochloric acid solution, stop stirring after reaction solution is at white, keep the temperature 30~40min；Again by reaction solution under room temperature 20~22h of growing the grain, then by carry out vacuum filter, washing filter cake and filtrate, filter cake is dried under 70~80 DEG C of baking ovens, is crushed, niacin is obtained；The present invention has not only saved reaction raw materials, shortens path and the time of niacin production, reduces production cost, improve production efficiency, and the niacin being prepared has the advantages that thin particle, purity is high, crystal form are good；The present invention re-uses waste liquid circulation simultaneously, reduces the discharge amount of waste liquid, protects environment, improves raw material availability.
Description
Technical field
The present invention relates to chemosynthesis technical fields, and in particular to a method of niacin is produced by raw material of niacinamide usp.
Background technique
Niacin also known as Nicotinicum Acidum are a kind of important water-soluble B vitamin, also referred to as vitamin B3 or vitamin
PP.Niacin is widely used in field of medicaments as important intermediate, such as: hexanicit, Buddhist nun can stop, niacinamide and isoniazid
The production of equal medicaments.In addition to this, niacin also has in fields such as food and feed additive, dye industry, household chemicals
Very extensive application, the synthesis of niacin is always deeply by the extensive concern of chemical industrial field.In current industrial production, niacin
It is mainly prepared by the oxidation to 3- picoline, main method is divided into liquid phase oxidation and vapour phase oxidation process.Liquid phase oxidation
During the reaction except a large amount of additive need to be added, when can also generate the by-products such as more NOx, inorganic wastes, and purify
Need to consume mass energy, high at production cost when producing on a large scale, production process all has seriously environment in waste liquid, exhaust gas
Pollution；For this purpose, the invention proposes a kind of methods for producing niacin as raw material using niacinamide usp.
Summary of the invention
In view of the above problems, the invention proposes a kind of methods for producing niacin as raw material using niacinamide usp.
In order to achieve the above purpose, the following technical solution is employed by the present invention:
A method of niacin being produced by raw material of niacinamide usp, this method mainly comprises the steps that
(1) niacin amine aqueous solution is put into stirring container and is stirred uniformly, then hydrochloric acid solution is uniformly added into niacinamide usp
It is acidified in solution, acidization stirs heating under the revolving speed of 400~600r/min, is uniformly heating to 50~65 DEG C, inspection
It surveys the pH of reaction solution and is adjusted to 3.5~6 by continuing dropwise addition hydrochloric acid solution, stop stirring, heat preservation after reaction solution is at white
30~40min；
(2) by above-mentioned reaction solution under room temperature 20~22h of growing the grain, then by carry out vacuum filter, washing filter cake and filter
Filter cake is dried under 70~80 DEG C of baking ovens, is crushed, obtains niacin by liquid.
Preferably, the concentration of hydrochloric acid solution is 0.03~0.08mol/L.
Preferably, the mass concentration of the niacin amine aqueous solution is 40~45%.
Preferably, the hydrochloric acid solution is added dropwise in filtrate in the step (2), adjusting filtrate pH is 4.5~6.5, then
The niacin amine aqueous solution of total filtrate quality 18~25% is added, is warming up to 55~65 DEG C and is stirred to react 5~10min, add niacin
Crystal seed keeps the temperature 40~45min, then is down to room temperature growing the grain 20~for 24 hours, then by it is identical in step (2) be filtered, washed, dry,
Crushing operation.
Preferably, the quality that the niacin crystal seed is added is the 0.3~0.8% of total filtrate quality.
Preferably, the filtrate pH is adjusted to 5.0.
Due to using above-mentioned technical solution, the beneficial effects of the present invention are:
(1) present invention produces niacin by niacinamide usp and has not only saved reaction raw materials, compared with the method phase of traditional mode of production niacin
Than, path and the time of niacin production are shortened, production cost is reduced, improves production efficiency, the niacin tool being prepared
Have the advantages that thin particle, purity is high, crystal form are good；
(2) waste liquid circulation that the present invention generates preparation re-uses, and not only reduces the discharge amount of waste liquid, protects ring
Border, also waste utilization improve raw material availability, and then save raw material, have accomplished Green Chemistry.
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.Based on the embodiment of the present invention, the common skill in this field
Art personnel every other embodiment obtained without creative efforts belongs to the model that the present invention protects
It encloses.
Embodiment 1:
A method of niacin being produced by raw material of niacinamide usp, this method mainly comprises the steps that
(1) the niacin amine aqueous solution that mass concentration is 42% is put into stirring container and is stirred uniformly, then general mole is dense
Degree is uniformly added into niacin amine aqueous solution for the hydrochloric acid solution of 0.05mol/L and is acidified, revolving speed of the acidization in 500r/min
Lower stirring heating, is uniformly heating to 60 DEG C, detects the pH of reaction solution and is adjusted to 4.5 by continuing dropwise addition hydrochloric acid solution, to anti-
It answers liquid at stopping stirring after white, keeps the temperature 30min；
(2) by above-mentioned reaction solution under room temperature growing the grain 21h, then by carry out vacuum filter, washing filter cake and filtrate, will
Filter cake is dried under 75 DEG C of baking ovens, is crushed, and niacin is obtained.
Wherein, hydrochloric acid solution is added dropwise in filtrate in step (2), adjusting filtrate pH is 5, adds total filtrate quality 20%
Niacin amine aqueous solution, be warming up to 60 DEG C and be stirred to react 10min, add quality be total filtrate quality 0.5% niacin crystal seed, protect
Warm 40min, then be down to room temperature growing the grain 20h, then by it is identical in step (2) be filtered, washed, dry, crushing operation.
Embodiment 2:
A method of niacin being produced by raw material of niacinamide usp, this method mainly comprises the steps that
(1) the niacin amine aqueous solution that mass concentration is 43% is put into stirring container and is stirred uniformly, then general mole is dense
Degree is uniformly added into niacin amine aqueous solution for the hydrochloric acid solution of 0.06mol/L and is acidified, revolving speed of the acidization in 400r/min
Lower stirring heating, is uniformly heating to 50 DEG C, detects the pH of reaction solution and is adjusted to 6 by continuing dropwise addition hydrochloric acid solution, wait react
Liquid keeps the temperature 40min at stopping stirring after white；
(2) by above-mentioned reaction solution under room temperature growing the grain 20h, then by carry out vacuum filter, washing filter cake and filtrate, will
Filter cake is dried under 70 DEG C of baking ovens, is crushed, and niacin is obtained.
Wherein, hydrochloric acid solution is added dropwise in filtrate in step (2), adjusting filtrate pH is 6.5, adds total filtrate quality
18% niacin amine aqueous solution is warming up to 55 DEG C and is stirred to react 5min, and it is brilliant to add the niacin that quality is total filtrate quality 0.4%
Kind, keep the temperature 43min, then be down to room temperature growing the grain 20h, then by it is identical in step (2) be filtered, washed, dry, crushing operation.
Embodiment 3:
A method of niacin being produced by raw material of niacinamide usp, this method mainly comprises the steps that
(1) the niacin amine aqueous solution that mass concentration is 44% is put into stirring container and is stirred uniformly, then general mole is dense
Degree is uniformly added into niacin amine aqueous solution for the hydrochloric acid solution of 0.03mol/L and is acidified, revolving speed of the acidization in 600r/min
Lower stirring heating, is uniformly heating to 65 DEG C, detects the pH of reaction solution and is adjusted to 3.5 by continuing dropwise addition hydrochloric acid solution, to anti-
It answers liquid at stopping stirring after white, keeps the temperature 30min；
(2) by above-mentioned reaction solution under room temperature growing the grain 22h, then by carry out vacuum filter, washing filter cake and filtrate, will
Filter cake is dried under 80 DEG C of baking ovens, is crushed, and niacin is obtained.
Wherein, hydrochloric acid solution is added dropwise in filtrate in step (2), adjusting filtrate pH is 4.5, adds total filtrate quality
25% niacin amine aqueous solution is warming up to 50 DEG C and is stirred to react 6min, and it is brilliant to add the niacin that quality is total filtrate quality 0.3%
Kind, keep the temperature 41min, then be down to room temperature growing the grain 22h, then by it is identical in step (2) be filtered, washed, dry, crushing operation.
Embodiment 4:
A method of niacin being produced by raw material of niacinamide usp, this method mainly comprises the steps that
(1) the niacin amine aqueous solution that mass concentration is 45% is put into stirring container and is stirred uniformly, then general mole is dense
Degree is uniformly added into niacin amine aqueous solution for the hydrochloric acid solution of 0.08mol/L and is acidified, revolving speed of the acidization in 400r/min
Lower stirring heating, is uniformly heating to 50 DEG C, detects the pH of reaction solution and is adjusted to 4 by continuing dropwise addition hydrochloric acid solution, wait react
Liquid keeps the temperature 35min at stopping stirring after white；
(2) by above-mentioned reaction solution under room temperature growing the grain 20h, then by carry out vacuum filter, washing filter cake and filtrate, will
Filter cake is dried under 80 DEG C of baking ovens, is crushed, and niacin is obtained.
Wherein, hydrochloric acid solution is added dropwise in filtrate in step (2), adjusting filtrate pH is 5, adds total filtrate quality 22%
Niacin amine aqueous solution, be warming up to 65 DEG C and be stirred to react 7min, add quality be total filtrate quality 0.8% niacin crystal seed, protect
Warm 44min, then be down to room temperature growing the grain for 24 hours, then by it is identical in step (2) be filtered, washed, dry, crushing operation.
Embodiment 5:
A method of niacin being produced by raw material of niacinamide usp, this method mainly comprises the steps that
(1) the niacin amine aqueous solution that mass concentration is 40% is put into stirring container and is stirred uniformly, then general mole is dense
Degree is uniformly added into niacin amine aqueous solution for the hydrochloric acid solution of 0.07mol/L and is acidified, revolving speed of the acidization in 600r/min
Lower stirring heating, is uniformly heating to 60 DEG C, detects the pH of reaction solution and is adjusted to 5 by continuing dropwise addition hydrochloric acid solution, wait react
Liquid keeps the temperature 40min at stopping stirring after white；
(2) by above-mentioned reaction solution under room temperature growing the grain 21h, then by carry out vacuum filter, washing filter cake and filtrate, will
Filter cake is dried under 75 DEG C of baking ovens, is crushed, and niacin is obtained.
Wherein, hydrochloric acid solution is added dropwise in filtrate in step (2), adjusting filtrate pH is 5.5, adds total filtrate quality
21% niacin amine aqueous solution is warming up to 55 DEG C and is stirred to react 8min, and it is brilliant to add the niacin that quality is total filtrate quality 0.7%
Kind, keep the temperature 45min, then be down to room temperature growing the grain 23h, then by it is identical in step (2) be filtered, washed, dry, crushing operation.
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 method for producing niacin as raw material using niacinamide usp, which is characterized in that this method mainly comprises the steps that
(1) niacin amine aqueous solution is put into stirring container and is stirred uniformly, then hydrochloric acid solution is uniformly added into niacin amine aqueous solution
In be acidified, acidization stirs heating under the revolving speed of 400~600r/min, is uniformly heating to 50~65 DEG C, and detection is anti-
It answers the pH of liquid and is adjusted to 3.5~6 by continuing dropwise addition hydrochloric acid solution, stop stirring after reaction solution is at white, heat preservation 30~
40min；
(2) by above-mentioned reaction solution under room temperature 20~22h of growing the grain, then by carry out vacuum filter, washing filter cake and filtrate, will
Filter cake is dried under 70~80 DEG C of baking ovens, is crushed, and niacin is obtained.
2. the method according to claim 1 for producing niacin as raw material using niacinamide usp, which is characterized in that the hydrochloric acid solution
Concentration is 0.03~0.08mol/L.
3. the method according to claim 1 for producing niacin as raw material using niacinamide usp, which is characterized in that the niacinamide usp is molten
The mass concentration of liquid is 40~45%.
4. the method according to claim 1 for producing niacin as raw material using niacinamide usp, which is characterized in that the step
(2) hydrochloric acid solution is added dropwise in filtrate, adjusting filtrate pH is 4.5~6.5, adds the cigarette of total filtrate quality 18~25%
Acid amide solution is warming up to 55~65 DEG C and is stirred to react 5~10min, adds niacin crystal seed, keeps the temperature 40~45min, then be down to room
Warm growing the grain 20~for 24 hours, then by it is identical in step (2) be filtered, washed, dry, crushing operation.
5. the method according to claim 4 for producing niacin as raw material using niacinamide usp, which is characterized in that the niacin crystal seed
The quality of addition is the 0.3~0.8% of total filtrate quality.
6. the method according to claim 4 for producing niacin as raw material using niacinamide usp, which is characterized in that the filtrate pH tune
Section is 5.0.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811102605.6A CN109232406A (en) | 2018-09-20 | 2018-09-20 | A method of niacin is produced by raw material of niacinamide usp |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811102605.6A CN109232406A (en) | 2018-09-20 | 2018-09-20 | A method of niacin is produced by raw material of niacinamide usp |
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| CN201811102605.6A Pending CN109232406A (en) | 2018-09-20 | 2018-09-20 | A method of niacin is produced by raw material of niacinamide usp |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008128744A1 (en) * | 2007-04-20 | 2008-10-30 | Lonza Ag | Method for the hydrolysis of heteroaromatic nitriles in aqueous fluids |
| CN105646339A (en) * | 2015-12-30 | 2016-06-08 | 西安航天华威化工生物工程有限公司 | Method for preparing nicotinic acid by low-temperature reaction crystallization |
| 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
- 2018-09-20 CN CN201811102605.6A patent/CN109232406A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008128744A1 (en) * | 2007-04-20 | 2008-10-30 | Lonza Ag | Method for the hydrolysis of heteroaromatic nitriles in aqueous fluids |
| CN105646339A (en) * | 2015-12-30 | 2016-06-08 | 西安航天华威化工生物工程有限公司 | Method for preparing nicotinic acid by low-temperature reaction crystallization |
| 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 |
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Application publication date: 20190118 |
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