CN108374025A - A kind of propionic acid preparation process - Google Patents
A kind of propionic acid preparation process Download PDFInfo
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- CN108374025A CN108374025A CN201810559638.7A CN201810559638A CN108374025A CN 108374025 A CN108374025 A CN 108374025A CN 201810559638 A CN201810559638 A CN 201810559638A CN 108374025 A CN108374025 A CN 108374025A
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- propionic acid
- rectifying
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- preparation process
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P7/00—Preparation of oxygen-containing organic compounds
- C12P7/40—Preparation of oxygen-containing organic compounds containing a carboxyl group including Peroxycarboxylic acids
- C12P7/52—Propionic acid; Butyric acids
Abstract
The invention belongs to technical field of food additives, are related to a kind of propionic acid preparation process；It specifically includes following steps：Sterilization treatment, inoculation, saccharification, fermentation, filtering, decoloration, rectifying tank rectifying；The present invention is using starch, malt as raw material, through high-temp steam sterilizing, inoculation, saccharification, fermentation, generate zymotic fluid, the gas with foreign flavor generated in fermentation process enters gas with foreign flavor processing system, filtrated air, inorganic nitrogen-sourced is supplemented in fermentation process, zymotic fluid is crystallized, filter, rectifying proposes 99% fermenting propionic acid, and for preparing culture medium after the steam condensation that rectifying generates, the propionic acid that rectifying goes out is according to calcium propionate production procedure production fermenting propionic acid calcium；The setting of its integrated artistic step improves the production efficiency and purity of propionic acid, reduces production cost, is convenient for commercial introduction and application.
Description
Technical field
The invention belongs to technical field of food additives, are related to a kind of propionic acid preparation process.
Background technology
It is important that propionic acid is that a kind of important industrial chemicals, propionic acid and its esters have in industries such as food, medicine, cosmetics
Purposes.The production method of propionic acid has chemical synthesis and biological fermentation process.Microorganism can utilize a variety of fermentable sugars next life
Propionic acid is produced, industrially can then introduce reactor first by a variety of biomass acid or enzyme hydrolysis at monosaccharide such as glucose or xyloses
Ferment, milk of lime be added after fermentation, precipitate, after filtering be added sodium sulphate carry out metathesis reaction, using filter and
Concentration is fractionated and is obtained after sulfuric acid conversion is added again, and immobilized protoplast tower reactor may be used in fermentation reactor,
Cell is fixed by following form：So that the filling ring surface to sterilize in advance is covered one layer with immersion method and passes through the bright containing 20% of sterilizing
The solution of glue and 1.5% shellac is sprayed with 2.5% glutaraldehyde water solution after doing, the macromolecule of filling ring surface is made to crosslink,
To increase intensity, then with aseptic water washing, is then sterilized, blown clean with sterilizing nitrogen after discharging ethylene glycol, hereafter with ethylene glycol
Propionic acid bacteria culture fluid is added into the reactor full of this ring type filling, it is made to form one layer of fixed cell membrane in filling ring surface,
Then can continuous charging ferment, but chemical synthesis pollution weight is of high cost, operating condition is harsh, therefore, biofermentation
Method becomes the important channel for preparing propionic acid, wherein the selection of nitrogen source, selection of pH value, raw material etc. are to propionic acid in biological fermentation process
Production all have large effect, it is also higher and higher to the repeatability of health with the raising of human living standard, to product
Requirement be also increasingly stringenter, existing biofermentation propionic acid have low production efficiency, purity is low, it is of high cost the problems such as, therefore, if
Count that a kind of production efficiency is high, propionic acid preparation process at low cost is very promising.
Invention content
It is an object of the invention to overcome disadvantage of the existing technology, propose to design a kind of propionic acid preparation process, to carry
The production efficiency and purity of high propionic acid.
To achieve the goals above, a kind of propionic acid preparation process of the present invention, specifically includes following steps：
（1）Sterilization treatment：Fermentation tank is passed through 0.6Mpa vapour cookings 30-40 minutes, is passed through filtrated air purging, it is dry；
（2）Inoculation, saccharification：30-50m is added into cooker3 Deionized water, then at the uniform velocity be added screening after starch and
The components by weight percent ratio of maltose, starch and maltose is 3：1, starch and maltose are added 30-50 tons altogether, are stirred when being added
It mixes, after being uniformly mixed, steam boiling 6-8 hours is added, boiling temperature is 120-145 DEG C, steam pressure 0.2MPa；
Then after being cooled to 85-90 DEG C, amylase, carbohydrase and bacillus is added, after stirring evenly, is sent into fermentation tank, carries out close
Close fermentation；
（3）Fermentation：Starch and maltose after being inoculated with, being saccharified keep the temperature 50-70 DEG C in fermentation tank, and supplement filtrated air,
Control air mass flow is 5m3/ h, supplement is inorganic nitrogen-sourced, and calcium bicarbonate is added, and control pH value is 3.0-4.5；Ferment the gas generated
The fermented tank top of body is discharged into gas absorption system；
（4）Filtering, decoloration：Fermented tank ferments 48 hours, and fermented liquid is flowed out at pressurization top, and fermented liquid enters after filtering
Zymotic fluid holding vessel, the thalline filtered out recycle；Filtered fermented liquid pump squeezes into bleacher, and activity is added
Filtrate after 50-55 DEG C of heating is decolourized, is sent into rectifying tank by charcoal；
（5）Rectifying tank rectifying：It is 75-80 DEG C of progress rectifying, reflux ratio 5 to control the heating temperature in rectifying tank：1, tower top temperature
53-57 DEG C of degree, overhead condensate reflux, middle part lateral line discharging to propionic acid coarse fodder tank receive propionic acid after testing and send to propionic acid after qualification
Finished pot is to get propionic acid finished product；
（6）Condensate liquid is formed after the steam condensation that rectifying tank tower top rectifying generates, condensate liquid enters tower top condensate tank, for preparing
Culture medium.
Step of the present invention（2）Middle amylase, carbohydrase and the components by weight percent of bacillus ratio are 4:2.5:0.5.
Propionic acid quality Fen Shuo≤99.0% prepared by the present invention, purity is high, has a extensive future.
Compared with prior art, the present invention having the advantages that：The present invention is using starch, malt as raw material, through high temperature
Steam sterilizing, inoculation, saccharification, fermentation, generate zymotic fluid, and the gas with foreign flavor generated in fermentation process enters gas with foreign flavor processing system
System, supplement filtrated air in fermentation process, inorganic nitrogen-sourced, zymotic fluid is crystallized, filtering, rectifying propose 99% fermenting propionic acid, rectifying
For preparing culture medium after the steam condensation of generation, the propionic acid that rectifying goes out produces fermenting propionic acid calcium according to calcium propionate production procedure；
The setting of its integrated artistic step improves the production efficiency and purity of propionic acid, reduces production cost, convenient for commercial introduction and
Using.
Description of the drawings：
Fig. 1 is the process flow chart of the present invention.
Specific implementation mode
Below by specific embodiment, the invention will be further described.
Embodiment 1：
Propionic acid preparation process described in the present embodiment, specifically includes following steps：
（1）Sterilization treatment：Fermentation tank is passed through 0.6Mpa vapour cookings 30 minutes, is passed through filtrated air purging, it is dry；
（2）Inoculation, saccharification：30m is added into cooker3 Deionized water, then at the uniform velocity be added screening after starch and malt
The components by weight percent ratio of sugar, starch and maltose is 3：1, starch and maltose are added 30 tons altogether, stir while adding, and stirring is mixed
After closing uniformly, steam boiling 6 hours is added, boiling temperature is 120 DEG C, steam pressure 0.2MPa；Then it is cooled to 85-90 DEG C
Afterwards, amylase, carbohydrase and bacillus is added, after stirring evenly, is sent into fermentation tank, carries out sealed fermenting；
（3）Fermentation：Starch and maltose after being inoculated with, being saccharified keep the temperature 50 DEG C in fermentation tank, and supplement filtrated air, control
Air mass flow is 5m3/ h supplements liquefied ammonia, and calcium bicarbonate is added, and control pH value is 3.0；Ferment the fermented tank deck of gas generated
Portion is discharged into gas absorption system；
（4）Filtering, decoloration：Fermented tank ferments 48 hours, and fermented liquid is flowed out at pressurization top, and fermented liquid enters after filtering
Zymotic fluid holding vessel, the thalline filtered out recycle；Filtered fermented liquid pump squeezes into bleacher, and activity is added
Filtrate after 50 DEG C of heating is decolourized, is sent into rectifying tank by charcoal；
（5）Rectifying tank rectifying：It is 75 DEG C of progress rectifying, reflux ratio 5 to control the heating temperature in rectifying tank：1, tower top temperature 53
DEG C, overhead condensate reflux, middle part lateral line discharging to propionic acid coarse fodder tank receives propionic acid after testing and send to propionic acid finished pot after qualification,
Up to propionic acid finished product；
（6）Condensate liquid is formed after the steam condensation that rectifying tank tower top rectifying generates, condensate liquid enters tower top condensate tank, for preparing
Culture medium.
Step described in the present embodiment（2）Middle amylase, carbohydrase and the components by weight percent of bacillus ratio are 4:2.5:
0.5。
Embodiment 2：
Propionic acid preparation process described in the present embodiment, specifically includes following steps：
（1）Sterilization treatment：Fermentation tank is passed through 0.6Mpa vapour cookings 35 minutes, is passed through filtrated air purging, it is dry；
（2）Inoculation, saccharification：40m is added into cooker3 Deionized water, then at the uniform velocity be added screening after starch and malt
The weight ratio of sugar, starch and maltose is 3：1, starch and maltose are added 40 tons altogether, stir while adding, and are stirred
After even, steam boiling 7 hours is added, boiling temperature is 130 DEG C, steam pressure 0.2MPa；Then 90 DEG C are cooled to, is added and forms sediment
Powder enzyme, carbohydrase and bacillus after stirring evenly, are sent into fermentation tank, carry out sealed fermenting；
（3）Fermentation：Starch and maltose after being inoculated with, being saccharified keep the temperature 60 DEG C in fermentation tank, and supplement filtrated air, control
Air mass flow is 5m3/ h supplements liquefied ammonia, and calcium bicarbonate is added, and control pH value is 3.5；Ferment the fermented tank deck of gas generated
Portion is discharged into gas absorption system；
（4）Filtering, decoloration：Fermented tank ferments 48 hours, and fermented liquid is flowed out at pressurization top, and fermented liquid enters after filtering
Zymotic fluid holding vessel, the thalline filtered out recycle；Filtered fermented liquid pump squeezes into bleacher, and activity is added
Filtrate after 53 DEG C of heating is decolourized, is sent into rectifying tank by charcoal；
（5）Rectifying tank rectifying：It is 77 DEG C of progress rectifying, reflux ratio 5 to control the heating temperature in rectifying tank：1, tower top temperature 56
DEG C, overhead condensate reflux, middle part lateral line discharging to propionic acid coarse fodder tank receives propionic acid after testing and send to propionic acid finished pot after qualification,
Up to propionic acid finished product；
（6）Condensate liquid is formed after the steam condensation that rectifying tank tower top rectifying generates, condensate liquid enters tower top condensate tank, for preparing
Culture medium.
Step described in the present embodiment（2）Middle amylase, carbohydrase and the components by weight percent of bacillus ratio are 4:2.5:
0.5。
Embodiment 3：
Propionic acid preparation process described in the present embodiment, specifically includes following steps：
（1）Sterilization treatment：Fermentation tank is passed through 0.6Mpa vapour cookings 40 minutes, is passed through filtrated air purging, it is dry；
（2）Inoculation, saccharification：50m is added into cooker3 Deionized water, then at the uniform velocity be added screening after starch and malt
The components by weight percent ratio of sugar, starch and maltose is 3：1, starch and maltose are added 50 tons altogether, stir while adding, and stirring is mixed
After closing uniformly, steam boiling 8 hours is added, boiling temperature is 145 DEG C, steam pressure 0.2MPa；Then after being cooled to 90 DEG C,
Amylase, carbohydrase and bacillus is added, after stirring evenly, is sent into fermentation tank, carries out sealed fermenting；
（3）Fermentation：Starch and maltose after being inoculated with, being saccharified keep the temperature 70 DEG C in fermentation tank, and supplement filtrated air, control
Air mass flow is 5m3/ h supplements liquefied ammonia, and calcium bicarbonate is added, and control pH value is 4.5；Ferment the fermented tank deck of gas generated
Portion is discharged into gas absorption system；
（4）Filtering, decoloration：Fermented tank ferments 48 hours, and fermented liquid is flowed out at pressurization top, and fermented liquid enters after filtering
Zymotic fluid holding vessel, the thalline filtered out recycle；Filtered fermented liquid pump squeezes into bleacher, and activity is added
Filtrate after 55 DEG C of heating is decolourized, is sent into rectifying tank by charcoal；
（5）Rectifying tank rectifying：It is 80 DEG C of progress rectifying, reflux ratio 5 to control the heating temperature in rectifying tank：1, tower top temperature 57
DEG C, overhead condensate reflux, middle part lateral line discharging to propionic acid coarse fodder tank receives propionic acid after testing and send to propionic acid finished pot after qualification,
Up to propionic acid finished product；
（6）Condensate liquid is formed after the steam condensation that rectifying tank tower top rectifying generates, condensate liquid enters tower top condensate tank, for preparing
Culture medium.
Step described in the present embodiment（2）Middle amylase, carbohydrase and the components by weight percent of bacillus ratio are 4:2.5:
0.5。
Comparative example 1：A kind of propionic acid preparation process
Comparative example 1 and the preparation method of embodiment 3 are essentially identical, difference lies in：Step in comparative example 1（3）The nitrogen source of supplement
For corn steep liquor.
Comparative example 2：A kind of propionic acid preparation process
Comparative example 2 and the preparation method of embodiment 3 are essentially identical, difference lies in：Step in comparative example 2（2）Starch and malt
The components by weight percent ratio of sugar is 3：2.
Comparative example 3：A kind of propionic acid preparation process
Comparative example 3 and the preparation method of embodiment 3 are essentially identical, difference lies in：Step in comparative example 3（2）Starch and malt
The components by weight percent ratio of sugar is 4：1.
Experimental example 1：Propionic acid prepares experiment：
In order to illustrate the effect of the present invention, applicant has been following contrast experiment：It is divided into 6 groups of experiments, the 1st group, the 2nd group and
3 groups prepare propionic acid according to the step of preparation process of embodiment 1, embodiment 2 and embodiment 3 respectively；4th group, the 5th group, the 6th component
Not Cai Yong comparative example 1, comparative example 2, comparative example 3 step of preparation process prepare propionic acid；After testing, the 1st group, the 2nd group and the 3rd group
The propionic acid mass fraction of preparation is respectively 99.2%, 99.3%, 99.6%, and the propionic acid quality of the 4th group, the 5th group, the 6th group preparation point
Number is respectively 60%, 80%, 83%, and the propionic acid mass fraction prepared using the present invention it can be seen from experimental result is higher, purity
It is high；By the 3rd group and the 4th group, the experimental results showed that, the selection of nitrogen source prepares purity to propionic acid has large effect, of the invention
Processing step selects corn steep liquor as nitrogen source, and the propionic acid mass fraction prepared is relatively low, and selects liquefied ammonia as nitrogen source, with this hair
Bright overall step is equipped with, and is substantially increased and is calculated mass fraction, improve production efficiency；By the 3rd group, the 5th group and the 6th
Group the experimental results showed that, the components by weight percent of starch and maltose, which compares propionic acid and prepares purity, equally has large effect, this hair
It is 3 that bright processing step, which selects starch and maltose components by weight percent ratio,:1 ratio is optimal proportion, the propionic acid quality prepared
Score substantially increases and calculates mass fraction, and improve production efficiency 90% or more.
Above-mentioned specific implementation mode is only the specific case of the present invention, and scope of patent protection of the invention includes but not limited to
The product form and style of above-mentioned specific implementation mode, any claims of the present invention and any technical field of meeting
The appropriate changes or modifications that those of ordinary skill does it, all shall fall within the protection scope of the present invention.
Claims (5)
1. a kind of propionic acid preparation process, it is characterised in that：Specifically include following steps：
（1）Sterilization treatment：Fermentation tank is passed through 0.6Mpa vapour cookings 30-40 minutes, is passed through filtrated air purging, it is dry；
（2）Inoculation, saccharification：30-50m is added into cooker3 Deionized water, then at the uniform velocity be added screening after starch and wheat
The components by weight percent ratio of bud sugar, starch and maltose is 3：1, starch and maltose are added 30-50 tons altogether, stir while adding,
After being uniformly mixed, steam boiling is added；Then after being cooled to 85-90 DEG C, amylase, carbohydrase and bacillus is added,
After stirring evenly, it is sent into fermentation tank, carries out sealed fermenting；
（3）Fermentation：Starch and maltose after being inoculated with, being saccharified keep the temperature 50-70 DEG C in fermentation tank, and supplement filtrated air,
Control air mass flow is 5m3/ h, supplement is inorganic nitrogen-sourced, and calcium bicarbonate is added, and control pH value is 3.0-4.5；Ferment the gas generated
The fermented tank top of body is discharged into gas absorption system；
（4）Filtering, decoloration：Fermented tank ferments 48 hours, and fermented liquid is flowed out at pressurization top, and fermented liquid enters after filtering
Zymotic fluid holding vessel, the thalline filtered out recycle；Filtered fermented liquid pump squeezes into bleacher, and activity is added
Filtrate after 50-55 DEG C of heating is decolourized, is sent into rectifying tank by charcoal；
（5）Rectifying tank rectifying：It is 75-80 DEG C of progress rectifying, reflux ratio 5 to control the heating temperature in rectifying tank：1, tower top temperature
53-57 DEG C of degree, overhead condensate reflux, middle part lateral line discharging to propionic acid coarse fodder tank receive propionic acid after testing and send to propionic acid after qualification
Finished pot is to get propionic acid finished product；
（6）Condensate liquid is formed after the steam condensation that rectifying tank tower top rectifying generates, condensate liquid enters tower top condensate tank, for preparing
Culture medium.
2. propionic acid preparation process according to claim 1, it is characterised in that：The step（2）Middle addition steam boiling
Time is 6-8 hours, and boiling temperature is 120-145 DEG C, steam pressure 0.2MPa.
3. propionic acid preparation process according to claim 1, it is characterised in that：The step（2）Middle amylase, carbohydrase
Components by weight percent ratio with bacillus is 4:2.5:0.5.
4. propionic acid preparation process according to claim 1, it is characterised in that：The step（3）The inorganic nitrogen of middle supplement
Source is liquefied ammonia.
5. propionic acid preparation process according to claim 1, it is characterised in that：Propionic acid prepared by the propionic acid preparation process
Quality Fen Shuo≤99.0%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112176005A (en) * | 2020-10-27 | 2021-01-05 | 清远一生自然生物研究院有限公司 | Production method of calcium propionate |
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Application publication date: 20180807 |