CN118059683A - Preparation method of high-concentration ethyl caproate solution - Google Patents

Preparation method of high-concentration ethyl caproate solution Download PDF

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Publication number
CN118059683A
CN118059683A CN202410208474.9A CN202410208474A CN118059683A CN 118059683 A CN118059683 A CN 118059683A CN 202410208474 A CN202410208474 A CN 202410208474A CN 118059683 A CN118059683 A CN 118059683A
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caproic acid
fermentation liquor
acid fermentation
concentration
ethyl caproate
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Inventor
冯小进
夏威汉
刘占奇
李俊薇
董孝元
李良
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Huanghelou Wine Industry Xianning Co ltd
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Huanghelou Wine Industry Xianning Co ltd
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Abstract

The invention discloses a preparation method of a high-concentration ethyl caproate solution, which belongs to the technical field of biological fermentation and comprises the following steps: step one, concentrating the caproic acid fermentation liquor, wherein an inorganic pervaporation membrane filter is communicated between a fermentation tank with the caproic acid fermentation liquor and a temporary storage tank through a pipeline, and a vacuum machine is also communicated with the outer side of the inorganic pervaporation membrane filter, and the caproic acid fermentation liquor is concentrated by adopting an inorganic pervaporation membrane, so that the concentration of the caproic acid is more than 100.00 g/L; and step two, deodorizing the caproic acid fermentation liquor, namely conveying the caproic acid fermentation liquor concentrated in the step one into a filter through a pump body, mixing the caproic acid fermentation liquor with high-temperature Daqu, and simultaneously using active carbon in the filter to achieve the purpose of removing the odor of the caproic acid fermentation liquor.

Description

Preparation method of high-concentration ethyl caproate solution
Technical Field
The invention relates to the technical field of biological fermentation, in particular to a preparation method of a high-concentration ethyl caproate solution.
Background
Bioengineering is generally considered to be an emerging technology based on the theory and technology of biology (especially microbiology, genetics, biochemistry and cytology) and combining with modern engineering technologies such as chemical engineering, machinery, electronic computers and the like, fully utilizing the latest achievements of molecular biology, intentionally manipulating genetic materials, directionally modifying organisms or functions thereof, creating new species with ultra-distant traits in a short period, and culturing the engineering bacteria or engineering cell lines in a large scale through a proper bioreactor so as to produce a large number of useful metabolites or exert unique physiological functions thereof.
Bioengineering includes five major projects, namely genetic engineering (genetic engineering), cellular engineering, microbial engineering (fermentation engineering), enzymatic engineering (biochemical engineering) and bioreactor engineering. In these five fields, the former two functions are to use conventional bacteria (or animal and plant cell lines) as specific genetic material receptors, so that they obtain foreign genes, and become "engineering bacteria" or "engineering cell lines" which are new species capable of expressing the ultra-distant traits. The latter three functions are that the new species with huge potential value creates good growth and propagation conditions, and large-scale culture is carried out to fully exert the inherent potential thereof, thereby providing huge economic and social benefits for people.
At present, many researches on caproic acid bacteria and related culture methods report that the concentration of caproic acid in the traditional caproic acid fermentation liquid is lower and generally not more than 15g/L, because caproic acid is a byproduct of fermentation of caproic acid bacteria, the caproic acid can reach an equilibrium in the fermentation process of caproic acid bacteria, the growth of caproic acid bacteria can be inhibited when the concentration of caproic acid is higher, the generated caproic acid is gradually reduced, and odor substances such as butyric acid can be generated in the process of culturing caproic acid bacteria, so that the traditional caproic acid fermentation liquid is difficult to produce high-concentration and odorless caproic acid ethyl fermentation liquid by means of esterification.
Disclosure of Invention
The invention aims to provide a preparation method of a high-concentration ethyl caproate solution, which aims to solve the problems in the background technology.
In order to achieve the above purpose, the present invention provides the following technical solutions: a preparation method of a high-concentration ethyl caproate solution comprises the following steps:
Step one, concentrating the caproic acid fermentation liquor, wherein an inorganic pervaporation membrane filter is communicated between a fermentation tank with the caproic acid fermentation liquor and a temporary storage tank through a pipeline, and a vacuum machine is also communicated with the outer side of the inorganic pervaporation membrane filter, and the caproic acid fermentation liquor is concentrated by adopting an inorganic pervaporation membrane, so that the concentration of the caproic acid is more than 100.00 g/L;
Step two, deodorizing the caproic acid fermentation liquor, namely conveying the caproic acid fermentation liquor concentrated in the step one into a filter through a pump body, mixing the caproic acid fermentation liquor with high-temperature Daqu before the step two, and simultaneously using active carbon in the filter to achieve the purpose of removing the odor of the caproic acid fermentation liquor;
Step three, esterifying the caproic acid fermentation liquor, regulating the PH value of the concentrated caproic acid fermentation liquor by using strong aromatic yellow water, adding edible alcohol and caproic acid esterifying enzyme, and starting stirring culture to obtain caproic acid esterified liquor with ethyl caproate concentration of more than 30.00 g/L;
and step four, distilling the caproic acid esterified liquid, distilling and extracting ethyl caproate by adopting a distillation device, and retaining the extracting liquid.
Preferably, the method for concentrating the caproic acid fermentation liquor in the step one comprises the steps of filtering the caproic acid fermentation liquor by using an inorganic permeable membrane, controlling the pore diameter of the membrane to allow water molecules to pass through, and then vacuumizing reversely by a vacuum machine to enable the water molecules to pass through the inorganic permeable membrane quickly, and controlling the multiple of concentration by controlling the amount of filtered water, thereby achieving the purpose of concentration.
Preferably, the deodorizing method for the dihexanoic acid fermentation liquor comprises the following steps: and (3) adding 2.00% of high-temperature Daqu powder into the caproic acid fermentation liquor by weight of the concentrated caproic acid fermentation liquor in the first step, uniformly stirring, and filtering the fermentation liquor by using a filter device with an active carbon fiber membrane after the culture is finished, so that the purpose of removing peculiar smell of the caproic acid fermentation liquor can be achieved after the filtration.
Preferably, in the esterification process of the caproic acid fermentation liquor in the third step, the pH of the fermentation liquor is regulated to be between 4 and 5 by using the concentrated aromatic yellow water after removing the peculiar smell in the second step, the caproic acid fermentation liquor is kept to be stirred in the process of adding the concentrated aromatic yellow water, the pH value of the solution is ensured to be stable, 60.00 percent of 98 percent of edible alcohol and 0.30 percent of caproic acid esterifying enzyme are added, and stirring culture is started for 1d at 50 ℃ to obtain the caproic acid esterifying liquor with the ethyl caproate concentration of more than 30.00 g/L.
Preferably, the distillation method of the caproic acid esterified liquid in the fourth step is as follows: the circulating water is heated rapidly by utilizing steam, the circulating water in the interlayer of the circulating fermentation tank is utilized, stirring is started, the caproic acid esterified liquid is heated uniformly rapidly, the circulating water is cooled by a cooling tower, the purpose of distilling and extracting ethyl caproate is achieved, the volume of the extracting solution is controlled, and the volume of the extracting solution is controlled: volume=1:5 of caproic acid esterification liquid.
Preferably, in the second step, the high-temperature Daqu powder is added into the fermentation tank and is cultured for 5 days at 34 ℃, and stirring is started for 10 minutes every 1 day.
Preferably, the fermentation tank and the temporary storage tank in the first to fourth steps are provided with stirring components for overturning the solution, and meanwhile, when medicines are added, the medicines are better dispersed uniformly, and meanwhile, the fermentation tank and the temporary storage tank are internally provided with a liquid level meter and a thermometer.
Preferably, the steam in the fourth step is communicated with the interlayer of the fermentation tank through the steam exchanger to form a loop, and meanwhile, an electric heating wire capable of heating the circulating water is arranged in the interlayer of the fermentation tank, so that the temperature of the circulating water is ensured to be stably increased.
Compared with the prior art, the invention has the beneficial effects that:
1. The caproic acid fermentation liquor is treated in the first step, and the concentration of the caproic acid can reach more than 100.00 g/L;
2. the caproic acid fermentation liquor is treated by the first and second steps, and has no peculiar smell;
3. the caproic acid fermentation liquid is treated by the first, second and third steps, the ethyl caproate content in the fermentation liquid can reach more than 30.00g/L, and the conversion efficiency of caproic acid can reach more than 50.00%;
4. The caproic acid fermentation liquor is treated by the first, second, third and fourth steps, and the concentration of ethyl caproate in the ethyl caproate fermentation liquor can reach 150g/L.
The concentration of the ethyl caproate solution obtained by concentrating, deodorizing, esterifying and distilling the caproic acid fermentation liquid generated by biological fermentation through the method is high, no peculiar smell exists, the ethyl caproate solution with higher purity can be obtained through byproducts of caproic acid bacteria fermentation, and the utilization rate of resources is improved.
Drawings
FIG. 1 is a schematic diagram of the step one caproic acid fermentation broth concentration process of the present invention;
FIG. 2 is a schematic diagram of the deodorizing process of a fermentation broth of step two caproic acid according to the present invention;
FIG. 3 is a schematic diagram of the distillation scheme of the step four caproic acid esterification liquid of the present invention;
FIG. 4 is a flow chart of a method for preparing a high-concentration ethyl caproate solution according to the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment provides a high-concentration ethyl caproate fermentation liquid, and the preparation process of the high-concentration ethyl caproate fermentation liquid comprises the following steps: 3000.00kg of caproic acid fermentation liquor (the concentration of caproic acid is 5.60 g/L) is taken, the fermentation liquor is concentrated by using an inorganic pervaporation membrane device shown in figure 1, the concentration of caproic acid in the concentrated caproic acid fermentation liquor reaches more than 100.00g/L, and the concentrated fermentation liquor is weighed and weighed, and the weight of the concentrated fermentation liquor is 159.00kg.
Adding 3.18kg of high-temperature Daqu into the concentrated caproic acid fermentation broth, culturing at 34 deg.C for 5d, stirring for 10min every day, and filtering with an activated carbon fiber membrane filter device shown in figure 2.
Adding strong aromatic yellow water to the fermentation broth to adjust pH to 4-5, adding 95.40kg of 98%vol edible alcohol and 0.48kg of esterifying enzyme, and culturing at 50deg.C under stirring for 1d.
Ethyl caproate was distilled from the caproate esterification liquid using the apparatus shown in fig. 3.
Example 2
The embodiment provides a high-concentration ethyl caproate fermentation liquid, and the preparation process of the high-concentration ethyl caproate fermentation liquid comprises the following steps: 3000.00kg of caproic acid fermentation liquor (the concentration of caproic acid is 10.80 g/L) is taken, the fermentation liquor is concentrated by using an inorganic pervaporation membrane device shown in figure 1, the concentration of caproic acid in the concentrated caproic acid fermentation liquor reaches more than 100.00g/L, and the concentrated fermentation liquor is weighed and weighed, and the weight of the concentrated fermentation liquor is 298.00kg.
Adding 5.96kg of high-temperature Daqu into the concentrated caproic acid fermentation broth, culturing at 34 deg.C for 5d, stirring for 10min every day, and filtering with an activated carbon fiber membrane filter device shown in figure 2.
Adding strong aromatic yellow water to the fermentation broth to adjust the pH to 4-5, adding 178.80kg of 98%vol edible alcohol and 0.89kg of esterifying enzyme, and culturing at 50 ℃ with stirring for 1d.
Ethyl caproate was distilled from the caproate esterification liquid using the apparatus shown in fig. 3.
Example 3
The embodiment provides a high-concentration ethyl caproate fermentation liquid, and the preparation process of the high-concentration ethyl caproate fermentation liquid comprises the following steps: 3000kg of caproic acid fermentation liquor (the concentration of caproic acid is 13.60 g/L) is taken, the fermentation liquor is concentrated by using an inorganic pervaporation membrane device shown in figure 1, the concentration of caproic acid in the concentrated caproic acid fermentation liquor reaches more than 100.00g/L, and the concentrated fermentation liquor is weighed, and the weight of the concentrated fermentation liquor is 398.00kg.
79.60Kg of high-temperature Daqu is added into the concentrated caproic acid fermentation broth, the mixture is cultured for 5 days at 34 ℃, stirring is started for 10min every day, and after the culture is finished, the mixture is filtered by an activated carbon fiber membrane filter device shown in figure 2.
Adding strong aromatic yellow water to the fermentation broth to adjust pH to 4-5, adding 238.80kg of 98%vol edible alcohol and 1.19kg of esterifying enzyme, and culturing at 50deg.C under stirring for 1d.
Ethyl caproate was distilled from the caproate esterification liquid using the apparatus shown in fig. 3.
When in specific use, the method comprises the following steps:
Step one, concentrating the caproic acid fermentation liquor, wherein an inorganic pervaporation membrane filter is communicated between a fermentation tank with the caproic acid fermentation liquor and a temporary storage tank through a pipeline, and a vacuum machine is also communicated with the outer side of the inorganic pervaporation membrane filter, and the caproic acid fermentation liquor is concentrated by adopting an inorganic pervaporation membrane, so that the concentration of the caproic acid is more than 100.00 g/L;
Step two, deodorizing the caproic acid fermentation liquor, namely conveying the caproic acid fermentation liquor concentrated in the step one into a filter through a pump body, mixing the caproic acid fermentation liquor with high-temperature Daqu before the step two, and simultaneously using active carbon in the filter to achieve the purpose of removing the odor of the caproic acid fermentation liquor;
Step three, esterifying the caproic acid fermentation liquor, regulating the PH value of the concentrated caproic acid fermentation liquor by using strong aromatic yellow water, adding edible alcohol and caproic acid esterifying enzyme, and starting stirring culture to obtain caproic acid esterified liquor with ethyl caproate concentration of more than 30.00 g/L;
Distilling the caproic acid esterified liquid, distilling and extracting ethyl caproate by adopting a distillation device, and retaining an extracting solution;
The method for concentrating the caproic acid fermentation liquor comprises the steps of filtering the caproic acid fermentation liquor by using an inorganic permeable membrane, controlling the pore diameter of the membrane to allow water molecules to pass, and then vacuumizing reversely by a vacuum machine to enable the water molecules to pass through the inorganic permeable membrane quickly, and controlling the multiple of concentration by controlling the amount of filtered water, so as to achieve the purpose of concentration;
The deodorizing method of the caproic acid fermentation liquor comprises the following steps: adding 2.00% of high-temperature Daqu powder into the caproic acid fermentation liquor by weight of the concentrated caproic acid fermentation liquor in the first step, uniformly stirring, filtering the fermentation liquor by using a filter device with an active carbon fiber membrane after the culture is finished, and removing peculiar smell of the caproic acid fermentation liquor after the filtration;
In the esterification process of the caproic acid fermentation liquor, the PH of the fermentation liquor is regulated to be between 4 and 5 by using the concentrated aromatic yellow water after the peculiar smell is removed in the second step, the caproic acid fermentation liquor is kept to be stirred in the process of adding the concentrated aromatic yellow water, the PH value of the solution is ensured to be stable, 60.00 percent of 98 percent of edible alcohol and 0.30 percent of caproic acid esterifying enzyme are added, stirring culture is started for 1d at 50 ℃, and the caproic acid esterifying liquor with the ethyl caproate concentration of more than 30.00g/L can be obtained;
The distillation method of the caproic acid esterified liquid in the fourth step is as follows: the circulating water is heated rapidly by utilizing steam, the circulating water in the interlayer of the circulating fermentation tank is utilized, stirring is started, the caproic acid esterified liquid is heated uniformly rapidly, the circulating water is cooled by a cooling tower, the purpose of distilling and extracting ethyl caproate is achieved, the volume of the extracting solution is controlled, and the volume of the extracting solution is controlled: volume=1:5 of caproic acid esterification liquid.
According to the data of the three embodiments, after the preparation method of the high-concentration ethyl caproate solution is used, the conversion rate of caproic acid esterification into ethyl caproate reaches more than 50%, and the concentration of the obtained ethyl caproate is greatly improved compared with the traditional preparation method.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (8)

1. A preparation method of a high-concentration ethyl caproate solution is characterized by comprising the following steps of: the method comprises the following steps:
Step one, concentrating the caproic acid fermentation liquor, wherein an inorganic pervaporation membrane filter is communicated between a fermentation tank with the caproic acid fermentation liquor and a temporary storage tank through a pipeline, and a vacuum machine is also communicated with the outer side of the inorganic pervaporation membrane filter, and the caproic acid fermentation liquor is concentrated by adopting an inorganic pervaporation membrane, so that the concentration of the caproic acid is more than 100.00 g/L;
Step two, deodorizing the caproic acid fermentation liquor, namely conveying the caproic acid fermentation liquor concentrated in the step one into a filter through a pump body, mixing the caproic acid fermentation liquor with high-temperature Daqu before the step two, and simultaneously using active carbon in the filter to achieve the purpose of removing the odor of the caproic acid fermentation liquor;
Step three, esterifying the caproic acid fermentation liquor, regulating the PH value of the concentrated caproic acid fermentation liquor by using strong aromatic yellow water, adding edible alcohol and caproic acid esterifying enzyme, and starting stirring culture to obtain caproic acid esterified liquor with ethyl caproate concentration of more than 30.00 g/L;
and step four, distilling the caproic acid esterified liquid, distilling and extracting ethyl caproate by adopting a distillation device, and retaining the extracting liquid.
2. The method for preparing the high-concentration ethyl caproate solution according to claim 1, wherein the method comprises the following steps: the method for concentrating the caproic acid fermentation liquor comprises the steps of filtering the caproic acid fermentation liquor by using an inorganic permeable membrane, controlling the pore diameter of the membrane to allow water molecules to pass, and then vacuumizing reversely by a vacuum machine to enable the water molecules to pass through the inorganic permeable membrane quickly, and controlling the concentration multiple by controlling the amount of filtered water, so that the purpose of concentration is achieved.
3. The method for preparing the high-concentration ethyl caproate solution according to claim 1, wherein the method comprises the following steps: the deodorizing method of the dihexanoic acid fermentation liquor comprises the following steps: and (3) adding 2.00% of high-temperature Daqu powder into the caproic acid fermentation liquor by weight of the concentrated caproic acid fermentation liquor in the first step, uniformly stirring, and filtering the fermentation liquor by using a filter device with an active carbon fiber membrane after the culture is finished, so that the purpose of removing peculiar smell of the caproic acid fermentation liquor can be achieved after the filtration.
4. The method for preparing the high-concentration ethyl caproate solution according to claim 1, wherein the method comprises the following steps: in the esterification process of the caproic acid fermentation liquor in the step III, the weight of the concentrated caproic acid fermentation liquor with the peculiar smell removed in the step II is used for regulating the pH value of the fermentation liquor to be between 4 and 5, the caproic acid fermentation liquor is kept to be stirred in the process of adding the concentrated yellow water, the pH value of the solution is ensured to be stable, 60.00 percent of 98 percent of edible alcohol and 0.30 percent of caproic acid esterifying enzyme are added, and stirring culture is started for 1d at 50 ℃ to obtain the caproic acid esterifying liquor with the ethyl caproate concentration of more than 30.00 g/L.
5. The method for preparing the high-concentration ethyl caproate solution according to claim 1, wherein the method comprises the following steps: the distillation method of the caproic acid esterified liquid in the step four is as follows: the circulating water is heated rapidly by utilizing steam, the circulating water in the interlayer of the circulating fermentation tank is utilized, stirring is started, the caproic acid esterified liquid is heated uniformly rapidly, the circulating water is cooled by a cooling tower, the purpose of distilling and extracting ethyl caproate is achieved, the volume of the extracting solution is controlled, and the volume of the extracting solution is controlled: volume=1:5 of caproic acid esterification liquid.
6. The method for preparing the high-concentration ethyl caproate solution according to claim 1, wherein the method comprises the following steps: in the second step, the high-temperature Daqu powder is added into the fermentation tank and is cultured for 5 days at 34 ℃, and stirring is started for 10 minutes every 1 day.
7. The method for preparing the high-concentration ethyl caproate solution according to claim 1, wherein the method comprises the following steps: the fermentation tank and the temporary storage tank in the first to fourth steps are provided with stirring components for overturning the solution, and meanwhile, when medicines are added, the medicines are better dispersed uniformly, and meanwhile, the fermentation tank and the temporary storage tank are internally provided with a liquid level meter and a thermometer.
8. The method for preparing the high-concentration ethyl caproate solution according to claim 1, wherein the method comprises the following steps: and in the fourth step, steam is communicated with the interlayer of the fermentation tank through the steam exchanger to form a loop, and meanwhile, an electric heating wire capable of heating the circulating water is arranged in the interlayer of the fermentation tank, so that the temperature of the circulating water is stably increased.
CN202410208474.9A 2024-02-26 2024-02-26 Preparation method of high-concentration ethyl caproate solution Pending CN118059683A (en)

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