CN105646339A - Method for preparing nicotinic acid by low-temperature reaction crystallization - Google Patents
Method for preparing nicotinic acid by low-temperature reaction crystallization Download PDFInfo
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- CN105646339A CN105646339A CN201511009211.2A CN201511009211A CN105646339A CN 105646339 A CN105646339 A CN 105646339A CN 201511009211 A CN201511009211 A CN 201511009211A CN 105646339 A CN105646339 A CN 105646339A
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- nicotinic acid
- hydrochloric acid
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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
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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
- C07D213/803—Processes of preparation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/13—Crystalline forms, e.g. polymorphs
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a method for preparing nicotinic acid by low-temperature reaction crystallization. Existing nicotinic acid preparation processes are mostly carried out at high temperature; equipment corrosion is severe; reaction steps are too many; equipment investment cost is high; granularity of a product obtained is low; purity is low; and content of impurities is high. The method of the invention comprises the following steps: preparing a sodium nicotinate solution and hydrochloric acid, adding the sodium nicotinate solution and hydrochloric acid into a crystallizer at the mol ratio of 1: (1-1.5), and stirring and reacting at 20-35 DEG C; ending a reaction when pH value is 1-4, growing crystals, carrying out vacuum filtration on a reaction liquid, and drying so as to obtain the product. By low-temperature reaction, problems of low product purity, low granularity and easy corrosion of equipment existing in a technology of firstly carrying out an acidification reaction at high temperature and then cooling for crystallization are overcome. The method has advantages as follows: granularity of the product is high; purity is high; energy consumption is low; and equipment corrosion is little.
Description
Technical field
The present invention relates to a kind of nicotinic acid acquisition methods, be specifically related to a kind of method that low-temp reaction crystallization obtains nicotinic acid.
Background technology
Nicotinic acid (NicotincAcid), formal name used at school Pyridinecarboxylic acid, also referred to as vitamin B3 or vitamin PP, it is one of 13 kinds of vitamin of needed by human, nicotiamide it is converted in human body, participate in HypercholesterolemicRats, the oxidizing process of Tissue respiration and saccharide anaerobic decomposition process, can as important medicine intermediate. Nicotinic acid is also widely used for food and field of fodder, uses mainly as feed supplement. Additionally, nicotinic acid can be additionally used in the raw material of line antitubercular agents such as isoniazid, teldane and .gamma.-pyridinecarboxylic acid fat, it is possible to as corrosion inhibitor, electroplating additive, photosensitive resin stabilizer and non-ferro metals floatation medicament etc.
Nicotinic acid production method includes potassium permanganate oxidation method, nitric acid oxidation method, ammonia oxidation and electrochemical oxidation process etc. Wherein nitric acid oxidation method is a kind of method that current industrial production nicotinic acid is the most frequently used, published patent CN102295599A is as follows about the preparation method of nicotinic acid: 3-picoline generates 3-picoline sulfate with sulfuric acid reaction, then it is blended in 200 DEG C of reactions with nitric acid and generates nicotinic acid sulfate, liquefied ammonia neutralisation of sulphuric acid, filtration, drying obtain nicotinic acid. Patent CN1141288A 3-picoline adds sulphuric acid and reacts (normal pressure, < 150 DEG C) in a kettle., the methvl-pyridinium sulfate obtained heats to 140-330 DEG C, dropping 30%-100% nitric acid, generation nicotinic acid sulfate moves to another reactor basic species (ammonia, NaOH etc.) and is neutralized, obtain white depositions, filter, dry obtain nicotinic acid.
The patent of report disclosed above belongs to nitric acid oxidation method and prepares nicotinic acid technique, and it all needs the acid of high concentration at high temperature to react. The method has the disadvantage in that
1, at high temperature reacting, equipment corrosion is serious;
2, reactions steps is too much, and equipment investment cost is big;
3, obtaining product granularity little, purity is low, and impurity content is high;
4, after filtering, solid phase water content is high, and follow-up energy consumption for drying is big;
5, owing to product granularity is little, it is necessary to pelletize can be only achieved index, cost of investment is added.
Summary of the invention
It is an object of the invention to provide a kind of method that low-temp reaction crystallization obtains nicotinic acid, reduce reactions steps, make equipment corrosion problem improve.
The technical solution adopted in the present invention is:
Low-temp reaction crystallization obtains the method for nicotinic acid, it is characterised in that:
Comprise the following steps:
Step one: preparation mass fraction is the naotin solution of 25%-30% and mass fraction is the hydrochloric acid of 10-30%;
Step 2: first naotin solution is joined in crystallizer, after hydrochloric acid is dropped in crystallizer, the mol ratio adding naotin and hydrochloric acid is 1:(1-1.5), stirring reaction at 20 DEG C of-35 DEG C of temperature;
When pH value is 1-4, reaction terminates, and reactant liquor vacuum is filtered, dries, obtain product after growing the grain.
In step 2, hydrochloric acid time for adding is 3-6h.
In step 2, speed of agitator is 200-800rmp.
In step 2, rearing crystal time is 1-5h.
The invention have the advantages that
1, the present invention adopts naotin solution dropping hydrochloric acid one-step method under low temperature to prepare nicotinic acid, reactions steps is greatly shortened, solving the corrosion-prone problem of traditional handicraft high-temperature reaction equipment, new technology reacts at low temperatures, and low acid and low temperature environment greatly reduce the corrosion to equipment;
2, take One-step production nicotinic acid, greatly reduce the investment of consersion unit and cost;
3, the nicotinic acid granularity produced is big, crystal formation good, purity is high;
4, by adjusting hydrochloric acid rate of addition, endpoint pH, speed of agitator and rearing crystal time, improve the granularity of product, reduce the water content of filter cake, significantly reduce the energy consumption of dry run;
5, product can meet and requires index, reduces the investment of traditional handicraft Granulation Equipments.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention will be described in detail.
The low-temp reaction crystallization that the present invention relates to obtains the method for nicotinic acid, specifically includes following steps:
Step one: preparation mass fraction is the naotin solution of 25%-30% and mass fraction is the hydrochloric acid of 10-30%;
Step 2: first naotin solution is joined in crystallizer, after hydrochloric acid is dropped in crystallizer, the mol ratio adding naotin and hydrochloric acid is 1:(1-1.5), stirring reaction;
When pH value is 1-4, reaction terminates, and reactant liquor vacuum is filtered, dries, obtain product after growing the grain.
In step 2:
Hydrochloric acid time for adding is 3-6h.
Reaction temperature in crystallizer is 20 DEG C-35 DEG C.
Speed of agitator is 200-800rmp.
Rearing crystal time is 1-5h.
Embodiment 1:
Step one: preparation mass fraction be 25% naotin solution and mass fraction be the hydrochloric acid of 30%;
Step 2: first naotin solution is joined in crystallizer, after hydrochloric acid is dropped in crystallizer, the mol ratio adding naotin and hydrochloric acid is 1:1, stirring reaction;
When pH value is 4, reaction terminates, and reactant liquor vacuum is filtered, dries, obtain product after growing the grain.
In step 2:
Hydrochloric acid time for adding is 3h.
Reaction temperature in crystallizer is 35 DEG C.
Speed of agitator is 200rmp.
Rearing crystal time is 5h.
The product granularity obtained is at 80-180 ��m, and product yield reaches more than 90%.
Embodiment 2:
Step one: preparation mass fraction be 28% naotin solution and mass fraction be the hydrochloric acid of 20%;
Step 2: first naotin solution is joined in crystallizer, after hydrochloric acid is dropped in crystallizer, the mol ratio adding naotin and hydrochloric acid is 1:1.2, stirring reaction;
When pH value is 2.6, reaction terminates, and reactant liquor vacuum is filtered, dries, obtain product after growing the grain.
In step 2:
Hydrochloric acid time for adding is 4.5h.
Reaction temperature in crystallizer is 28 DEG C.
Speed of agitator is 500rmp.
Rearing crystal time is 3h.
The product granularity obtained is at 80-180 ��m, and product yield reaches more than 90%.
Embodiment 3:
Step one: preparation mass fraction be 30% naotin solution and mass fraction be the hydrochloric acid of 10;
Step 2: first naotin solution is joined in crystallizer, after hydrochloric acid is dropped in crystallizer, the mol ratio adding naotin and hydrochloric acid is 1:1.5, stirring reaction;
When pH value is 1, reaction terminates, and reactant liquor vacuum is filtered, dries, obtain product after growing the grain.
In step 2:
Hydrochloric acid time for adding is 6h.
Reaction temperature in crystallizer is 20 DEG C.
Speed of agitator is 800rmp.
Rearing crystal time is 1h.
The product granularity obtained is at 80-180 ��m, and product yield reaches more than 90%.
Present disclosure is not limited to cited by embodiment, and the conversion of any equivalence that technical solution of the present invention is taked by those of ordinary skill in the art by reading description of the present invention, the claim being the present invention is contained.
Claims (4)
1. the method that low-temp reaction crystallization obtains nicotinic acid, it is characterised in that:
Comprise the following steps:
Step one: preparation mass fraction is the naotin solution of 25%-30% and mass fraction is the hydrochloric acid of 10-30%;
Step 2: first naotin solution is joined in crystallizer, after hydrochloric acid is dropped in crystallizer, the mol ratio adding naotin and hydrochloric acid is 1:(1-1.5), stirring reaction at 20 DEG C of-35 DEG C of temperature;
When pH value is 1-4, reaction terminates, and reactant liquor vacuum is filtered, dries, obtain product after growing the grain.
2. the method that low-temp reaction crystallization according to claim 1 obtains nicotinic acid, it is characterised in that:
In step 2, hydrochloric acid time for adding is 3-6h.
3. the method that low-temp reaction crystallization according to claim 1 obtains nicotinic acid, it is characterised in that:
In step 2, speed of agitator is 200-800rmp.
4. the method that low-temp reaction crystallization according to claim 1 obtains nicotinic acid, it is characterised in that:
In step 2, rearing crystal time is 1-5h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511009211.2A CN105646339A (en) | 2015-12-30 | 2015-12-30 | Method for preparing nicotinic acid by low-temperature reaction crystallization |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511009211.2A CN105646339A (en) | 2015-12-30 | 2015-12-30 | Method for preparing nicotinic acid by low-temperature reaction crystallization |
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| CN105646339A true CN105646339A (en) | 2016-06-08 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109232406A (en) * | 2018-09-20 | 2019-01-18 | 安徽瑞邦生物科技有限公司 | A method of niacin is produced by raw material of niacinamide usp |
| CN114957109A (en) * | 2022-05-12 | 2022-08-30 | 山东泓达生物科技有限公司 | Method for preparing agglomerated large-particle-size high-fluidity nicotinic acid crystal |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
-
2015
- 2015-12-30 CN CN201511009211.2A patent/CN105646339A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109232406A (en) * | 2018-09-20 | 2019-01-18 | 安徽瑞邦生物科技有限公司 | A method of niacin is produced by raw material of niacinamide usp |
| CN114957109A (en) * | 2022-05-12 | 2022-08-30 | 山东泓达生物科技有限公司 | Method for preparing agglomerated large-particle-size high-fluidity nicotinic acid crystal |
| CN114957109B (en) * | 2022-05-12 | 2024-03-08 | 山东泓达生物科技有限公司 | Method for preparing agglomerated large-granularity high-fluidity nicotinic acid crystals |
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Application publication date: 20160608 |
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