CN115418381A - Purification method of ammonium nicotinate reaction liquid - Google Patents

Purification method of ammonium nicotinate reaction liquid Download PDF

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CN115418381A
CN115418381A CN202211108372.7A CN202211108372A CN115418381A CN 115418381 A CN115418381 A CN 115418381A CN 202211108372 A CN202211108372 A CN 202211108372A CN 115418381 A CN115418381 A CN 115418381A
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reaction
ammonium nicotinate
nicotinic acid
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liquid
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周媛
胡昊
韩道平
杨红军
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Anhui Redpont Biotechnology Co ltd
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    • C12P17/00—Preparation of heterocyclic carbon compounds with only O, N, S, Se or Te as ring hetero atoms
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    • 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
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    • 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
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    • C12Y305/00—Hydrolases acting on carbon-nitrogen bonds, other than peptide bonds (3.5)
    • C12Y305/01—Hydrolases acting on carbon-nitrogen bonds, other than peptide bonds (3.5) in linear amides (3.5.1)
    • C12Y305/01019—Nicotinamidase (3.5.1.19)

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Abstract

The invention discloses a method for purifying ammonium nicotinate reaction liquid, which belongs to the technical field of biochemical engineering and comprises the following steps: step 1: fermenting the nicotinamide enzyme; and 2, step: carrying out biocatalytic reaction; and step 3: filtering the ammonium nicotinate catalytic liquid by a ceramic membrane; and 4, step 4: spray drying the ammonium nicotinate clear liquid. According to the invention, the nicotinamide-containing wastewater in the 3-cyanogen workshop is catalyzed by amidase to generate ammonium nicotinate, and then the ammonium nicotinate is subjected to spray drying by utilizing the principle that the ammonium nicotinate can be decomposed into nicotinic acid and ammonia at the temperature of more than 150 ℃, so that nicotinic acid crystalline powder is further prepared, high energy consumption and high pollution caused by the traditional chemical method are avoided, and the method has the advantages of low cost, small pollution, mild reaction and suitability for industrial production.

Description

Purification method of ammonium nicotinate reaction liquid
Technical Field
The invention relates to the technical field of biochemical engineering, in particular to a method for purifying ammonium nicotinate reaction liquid.
Background
Nicotinic acid belongs to vitamin B3, is also called nicotinic acid and scabies resisting factor, has good thermal stability and can be sublimated, and the nicotinic acid is purified by a sublimation method in industry. Nicotinic acid is white or yellowish crystal in appearance, is soluble in water, mainly exists in animal internal organs and muscle tissues, and also exists in fruits and egg yolks in trace amount, is one of 13 vitamins essential to human bodies, and belongs to the vitamin B group. At present, nicotinic acid is mainly used as a feed additive, can improve the utilization rate of feed protein, and can improve the milk yield of dairy cows and the meat yield and quality of fish, chicken, duck, cattle, sheep and other livestock. Nicotinic acid is a widely used medical intermediate, and can be used as a raw material to synthesize various medicines, such as nicotemide, inositol nicotinate and the like. In addition, nicotinic acid also plays an irreplaceable role in the fields of luminescent materials, dyes, electroplating industries and the like.
The existing synthesis method of nicotinic acid comprises the following steps:
nitric acid oxidation method:
the method comprises the steps of introducing a mixture of aqueous nitric acid solution and MEP into a titanium tubular reactor by using nitric acid as an oxidant, reacting for 8 hours at 330 ℃ and 29MPa, and then separating and refining to obtain a pure nicotinic acid product.
(II) air oxidation:
the air oxidation method directly oxidizes 3-methylpyridine to synthesize nicotinic acid by using air as an oxidant, and has attracted attention in recent years due to the characteristics of high efficiency and low cost. The method firstly carries out oxidation reaction in alkyl pyridine with catalyst by introducing air, and then is improved to synthesize nicotinic acid by taking 3-methylpyridine as a raw material and carrying out gas-solid phase catalytic oxidation reaction for 3 hours at 350-400 ℃ in a fixed bed reactor. The catalyst can be used for a long time, and 3-methylpyridine is directly oxidized by air to obtain nicotinic acid.
(III) electrolytic oxidation method:
the electrolytic oxidation method has the advantages of mild conditions, low price of oxidant, low toxicity and pollution, low production cost and the like, so the electrolytic oxidation method is widely applied to production. Similar to the chemical oxidation method, the electrochemical oxidation of alkyl pyridine compounds is usually used to synthesize nicotinic acid, but the method has the disadvantage of low electrolysis efficiency, mainly because the selective permeability of the isolating membrane used in the electrolytic bath is poor, so that the industrial production of the method is greatly limited.
(IV) Ammonia Oxidation method:
the raw material of the ammoxidation method is the byproduct 3-methylpyridine with the highest proportion produced in the pyridine base production process, has low price, wide source and relatively mild reaction conditions, can be carried out under the conditions of normal pressure or low pressure, has safe and reliable production, has higher conversion per pass and better selectivity in the prior art, obtains a product with high purity, can realize continuous synthesis, is suitable for large-scale industrial production, and becomes one of the most widely applied methods for preparing nicotinic acid in the industry at present.
Disclosure of Invention
The invention aims to provide a method for purifying an ammonium nicotinate reaction liquid, which is characterized in that waste water containing nicotinamide in a 3-cyanogen workshop is catalyzed by amidase to generate ammonium nicotinate, and then the ammonium nicotinate is subjected to a spray drying method, so that the principle that the ammonium nicotinate can be decomposed into nicotinic acid and ammonia at the temperature of more than 150 ℃ is utilized, and nicotinic acid crystalline powder is further prepared, high energy consumption and high pollution caused by the traditional chemical method are avoided, and the method has the advantages of low cost, small pollution, mild reaction and suitability for industrial production, and is used for solving the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for purifying ammonium nicotinate reaction liquid comprises the following steps;
step 1: fermenting the nicotinamide enzyme;
step 2: carrying out biocatalytic reaction;
and step 3: filtering the ammonium nicotinate catalytic liquid by a ceramic membrane;
and 4, step 4: spray drying the ammonium nicotinate clear liquid.
Further, the fermenting nicotinamide enzyme comprises the following steps:
activating strains: streaking the strain on an LB (Langmuir-Blodgett) plate, and culturing for 16h in a constant-temperature incubator at 37 ℃;
first-stage seed liquid culture: selecting a single clone, transferring the single clone into a 40ml LB shake flask, and carrying out shake culture at 37 ℃ and 220rpm for 8 hours;
secondary seed liquid culture: transferring 40mL of the first-stage seed solution into a shake flask of 150mL of a second-stage culture medium, and carrying out shake culture at 37 ℃ and 220rpm for 8 hours;
fermentation and tank culture: transferring 150mL of the secondary seed solution into a 5L fermentation tank filled with a fermentation culture medium, performing fermentation culture at 35 ℃ to about OD60060, cooling to 18 ℃, and adding an inducer for induction.
Detecting OD of the fermentation liquor: sampling every 6-8h to detect the OD value of the fermentation liquor and the enzyme activity, and putting the fermentation liquor into a tank until the enzyme activity is not increased.
Further, the biocatalytic reaction comprises the steps of:
putting 25L of nicotinamide wastewater and bacterial sludge successfully fermented together into a 50L reaction kettle, setting the reaction temperature to be 37 +/-2 ℃, the pH to be 7.0 +/-0.2 and the rotation speed to be 120rpm, adding 6.6U/ml of enzyme for reaction, and obtaining ammonium nicotinate catalytic solution after the reaction is finished.
Further, the ceramic membrane filtration of the ammonium nicotinate catalytic solution comprises the following steps:
removing thalli and insoluble solid impurities from catalytic liquid containing bacteria and ammonia obtained by catalytic reaction through a microfiltration membrane, removing organic matters and bacteria from clear liquid obtained by microfiltration through an ultrafiltration membrane, and obtaining clear liquid obtained by ultrafiltration through a nanofiltration membrane;
the ammonium nicotinate clear liquid obtained by ceramic membrane filtration can be directly spray-dried.
Further, the spray drying of the ammonium nicotinate clear liquid comprises the following steps:
determining the inlet temperature of spray drying: the temperature of an inlet and an outlet of a spray dryer adopted has certain coupling performance, and different inlet temperatures of 200-250 ℃ are set to influence the purity of the nicotinic acid according to the characteristics of the pretreated conversion solution and the melting point of the nicotinic acid;
determining the vacuum drying temperature of the nicotinic acid finished product: the residual moisture and ammonia of the nicotinic acid finished product after spray drying are more, the finished product is further purified and dried, different drying temperatures are set to be 65-115 ℃, and the optimal vacuum drying temperature is determined.
Further, three batches of repeated experiments are carried out on the ammonium nicotinate nanofiltration clear liquid, and the three batches are subjected to spray drying at 230 ℃ and high-temperature drying for 8 hours.
Compared with the prior art, the invention has the beneficial effects that:
the invention adopts a biological synthesis method, which uses underground pool waste water containing nicotinamide in a workshop as a raw material, converts the nicotinamide into nicotinic acid under the action of amidase, obtains clear liquid of ammonium nicotinate catalytic liquid by membrane filtration of the nicotinic acid, obtains finished nicotinic acid products by a spray drying technology of the clear liquid, further purifies and dries the finished nicotinic acid products to obtain pure nicotinic acid products, has incomparable superiority of a chemical method, has the advantages of high efficiency, good selectivity, mild reaction conditions, small environmental pollution, low cost, high optical purity of the products and the like, and conforms to the development direction of green chemistry.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
1. Fermentation technology of nicotinamide enzyme
Activating strains: the strain is streaked on an LB (Kana: 50 ug/mL) plate, and cultured in a constant temperature incubator at 37 ℃ for about 16h;
first-stage seed liquid culture: selecting a single clone, transferring the single clone into a 40mL LB (Kana: 50 ug/mL) shake flask, and carrying out shake culture at 37 ℃ and 220rpm for about 8h;
secondary seed liquid culture: transferring the first-stage seed solution (40 mL) into a 150mL second-stage culture medium (Kana: 50 ug/mL) shake flask, and performing shake culture at 37 ℃ and 220rpm for about 8h;
fermentation and tank-feeding culture: transferring the secondary seed solution (150 mL) into 5L fermentation tank containing fermentation culture medium (2L base material volume), fermenting at 35 deg.C until OD60060 is about, cooling to 18 deg.C, and adding inducer for inducing.
And (3) detecting the OD of the fermentation liquor: sampling every 6-8h to detect the OD value of the fermentation liquor and the enzyme activity, and canning until the enzyme activity is not increased.
The enzyme activity determination method comprises the following steps:
loading: and (4) diluting the centrifuged reaction liquid supernatant by 6 times and loading.
And (3) calculating: and (3) calculating and obtaining: crude enzyme liquid enzyme activity (U/mL) = CxV xX/123.1/T/V
c-nicotinic acid concentration by liquid chromatography,. Mu.g/mL;
v-reaction volume, here 800. Mu.L reaction solution + 200. Mu.L sulfuric acid test solution;
x-dilution multiple (6) before reaction sample injection;
t-reaction time, 10min;
v-volume of crude enzyme solution added, 10. Mu.L
123.1-nicotinic acid molecular weight, g/moL.
Enzyme activity of fermentation liquor (U/mL) = crude enzyme activity of enzyme liquor x dilution times of fermentation liquor (N).
Statistics of fermentation enzyme activity
Figure BDA0003842332860000051
2. Biocatalytic reactions
Putting 25L of nicotinamide wastewater and bacterial sludge successfully fermented together into a 50L reaction kettle, setting the reaction temperature at 37 +/-2 ℃, the pH at 7.0 +/-0.2 and the rotation speed at 120rpm, adding 6.6U/ml of enzyme for reaction, and obtaining ammonium nicotinate catalytic solution after the reaction is finished
3. Ceramic membrane filtration of ammonium nicotinate catalytic liquid
Removing thalli and insoluble solid impurities from catalytic liquid containing bacteria and ammonia obtained by catalytic reaction through a microfiltration membrane, removing organic matters, bacteria and other macromolecular substances from clear liquid obtained by microfiltration through an ultrafiltration membrane, effectively intercepting target components from the clear liquid obtained by ultrafiltration through a nanofiltration membrane, and removing a solvent to achieve the purpose of concentration;
the clear liquid of ammonium nicotinate obtained by ceramic membrane filtration can be directly spray-dried.
4. Spray drying of ammonium nicotinate clear liquid
Determining the inlet temperature of spray drying: the temperature of an inlet and an outlet of a spray dryer adopted in the experiment has certain coupling property, and the influence of different inlet temperatures (200 ℃) on the purity of the nicotinic acid is set according to the characteristics of the pretreated conversion solution and the melting point of the nicotinic acid;
determining the vacuum drying temperature of the finished nicotinic acid product: the nicotinic acid finished product has more residual moisture and ammonia after spray drying, the finished product is further purified and dried, the volatilization of the moisture and the ammonia can be accelerated, different drying temperatures (65 ℃) are set, and the optimal vacuum drying temperature is determined.
Example 2
The same parts of this embodiment as those of embodiment 1 are not described in detail, and the differences from embodiment 1 are as follows:
determining the inlet temperature of spray drying: the temperature of an inlet and an outlet of a spray dryer adopted in the experiment has certain coupling property, and the influence of different inlet temperatures (210 ℃) on the purity of the nicotinic acid is set according to the characteristics of the pretreated conversion solution and the melting point of the nicotinic acid;
determining the vacuum drying temperature of the nicotinic acid finished product: the nicotinic acid finished product has more residual moisture and ammonia after spray drying, the finished product is further purified and dried, the volatilization of the moisture and the ammonia can be accelerated, different drying temperatures (75 ℃) are set, and the optimal vacuum drying temperature is determined.
Example 3
The same parts of this embodiment as those of embodiment 1 are not described in detail, but are different from embodiment 1;
determining the spray drying inlet temperature: the inlet and outlet temperatures of the spray dryer adopted in the experiment have certain coupling property, and the influence of different inlet temperatures (220 ℃) on the purity of the nicotinic acid is set according to the characteristics of the pretreatment conversion solution and the melting point of the nicotinic acid;
determining the vacuum drying temperature of the nicotinic acid finished product: the nicotinic acid finished product has more residual moisture and ammonia after spray drying, the finished product is further purified and dried, the volatilization of the moisture and the ammonia can be accelerated, different drying temperatures (85 ℃) are set, and the optimal vacuum drying temperature is determined.
Example 4
The same parts of this embodiment as those of embodiment 1 are not described in detail, and the differences from embodiment 1 are that;
determining the spray drying inlet temperature: the temperature of an inlet and an outlet of a spray dryer adopted in the experiment has certain coupling property, and the influence of different inlet temperatures (230 ℃) on the purity of the nicotinic acid is set according to the characteristics of the pretreated conversion solution and the melting point of the nicotinic acid;
determining the vacuum drying temperature of the finished nicotinic acid product: the nicotinic acid finished product has more residual moisture and ammonia after spray drying, the finished product is further purified and dried, the volatilization of the moisture and the ammonia can be accelerated, different drying temperatures (95 ℃) are set, and the optimal vacuum drying temperature is determined.
Example 5
The same parts of this embodiment as those of embodiment 1 are not described in detail, but are different from embodiment 1;
determining the inlet temperature of spray drying: the temperature of the inlet and the outlet of the spray dryer adopted in the experiment has certain coupling property, and the influence of different inlet temperatures (240 ℃) on the purity of the nicotinic acid is set according to the characteristics of the pretreated conversion solution and the melting point of the nicotinic acid;
determining the vacuum drying temperature of the finished nicotinic acid product: the nicotinic acid finished product has more residual moisture and ammonia after spray drying, the finished product is further purified and dried, the volatilization of the moisture and the ammonia can be accelerated, different drying temperatures (105 ℃) are set, and the optimal vacuum drying temperature is determined.
Example 6
The same parts of this embodiment as those of embodiment 1 are not described in detail, but are different from embodiment 1;
determining the inlet temperature of spray drying: the inlet and outlet temperatures of the spray dryer adopted in the experiment have certain coupling property, and the influence of different inlet temperatures (250 ℃) on the purity of the nicotinic acid is set according to the characteristics of the pretreatment conversion solution and the melting point of the nicotinic acid;
determining the vacuum drying temperature of the finished nicotinic acid product: the nicotinic acid finished product has more residual moisture and ammonia after spray drying, the finished product is further purified and dried, the volatilization of the moisture and the ammonia can be accelerated, different drying temperatures (115 ℃) are set, and the optimal vacuum drying temperature is determined.
In the above 6 examples, the relationship between spray drying temperature and niacin purity is as follows:
Figure BDA0003842332860000071
relationship between drying temperature and purity of nicotinic acid finished product
Figure BDA0003842332860000072
Figure BDA0003842332860000081
Nicotinic acid spray drying and purification stability experiment
Three batches of repeated experiments are carried out on the ammonium nicotinate nanofiltration clear liquid, the following experimental data are obtained by spray drying at 230 ℃ and high-temperature drying for 8 hours, and it can be found that the pure nicotinic acid content is stabilized at about 99.40%, the ammonium root residue is 0.3%, the drying weight loss and other impurities reach the national standard, and the specific experimental parameters are as follows:
data on nicotinic acid finished product
Figure BDA0003842332860000082
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.

Claims (6)

1. A method for purifying ammonium nicotinate reaction liquid is characterized by comprising the following steps;
step 1: fermenting the nicotinamide enzyme;
step 2: carrying out biocatalytic reaction;
and 3, step 3: filtering by using a ceramic membrane for the ammonium nicotinate catalytic liquid;
and 4, step 4: spray drying the ammonium nicotinate clear liquid.
2. The method of claim 1, wherein said fermenting nicotinamidase comprises the steps of:
activating strains: streaking the strain on an LB (Langmuir-Blodgett) plate, and culturing for 16h in a constant-temperature incubator at 37 ℃;
primary seed liquid culture: selecting a single clone, transferring the single clone into a 40ml LB shake flask, and carrying out shake culture at 37 ℃ and 220rpm for 8 hours;
secondary seed liquid culture: transferring 40mL of the first-stage seed solution into a shake flask of 150mL of a second-stage culture medium, and carrying out shake culture at 37 ℃ and 220rpm for 8 hours;
fermentation and tank-feeding culture: transferring 150mL of the secondary seed solution into a 5L fermentation tank filled with a fermentation culture medium, performing fermentation culture at 35 ℃ to about OD60060, cooling to 18 ℃, and adding an inducer for induction.
Detecting OD of the fermentation liquor: sampling every 6-8h to detect the OD value of the fermentation liquor and the enzyme activity, and canning until the enzyme activity is not increased.
3. The method of claim 1, wherein the biocatalytic reaction comprises the steps of:
putting 25L of nicotinamide wastewater and bacterial sludge successfully fermented together into a 50L reaction kettle, setting the reaction temperature to be 37 +/-2 ℃, the pH to be 7.0 +/-0.2 and the rotation speed to be 120rpm, adding 6.6U/ml of enzyme for reaction, and obtaining ammonium nicotinate catalytic solution after the reaction is finished.
4. The method of claim 1, wherein the ammonium nicotinate catalyst ceramic membrane filtration comprises the steps of:
removing thalli and insoluble solid impurities from a catalytic liquid containing bacteria and ammonia obtained by catalytic reaction through a microfiltration membrane, removing organic matters and bacteria from a clear liquid obtained by microfiltration through an ultrafiltration membrane, and performing ultrafiltration to obtain a clear liquid through a nanofiltration membrane;
the clear liquid of ammonium nicotinate obtained by ceramic membrane filtration can be directly spray-dried.
5. The method of claim 1, wherein said spray drying of said ammonium nicotinate supernatant comprises the steps of:
determining the inlet temperature of spray drying: the temperature of an inlet and an outlet of a spray dryer adopted has certain coupling performance, and different inlet temperatures of 200-250 ℃ are set to influence the purity of the nicotinic acid according to the characteristics of the pretreated conversion solution and the melting point of the nicotinic acid;
determining the vacuum drying temperature of the finished nicotinic acid product: the residual moisture and ammonia of the nicotinic acid finished product after spray drying are more, the finished product is further purified and dried, different drying temperatures are set to be 65-115 ℃, and the optimal vacuum drying temperature is determined.
6. The method as claimed in claim 1, characterized in that the ammonium nicotinate reaction solution purification method is characterized in that three batches of repeated experiments are carried out on the ammonium nicotinate nanofiltration clear solution, spray drying is carried out at 230 ℃, and drying is carried out at high temperature for 8h.
CN202211108372.7A 2022-09-13 2022-09-13 Purification method of ammonium nicotinate reaction liquid Pending CN115418381A (en)

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