CN1141288A - Process for preparing nicotinic acid - Google Patents
Process for preparing nicotinic acid Download PDFInfo
- Publication number
- CN1141288A CN1141288A CN 96104748 CN96104748A CN1141288A CN 1141288 A CN1141288 A CN 1141288A CN 96104748 CN96104748 CN 96104748 CN 96104748 A CN96104748 A CN 96104748A CN 1141288 A CN1141288 A CN 1141288A
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- Prior art keywords
- nicotinic acid
- picoline
- vitriol
- acid
- reaction
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- Pyridine Compounds (AREA)
Abstract
In the nicotinic acid prodn. 3-methyl pyridine and sulfuric acid is used to produce methyl pyridine sulfate, and then to react with nitric acid as oxidizing agent to produce niacin sulfate. Finally, alkali solution is used to neutralize the niacin sulfate, and nicotinic acid is obtained. This technology is simple and raw material recovery can be as high as 90%.
Description
Nicotinic acid claims vitamin B5 or nicotinic acid again.Chemical name: 3-pyridine carboxylic acid.The nicotinic acid of chemosynthesis manufacturing is applied to medicine, the food and feed additive industry.
The processing method that the synthetic nicotinic acid of number of chemical was arranged in the past.Its pros and cons are respectively arranged.
1. 2-methyl-5-ethylpyridine (MEP) oxidation style:
At first MEP is oxidized to the intermediate dinicotinic acid, decarboxylation prepares nicotinic acid then, is about to 6.4% MEP and about 33% salpeter solution and feeds titanium system reactor, and at 330 ℃, 290atm reacted about 5 minutes down.Obtain nicotinic acid nitrate after the reactant cooling, after neutralizing, making with extra care, make nicotinic acid.Technology total recovery 84～90% (, as follows) in the raw material happy per-cent that rubs.
The synthetic nicotinic acid product yield of this method is higher, but complex process, reaction conditions is very harsh, and safety production condition requires also very high, and raw material MEP source is limited.
2. 3-picoline oxidation proceses of ammonia
3-picoline and air, ammonia, water are mixed in proportion and pass through V
2O
5～Al
2O
3Beds, at 360 ℃ of following catalysis synthetic intermediate 3-cyanopyridines, hydrolysis obtains nicotinic acid under alkaline condition then, and this technology total recovery is 72～84% (crude products).
It is low to adopt these method processing condition to require, technology maturation, but the final product yield is lower.
3. quinoline nitration mixture oxidation style
Sulfuric acid and quinoline is warm altogether, drip nitric acid oxidation then, catalyzer adopts V
2O
5, M
0O
2Deng, its processing condition are quinoline: sulfuric acid: 220～230 ℃ of nitric acid=1: 1.4: 15 temperature of reaction, reaction solution product yield 77～79%.
This method process recovery ratio is low, and by product is more, and particularly the formation of by product Yi Yansuan etc. is difficult to separate with nicotinic acid.
The purpose of this invention is to provide the method for preparing nicotinic acid that a kind of technology is simple, product yield is high
Nicotinic acid manufacturing process of the present invention is to add sulfuric acid with the 3-picoline to make it to generate picoline vitriol, be that oxygenant and picoline vitriol carry out oxidizing reaction then with nitric acid, make nicotinic acid vitriol, and then with alkaline solution nicotinic acid vitriol is neutralized and to make nicotinic acid, again the nicotinic acid that makes is made with extra care, isolate the inorganic salt mixt that is contained, finally can obtain pharmaceutical grade finished product nicotinic acid.
Its technical process is:
Its concrete process for making is:
3-picoline and sulfuric acid are blended in normal pressure with 1: 0.5～10 ratio (mol ratio) in reactor, react under＜150 ℃ the temperature.Obtain picoline vitriol; Then picoline vitriol is heated to 140～330 ℃ of scopes in reactor, is added dropwise to 30%～100% nitric acid, the nitric acid amount of adding is 2～50 times (weight ratios) of picoline vitriol.Reaction product is a nicotinic acid vitriol; Nicotinic acid vitriol is moved to usefulness alkaline substance (NaOH) in another reactor, ammoniacal liquor etc.) be neutralized to till its pH value 3.1～3.5.Neutralization back gained white depositions is filtered, and promptly gets nicotinic acid after the oven dry.Can reach more than 90% with this manufactured nicotinic acid main raw material 3-picoline yield.
Illustrate that embodiment is as follows:
580 liter 96% the vitriol oil is added in the 1# salt-forming reaction still, under whipped state, add 760kg 3-picoline gradually, temperature of reaction≤45 ℃, pressure is normal pressure, time≤4 hour, reaction finishes post-heating and is warming up to 90 ℃, material is moved to the 2# still continue heating, stir, be warming up to 185 ℃～195 ℃, feed 2500 liters in 68%～70% nitric acid gradually, add sour speed must control reaction temperature at 195 ℃ ± 5 ℃, time is about 25～30 hours, and reactant gases (NOx) is discharged and absorbed with alkaline solution.Reactant nicotinic acid vitriol is cooled to 60 ℃, adds the sodium hydroxide solution neutralization of 40% content again, controlled temperature≤70 ℃, stop to add alkaline solution when reaching PH=3.4, it is stable to continue to be stirred to pH value, is cooled to 40 ℃ of centrifugations, promptly get rough nicotinic acid 1152Kg, nicotinic acid content 70.1%.Rough nicotinic acid decolours through conventional method, treating processes such as recrystallization get final product refining nicotinic acid 737Kg, purity 99.2%.
It is simple to make nicotinic acid technology with technology of the present invention, the product yield height.
Claims (4)
1, a kind of nicotinic acid manufacturing process, it is characterized in that adding sulfuric acid with the 3-picoline makes it to generate picoline vitriol, be that oxygenant and picoline vitriol carry out oxidizing reaction with nitric acid then, make nicotinic acid vitriol, and then with alkaline solution nicotinic acid vitriol is neutralized and to make nicotinic acid.
2, according to the said nicotinic acid manufacturing process of claim 1, it is characterized in that 3-picoline and sulfuric acid generate the process of picoline vitriol, 3-picoline and vitriolic ratio are 1: 0.5～10, temperature of reaction is＜150 ℃.
3,, it is characterized in that the ratio with nitric acid oxidation picoline vitriol nitric acid and picoline vitriol is that 2～50 (weight) temperature of reaction is 140～300 ℃ according to claim 1,2 said nicotinic acid manufacturing process.
4,, it is characterized in that making solution PH with nicotinic acid vitriol in the alkaline substance is 3.1～3.5 according to the technology of claim 1,2,3 said manufacturing nicotinic acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 96104748 CN1141288A (en) | 1996-04-26 | 1996-04-26 | Process for preparing nicotinic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 96104748 CN1141288A (en) | 1996-04-26 | 1996-04-26 | Process for preparing nicotinic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1141288A true CN1141288A (en) | 1997-01-29 |
Family
ID=5118501
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 96104748 Pending CN1141288A (en) | 1996-04-26 | 1996-04-26 | Process for preparing nicotinic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1141288A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101985434A (en) * | 2010-11-12 | 2011-03-16 | 安徽泰格生物技术股份有限公司 | Method for preparing nicotinic acid |
| CN102295599A (en) * | 2011-06-09 | 2011-12-28 | 许万根 | Production method and granulation method for nicotinic acid |
| CN112812058A (en) * | 2021-01-19 | 2021-05-18 | 绵阳市崴尼达医药科技有限责任公司 | Method for recovering organic matters in nicotinic acid production wastewater |
| CN115108975A (en) * | 2022-07-07 | 2022-09-27 | 山东泓瑞医药科技股份公司 | Preparation method of nicotinic acid |
-
1996
- 1996-04-26 CN CN 96104748 patent/CN1141288A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101985434A (en) * | 2010-11-12 | 2011-03-16 | 安徽泰格生物技术股份有限公司 | Method for preparing nicotinic acid |
| CN102295599A (en) * | 2011-06-09 | 2011-12-28 | 许万根 | Production method and granulation method for nicotinic acid |
| CN112812058A (en) * | 2021-01-19 | 2021-05-18 | 绵阳市崴尼达医药科技有限责任公司 | Method for recovering organic matters in nicotinic acid production wastewater |
| CN115108975A (en) * | 2022-07-07 | 2022-09-27 | 山东泓瑞医药科技股份公司 | Preparation method of nicotinic acid |
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| C06 | Publication | ||
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |