CN104557685A - Method for producing nicotinic acid by using nicotinamide mother solution - Google Patents
Method for producing nicotinic acid by using nicotinamide mother solution Download PDFInfo
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- CN104557685A CN104557685A CN201410797378.9A CN201410797378A CN104557685A CN 104557685 A CN104557685 A CN 104557685A CN 201410797378 A CN201410797378 A CN 201410797378A CN 104557685 A CN104557685 A CN 104557685A
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- niacinamide
- nicotinic 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
- C07D213/803—Processes of preparation
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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 invention provides a method for producing nicotinic acid by using a nicotinamide mother solution, which comprises the following steps: hydrolysis reaction: adding the nicotinamide mother solution and caustic soda flakes into a four-neck flask, measuring a certain amount of purified water by using a measuring cylinder, and adding into the four-neck flask, wherein the mass ratio of the nicotinamide, sodium hydroxide and purified water in the four-neck flask is 1:(0.39-0.80):(2-4); starting stirring and heating, starting timing when the temperature rises to 90-115 DEG C, and reacting for 2.5-3.5 hours while controlling the temperature at 90-115 DEG C, wherein a right amount of purified water is supplemented in the hydrolysis reaction process; after the hydrolysis reaction finishes, obtaining sodium 3-pyridyl-formate; and decolorizing, crystallizing, separating, drying and the like to obtain the nicotinic acid finished product. The method provides a powerful technical support for mother solution treatment in the nicotinamide technique, maximizes the benefits of the nicotinamide and nicotinic acid product, minimizes the discharge, and solves the problem of reuse of the nicotinamide mother solution, thereby enhancing the nicotinamide quality.
Description
Technical field
The present invention relates to the production technical field of nicotinic acid, particularly relate to a kind of method using niacinamide mother liquor to produce nicotinic acid.
Background technology
Nicotinic acid is also referred to as vitamin B3 or 3-pyridine-carboxylic acid, and niacinamide is also known as 3-pyridine-2-carboxamide, and nicotinic acid and niacinamide are referred to as vitamin PP, is that 13 kinds of needed by human one of are supported one's family.Nicotinic acid is converted into niacinamide in human body.Nicotinic acid and niacinamide after choline or choline chloride 60 compound for the fodder additives of livestock and poultry.Niacinamide and nicotinic acid are also widely used in foodstuff additive, for improving Nutritive value of food.The nicotinic acid of pharmaceutical grade and niacinamide are simultaneously also for the VITAMIN tablet of the mankind.
No matter adopt which kind of technique, the main production raw material of most niacinamide and nicotinic acid is nicotinonitrile.Traditionally, nicotinic acid is generated by nicotinonitrile mainly through hydrolysis method.The processing route producing niacinamide then has a lot, but no matter any technique, all can produce mother liquor, and recycled.
Existing niacinamide mother liquor through recycled is some take turns after, due to too much impure, can not having continued to apply mechanically, for avoiding loss of material, having needed to reclaim the niacinamide in mother liquor.Recovery method is that after finite concentration, carry out centrifugal drying worry, in whizzer pocket, gained material is the niacinamide of recovery by distillation and concentration in mother liquor suction reactor.Even disposing mother liquor, the niacinamide quality that it obtains is also very poor, and in recovery, have relatively large quantity loss.In this course, the impurity in mother liquor is also concentrated, and after centrifugal drying is considered, the overwhelming majority is mixed in the niacinamide of recovery, can not be removed, and make the impure amount of the niacinamide reclaimed very high, quality is very poor; Owing to yet containing a lot of niacinamide in the water-soluble very high mother liquor discarded after rejection filter of niacinamide, cause a certain amount of loss of material.
Summary of the invention
The problem to be solved in the present invention is to provide a kind of method using niacinamide mother liquor to produce nicotinic acid, this does not reclaim the niacinamide in niacinamide mother liquor, and directly the niacinamide in mother liquor and other various pyridines materials are all converted into nicotinic acid, effectively prevent the loss of material, the quality of its nicotinic acid produced can reach the quality of the nicotinic acid using nicotinonitrile direct production.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of method using niacinamide mother liquor to produce nicotinic acid, comprises following preparation process,
1), hydrolysis reaction
First niacinamide mother liquor, sheet alkali are dropped in four-hole bottle, then drop in four-hole bottle by the purified water of graduated cylinder measured amounts, in four-hole bottle, the mass ratio of niacinamide, sodium hydroxide and purified water is 1:0.39 ~ 0.80:2 ~ 4; Start and stir and start heating, when temperature rises to 90 ~ 115 DEG C, start timing, temperature controls at 90 ~ 115 DEG C, reaction times is 2.5 ~ 3.5 hours, in hydrolysis reaction, supplements purified water in right amount, ensure that the volume of liquid in four-hole bottle is unchanged, after hydrolysis reaction, obtain 3-pyridine-carboxylic acid sodium;
The chemical equation of hydrolysis reaction is as follows:
2), decolour
By step 1) temperature of solution that obtains after reaction is down to 70 ~ 80 DEG C, and add gac, start timing insulation 0.5 ~ 1.5 hour, temperature controls at 70 ~ 80 DEG C, and after decolouring, gac is removed by suction filtration;
3), crystallization
By step 2) in filtrate after suction filtration be reentered in four-hole bottle, drip with hydrochloric acid, limit drips the pH that solution in four-hole bottle is measured on hydrochloric acid limit, until its pH is repetition measurement after 3.5 ~ 4.0,5 ~ 15 minutes, its pH is still 3.5 ~ 4.0, stops dripping hydrochloric acid;
The chemical equation of crystallisation step is as follows:
4), be separated
By step 3) in solution after crystallization carry out suction filtration washing, after suction filtration, obtain wet product;
5), dry
By step 4) wet product that obtains puts into drying baker dries, and obtains nicotinic acid finished product after oven dry.
Preferably, step 1) in, the reaction times is 3 hours.
Preferably, step 2) in, by step 1) temperature of solution that obtains after reaction is down to 80 DEG C, and add gac, start timing and be incubated 1 hour.
Preferably, step 3) in, limit drips the pH that solution in four-hole bottle is measured on hydrochloric acid limit, until its pH is repetition measurement after 3.5 ~ 4.0,10 minutes.
The advantage that the present invention has and positively effect are:
1), the present invention is that in niacinamide technique, mother liquid disposal provides strong technical support, and by niacinamide and nicotinic acid product benefit, discharge minimizes, and solves niacinamide mother liquid recycle problem, thus improves the quality of niacinamide.
2), niacinamide mother liquor is through hydrolysis reaction with after dripping acid crystal reaction, reaction product only has nicotinic acid, ammonia and sodium-chlor, ammonia is reclaimed can be made ammoniacal liquor by recovery tower, it is a kind of important agricultural fertilizer, also no matter may be used for boiler house boiler desulfuration dedusting, and sodium-chlor can be removed by rinsing major part, be the sodium-chlor in product or the sodium-chlor in waste liquid, concentration is all very low, can not impact quality product and environment.
3), hydrolysis after through filter progress, issuable impurity in hydrolysis reaction is removed, has increased substantially the quality of product, nicotinic acid wet product content >=99.0%, nicotinic acid dry product content >=99.2%, residue on ignition≤0.5%.
4), steam only for intensification and the insulation of hydrolysis reaction, the duration of service of every day is limited, and crystallization uses circulating water cooling, does not need cool brine lower the temperature, energy consumption in whole technical process is significantly reduced, minimizing energy dissipation.
5), hydrolysis method reaction carry out in airtight retort, by the size control temperature of steam, production technique is simplified, and the security of whole production technique increases substantially.
Accompanying drawing explanation
Fig. 1 is the process flow sheet using niacinamide mother liquor to produce the method for nicotinic acid in the present invention;
Embodiment
Embodiment one
Use niacinamide mother liquor to produce a method for nicotinic acid, comprise following preparation process,
1), hydrolysis reaction
Take niacinamide mother liquor 450g, wherein in niacinamide mother liquor, the mass concentration of niacinamide is 28.0%, niacinamide mother liquor, sheet alkali are dropped in four-hole bottle, drop in four-hole bottle by the purified water of graduated cylinder measured amounts, in four-hole bottle, the mass ratio of niacinamide, sodium hydroxide and purified water is 1:0.80:4 again; Start and stir and start heating, when temperature rises to 108 DEG C, start timing, temperature controls at 108 ~ 115 DEG C, and the reaction times is 3 hours, in hydrolysis reaction, appropriate supplementary purified water, ensures that the volume of liquid in four-hole bottle is unchanged, obtains 3-pyridine-carboxylic acid sodium after hydrolysis reaction;
2), decolour
By step 1) temperature of solution that obtains after reaction is down to 80 DEG C, and add gac, start timing and be incubated 1 hour, temperature controls at 70 ~ 80 DEG C, and after decolouring, gac is removed by suction filtration;
3), crystallization
By step 2) in filtrate after suction filtration be reentered in four-hole bottle, drip with hydrochloric acid, limit drips the pH that solution in four-hole bottle is measured on hydrochloric acid limit, until its pH is 3.5, repetition measurement after 10 minutes, its pH is still 3.5, stops dripping hydrochloric acid, the consumption of hydrochloric acid is 275mL, and its massfraction is 36.0%;
4), be separated
By step 3) in solution after crystallization carry out suction filtration washing, after suction filtration, obtain wet product 182g;
5), dry
By step 4) wet product that obtains puts into drying baker, and dry at 105 ~ 110 DEG C, after oven dry, obtain nicotinic acid finished product 120.5g.
By the nicotinic acid finished product of preparation, sampling censorship, its test basis is << Chinese Pharmacopoeia >>2010 version first enlarged edition, the main physical and chemical index of sample: outward appearance: qualified; Uptake factor: 256; Solution colour: qualified; Muriate: qualified; Sulfide: qualified; Weight loss on drying: 0.13%; Residue on ignition: 0.02%, heavy metal: qualified; Nicotinic Acid Content 99.7%; Nicotinic acid transformation efficiency: 94.9%.
Embodiment two
Use niacinamide mother liquor to produce a method for nicotinic acid, comprise following preparation process,
1), hydrolysis reaction
Take niacinamide mother liquor 450g, wherein in niacinamide mother liquor, the mass concentration of niacinamide is 28.0%, niacinamide mother liquor, sheet alkali are dropped in four-hole bottle, pull in four-hole bottle by the purified water of graduated cylinder measured amounts again, in four-hole bottle, the mass ratio of niacinamide, sodium hydroxide and purified water is 1:0.6:4; Start and stir and start heating, when temperature rises to 105 DEG C, start timing, temperature controls at 105 ~ 112 DEG C, reaction times is 2.5 ~ 3.5 hours, in hydrolysis reaction, supplements purified water in right amount, ensure that the volume of liquid in four-hole bottle is unchanged, after hydrolysis reaction, obtain 3-pyridine-carboxylic acid sodium;
2), decolour
By step 1) temperature of solution that obtains after reaction is down to 80 DEG C, and add gac, start timing and be incubated 1 hour, temperature controls at 70 ~ 80 DEG C, and after decolouring, gac is removed by suction filtration;
3), crystallization
By step 2) in filtrate after suction filtration be reentered in four-hole bottle, drip with hydrochloric acid, limit drips the pH that solution in four-hole bottle is measured on hydrochloric acid limit, until its pH is 3.7, repetition measurement after 10 minutes, its pH is still 3.7, stops dripping hydrochloric acid, the consumption of hydrochloric acid is 205mL, and its massfraction is 36.0%;
4), be separated
By step 3) in solution after crystallization carry out suction filtration washing, after suction filtration, obtain wet product 185g;
5), dry
By step 4) wet product that obtains puts into drying baker, and dry at 105 ~ 110 DEG C, after oven dry, obtain nicotinic acid finished product 120.3g.
By the nicotinic acid finished product of preparation, sampling censorship, its test basis is << Chinese Pharmacopoeia >>2010 version first enlarged edition, the main physical and chemical index of sample: outward appearance: qualified; Uptake factor: 258; Solution colour: qualified; Muriate: qualified; Sulfide: qualified; Weight loss on drying: 0.15%; Residue on ignition: 0.01%; Heavy metal: qualified; Nicotinic Acid Content 99.8%.
Nicotinic acid transformation efficiency: 94.7%.
Embodiment three
Use niacinamide mother liquor to produce a method for nicotinic acid, comprise following preparation process,
1), hydrolysis reaction
Take niacinamide mother liquor 450g, wherein in niacinamide mother liquor, the mass concentration of niacinamide is 28.0%, niacinamide mother liquor, sheet alkali are dropped in four-hole bottle, pull in four-hole bottle by the purified water of graduated cylinder measured amounts again, in four-hole bottle, the mass ratio of niacinamide, sodium hydroxide and purified water is 1:0.40:4; Start and stir and start heating, when temperature rises to 102 DEG C, start timing, temperature controls at 102 ~ 108 DEG C, and the reaction times is 3 hours, in hydrolysis reaction, appropriate supplementary purified water, ensures that the volume of liquid in four-hole bottle is unchanged, obtains 3-pyridine-carboxylic acid sodium after hydrolysis reaction;
2), decolour
By step 1) temperature of solution that obtains after reaction is down to 80 DEG C, and add gac, start timing and be incubated 1 hour, temperature controls at 70 ~ 80 DEG C, and after decolouring, gac is removed by suction filtration;
3), crystallization
By step 2) in filtrate after suction filtration be reentered in four-hole bottle, drip with hydrochloric acid, limit drips the pH that solution in four-hole bottle is measured on hydrochloric acid limit, until its pH is 3.5, repetition measurement after 10 minutes, its pH is still 3.5, stops dripping hydrochloric acid, the consumption of hydrochloric acid is 130mL, and its massfraction is 36.0%;
4), be separated
By step 3) in solution after crystallization carry out suction filtration washing, after suction filtration, obtain wet product 180g;
5), dry
By step 4) wet product that obtains puts into drying baker dries, and dry at 105 ~ 110 DEG C, after oven dry, obtain nicotinic acid finished product 120.5g.
By the nicotinic acid finished product of preparation, sampling censorship, its test basis is << Chinese Pharmacopoeia >>2010 version first enlarged edition, the main physical and chemical index of sample: outward appearance: qualified; Uptake factor: 256; Solution colour: qualified; Muriate: qualified; Sulfide: qualified; Weight loss on drying: 0.18%; Residue on ignition: 0.02%; Heavy metal: qualified; Nicotinic Acid Content 99.6%.
Nicotinic acid transformation efficiency: 94.9%.
Embodiment four
Use niacinamide mother liquor to produce a method for nicotinic acid, comprise following preparation process,
1), hydrolysis reaction
Take niacinamide mother liquor 450g, wherein in niacinamide mother liquor, the mass concentration of niacinamide is 28.0%, niacinamide mother liquor, sheet alkali are dropped in four-hole bottle, pull in four-hole bottle by the purified water of graduated cylinder measured amounts again, in four-hole bottle, the mass ratio of niacinamide, sodium hydroxide and purified water is 1:0.40:3; Start and stir and start heating, when temperature rises to 102 DEG C, start timing, temperature controls at 102 ~ 108 DEG C, and the reaction times is 3 hours, in hydrolysis reaction, appropriate supplementary purified water, ensures that the volume of liquid in four-hole bottle is unchanged, obtains 3-pyridine-carboxylic acid sodium after hydrolysis reaction;
2), decolour
By step 1) temperature of solution that obtains after reaction is down to 80 DEG C, and add gac, start timing and be incubated 1 hour, temperature controls at 70 ~ 80 DEG C, and after decolouring, gac is removed by suction filtration;
3), crystallization
By step 2) in filtrate after suction filtration be reentered in four-hole bottle, drip with hydrochloric acid, limit drips the pH that solution in four-hole bottle is measured on hydrochloric acid limit, until its pH is 3.5, repetition measurement after 10 minutes, its pH is still 3.5, stops dripping hydrochloric acid, the consumption of hydrochloric acid is 135mL, and its massfraction is 36.0%;
4), be separated
By step 3) in solution after crystallization carry out suction filtration washing, after suction filtration, obtain wet product 185g;
5), dry
By step 4) wet product that obtains puts into drying baker dries, and dry at 105 ~ 110 DEG C, after oven dry, obtain nicotinic acid finished product 121.2g.
By the nicotinic acid finished product of preparation, sampling censorship, its test basis is << Chinese Pharmacopoeia >>2010 version first enlarged edition, the main physical and chemical index of sample: outward appearance: qualified; Uptake factor: 256; Solution colour: qualified; Muriate: qualified; Sulfide: qualified; Weight loss on drying: 0.10%; Residue on ignition: 0.02%; Heavy metal: qualified; Nicotinic Acid Content 99.7%.
Nicotinic acid transformation efficiency: 95.4%.
Embodiment five
Use niacinamide mother liquor to produce a method for nicotinic acid, comprise following preparation process,
1), hydrolysis reaction
Take niacinamide mother liquor 450g, wherein in niacinamide mother liquor, the mass concentration of niacinamide is 28.0%, niacinamide mother liquor, sheet alkali are dropped in four-hole bottle, pull in four-hole bottle by the purified water of graduated cylinder measured amounts again, in four-hole bottle, the mass ratio of niacinamide, sodium hydroxide and purified water is 1:0.40:2; Start and stir and start heating, when temperature rises to 102 DEG C, start timing, temperature controls at 102 ~ 108 DEG C, and the reaction times is 3 hours, in hydrolysis reaction, appropriate supplementary purified water, ensures that the volume of liquid in four-hole bottle is unchanged, obtains 3-pyridine-carboxylic acid sodium after hydrolysis reaction;
2), decolour
By step 1) temperature of solution that obtains after reaction is down to 80 DEG C, and add gac, start timing and be incubated 1 hour, temperature controls at 70 ~ 80 DEG C, and after decolouring, gac is removed by suction filtration;
3), crystallization
By step 2) in filtrate after suction filtration be reentered in four-hole bottle, drip with hydrochloric acid, limit drips the pH that solution in four-hole bottle is measured on hydrochloric acid limit, until its pH is 3.5, repetition measurement after 10 minutes, its pH is still 3.5, stops dripping hydrochloric acid, the consumption of hydrochloric acid is 128mL, and its massfraction is 36.0%;
4), be separated
By step 3) in solution after crystallization carry out suction filtration washing, after suction filtration, obtain wet product 178g;
5), dry
By step 4) wet product that obtains puts into drying baker dries, and dry at 105 ~ 110 DEG C, after oven dry, obtain nicotinic acid finished product 119g.
By the nicotinic acid finished product of preparation, sampling censorship, its test basis is << Chinese Pharmacopoeia >>2010 version first enlarged edition, the main physical and chemical index of sample: outward appearance: qualified; Uptake factor: 260; Solution colour: qualified; Muriate: qualified; Sulfide: qualified; Weight loss on drying: 0.15%; Residue on ignition: 0.02%; Heavy metal: qualified; Nicotinic Acid Content 99.6%.
Nicotinic acid transformation efficiency: 93.7%.
Embodiment six
Use niacinamide mother liquor to produce a method for nicotinic acid, comprise following preparation process,
1), hydrolysis reaction
Take niacinamide mother liquor 450g, wherein in niacinamide mother liquor, the mass concentration of niacinamide is 28.0%, niacinamide mother liquor, sheet alkali are dropped in four-hole bottle, pull in four-hole bottle by the purified water of graduated cylinder measured amounts again, in four-hole bottle, the mass ratio of niacinamide, sodium hydroxide and purified water is 1:0.40:3; Start and stir and start heating, when temperature rises to 100 DEG C, start timing, temperature controls at 100 ~ 103 DEG C, and the reaction times is 3 hours, in hydrolysis reaction, appropriate supplementary purified water, ensures that the volume of liquid in four-hole bottle is unchanged, obtains 3-pyridine-carboxylic acid sodium after hydrolysis reaction;
2), decolour
By step 1) temperature of solution that obtains after reaction is down to 80 DEG C, and add gac, start timing and be incubated 1 hour, temperature controls at 70 ~ 80 DEG C, and after decolouring, gac is removed by suction filtration;
3), crystallization
By step 2) in filtrate after suction filtration be reentered in four-hole bottle, drip with hydrochloric acid, limit drips the pH that solution in four-hole bottle is measured on hydrochloric acid limit, until its pH is 3.6, repetition measurement after 10 minutes, its pH is still 3.6, stops dripping hydrochloric acid, the consumption of hydrochloric acid is 133mL, and its massfraction is 36.0%;
4), be separated
By step 3) in solution after crystallization carry out suction filtration washing, after suction filtration, obtain wet product;
5), dry
By step 4) wet product that obtains puts into drying baker dries, and dry at 105 ~ 110 DEG C, after oven dry, obtain nicotinic acid finished product.
By the nicotinic acid finished product of preparation, sampling censorship, its test basis is << Chinese Pharmacopoeia >>2010 version first enlarged edition, the main physical and chemical index of sample: outward appearance: qualified; Uptake factor: 258; Solution colour: qualified; Muriate: qualified; Sulfide: qualified; Weight loss on drying: 0.16%; Residue on ignition: 0.01%; Heavy metal: qualified; Nicotinic Acid Content 99.7%.
Nicotinic acid transformation efficiency: 95.3%.
Embodiment seven
1. use niacinamide mother liquor to produce a method for nicotinic acid, it is characterized in that: comprise following preparation process,
1), hydrolysis reaction
Take niacinamide mother liquor 450g, wherein in niacinamide mother liquor, the mass concentration of niacinamide is 28.0%, niacinamide mother liquor, sheet alkali are dropped in four-hole bottle, pull in four-hole bottle by the purified water of graduated cylinder measured amounts again, in four-hole bottle, the mass ratio of niacinamide, sodium hydroxide and purified water is 1:0.40:3; Start and stir and start heating, when temperature rises to 95 DEG C, start timing, temperature controls at 90 ~ 100 DEG C, and the reaction times is 3 hours, in hydrolysis reaction, appropriate supplementary purified water, ensures that the volume of liquid in four-hole bottle is unchanged, obtains 3-pyridine-carboxylic acid sodium after hydrolysis reaction;
2), decolour
By step 1) temperature of solution that obtains after reaction is down to 80 DEG C, and add gac, start timing and be incubated 1 hour, temperature controls at 70 ~ 80 DEG C, and after decolouring, gac is removed by suction filtration;
3), crystallization
By step 2) in filtrate after suction filtration be reentered in four-hole bottle, drip with hydrochloric acid, limit drips the pH that solution in four-hole bottle is measured on hydrochloric acid limit, until its pH is 3.5, repetition measurement after 10 minutes, its pH is still 3.5, stops dripping hydrochloric acid, the consumption of hydrochloric acid is 132mL, and its massfraction is 36.0%;
4), be separated
By step 3) in solution after crystallization carry out suction filtration washing, after suction filtration, obtain wet product 178g;
5), dry
By step 4) wet product that obtains puts into drying baker dries, and dry at 105 ~ 110 DEG C, after oven dry, obtain nicotinic acid finished product 119.8.
By the nicotinic acid finished product of preparation, sampling censorship, its test basis is << Chinese Pharmacopoeia >>2010 version first enlarged edition, the main physical and chemical index of sample: outward appearance: qualified; Uptake factor: 256; Solution colour: qualified; Muriate: qualified; Sulfide: qualified; Weight loss on drying: 0.19%; Residue on ignition: 0.01%; Heavy metal: qualified; Nicotinic Acid Content 99.5%.
Nicotinic acid transformation efficiency: 94.3%.
Embodiment eight
Use niacinamide mother liquor to produce a method for nicotinic acid, comprise following preparation process,
1), hydrolysis reaction
Take niacinamide mother liquor 450g, wherein in niacinamide mother liquor, the mass concentration of niacinamide is 28.0%, niacinamide mother liquor, sheet alkali are dropped in four-hole bottle, pull in four-hole bottle by the purified water of graduated cylinder measured amounts again, in four-hole bottle, the mass ratio of niacinamide, sodium hydroxide and purified water is 1:0.40:3; Start and stir and start heating, when temperature rises to 90 DEG C, start timing, temperature controls at 90 ~ 95 DEG C, and the reaction times is 3 hours, in hydrolysis reaction, appropriate supplementary purified water, ensures that the volume of liquid in four-hole bottle is unchanged, obtains 3-pyridine-carboxylic acid sodium after hydrolysis reaction;
2), decolour
By step 1) temperature of solution that obtains after reaction is down to 80 DEG C, and add gac, start timing and be incubated 1 hour, temperature controls at 70 ~ 80 DEG C, and after decolouring, gac is removed by suction filtration;
3), crystallization
By step 2) in filtrate after suction filtration be reentered in four-hole bottle, drip with hydrochloric acid, limit drips the pH that solution in four-hole bottle is measured on hydrochloric acid limit, until its pH is repetition measurement after 3.5,10 minutes, its pH is still 3.5, stops dripping hydrochloric acid;
4), be separated
By step 3) in solution after crystallization carry out suction filtration washing, after suction filtration, obtain wet product 175g;
5), dry
By step 4) wet product that obtains puts into drying baker dries, and dry at 105 ~ 110 DEG C, after oven dry, obtain nicotinic acid finished product 119.0g.
By the nicotinic acid finished product of preparation, sampling censorship, its test basis is << Chinese Pharmacopoeia >>2010 version first enlarged edition, the main physical and chemical index of sample: outward appearance: qualified; Uptake factor: 256; Solution colour: qualified; Muriate: qualified; Sulfide: qualified; Weight loss on drying: 0.15%; Residue on ignition: 0.04%; Heavy metal: qualified; Nicotinic Acid Content 99.5%.
Nicotinic acid transformation efficiency: 93.7%.
Above embodiments of the invention have been described in detail, but described content being only preferred embodiment of the present invention, can not being considered to for limiting practical range of the present invention.All equalizations done according to the scope of the invention change and improve, and all should still belong within this patent covering scope.
Claims (4)
1. use niacinamide mother liquor to produce a method for nicotinic acid, it is characterized in that: comprise following preparation process,
1), hydrolysis reaction
First niacinamide mother liquor, sheet alkali are dropped in four-hole bottle, then drop in four-hole bottle by the purified water of graduated cylinder measured amounts, in four-hole bottle, the mass ratio of niacinamide, sodium hydroxide and purified water is 1:0.39 ~ 0.80:2 ~ 4; Start and stir and start heating, when temperature rises to 90 ~ 115 DEG C, start timing, temperature controls at 90 ~ 115 DEG C, reaction times is 2.5 ~ 3.5 hours, in hydrolysis reaction, supplements purified water in right amount, ensure that the volume of liquid in four-hole bottle is unchanged, after hydrolysis reaction, obtain 3-pyridine-carboxylic acid sodium;
2), decolour
By step 1) temperature of solution that obtains after reaction is down to 70 ~ 80 DEG C, and add gac, start timing insulation 0.5 ~ 1.5 hour, temperature controls at 70 ~ 80 DEG C, and after decolouring, gac is removed by suction filtration;
3), crystallization
By step 2) in filtrate after suction filtration be reentered in four-hole bottle, drip with hydrochloric acid, limit drips the pH that solution in four-hole bottle is measured on hydrochloric acid limit, until its pH is repetition measurement after 3.5 ~ 4.0,5 ~ 15 minutes, its pH is still 3.5 ~ 4.0, stops dripping hydrochloric acid;
4), be separated
By step 3) in solution after crystallization carry out suction filtration washing, after suction filtration, obtain wet product;
5), dry
By step 4) wet product that obtains puts into drying baker, and dry at 105 ~ 110 DEG C, after oven dry, obtain nicotinic acid finished product.
2. use niacinamide mother liquor according to claim 1 produces the method for nicotinic acid, it is characterized in that: step 1) in, the reaction times is 3 hours.
3. use niacinamide mother liquor according to claim 1 produces the method for nicotinic acid, it is characterized in that: step 2) in, by step 1) temperature of solution that obtains after reaction is down to 80 DEG C, and add gac, start timing and be incubated 1 hour.
4. use niacinamide mother liquor according to claim 1 produces the method for nicotinic acid, it is characterized in that: step 3) in, limit drips the pH that solution in four-hole bottle is measured on hydrochloric acid limit, until its pH is repetition measurement after 3.5 ~ 4.0,10 minutes.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109232409A (en) * | 2018-10-24 | 2019-01-18 | 张刘兵 | A kind of technique of niacinamide usp concentrated acid crystallization production niacin |
| CN114456106A (en) * | 2020-11-10 | 2022-05-10 | 安徽瑞邦生物科技有限公司 | Method for recovering nicotinic acid in industrial wastewater |
Citations (2)
| 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 |
| US20120022262A1 (en) * | 2007-04-20 | 2012-01-26 | Lothar Ott | Process of hydrolysis of heteroaromatic nitrils in aqueous fluids |
-
2014
- 2014-12-18 CN CN201410797378.9A patent/CN104557685A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120022262A1 (en) * | 2007-04-20 | 2012-01-26 | Lothar Ott | Process of hydrolysis of heteroaromatic nitrils in aqueous fluids |
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 王玲运: "烟酸和烟酞胺的国内外生产简况及合成路线", 《海峡药学》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109232409A (en) * | 2018-10-24 | 2019-01-18 | 张刘兵 | A kind of technique of niacinamide usp concentrated acid crystallization production niacin |
| CN114456106A (en) * | 2020-11-10 | 2022-05-10 | 安徽瑞邦生物科技有限公司 | Method for recovering nicotinic acid in industrial wastewater |
| CN114456106B (en) * | 2020-11-10 | 2024-01-16 | 安徽瑞邦生物科技有限公司 | Method for recycling nicotinic acid in industrial wastewater |
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