CN110904279B - Segmented pH control method in lactic acid fermentation production - Google Patents
Segmented pH control method in lactic acid fermentation production Download PDFInfo
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Abstract
The invention discloses a segmented pH control method in lactic acid fermentation production, which comprises the following steps: (1) Adding an acid releasing agent into the fermentation liquid at the end stage of the rapid growth stage of the lactobacillus; (2) And adding an alkali releasing agent into the fermentation liquid at the final stage of the growth inhibition stage of the lactobacillus. The invention can effectively shorten the time for adjusting the pH of the fermentation liquid twice with one lower part and one higher part in the lactic acid fermentation production.
Description
Technical Field
The invention relates to the technical field of fermentation production of lactic acid. In particular to a segmented pH control method in lactic acid fermentation production.
Background
In 400 tonsFor example, as shown in FIG. 1, in the initial stage of adding lactic acid bacteria to the fermentation liquid, the fermentation liquid is weak in acidity (pH) Fast growth of thallus ) At the moment, the environment of the fermentation liquid is suitable for rapid growth of the lactic acid bacteria, but is not beneficial to acid production of the lactic acid bacteria; when the lactobacillus in the fermentation tank enters a stabilization period, the acidity of the fermentation liquid needs to be improved to pH Inhibition of bacterial growth The aim is to inhibit the rapid growth of the lactic acid bacteria, promote the lactic acid bacteria to convert sugar in the fermentation feed liquid into acid, and reduce the consumption of the lactic acid bacteria to the sugar in the fermentation feed liquid, the method for improving the acidity of the fermentation feed liquid in the prior art is to reduce the addition amount of a neutralizer, and the acidity of the fermentation feed liquid is gradually improved by using the acid produced by the lactic acid bacteria, which takes about 5 hours; when the rapid growth of lactobacillus is inhibited, the flow of neutralizer is increased to adjust the pH of the fermented liquid to Growth and acid production balance ，pH Fast growth of thallus <pH Growth and acid production balance <pH Inhibition of bacterial growth It takes about 5 hours. Therefore, it takes about 10 hours to adjust the pH of the fermentation broth twice, i.e., lower and higher, in the lactic acid fermentation production.
Disclosure of Invention
Therefore, the technical problem to be solved by the present invention is to provide a method for controlling pH in a staged manner in lactic acid fermentation production, which effectively shortens the time for adjusting the pH of the fermentation liquid twice, i.e. one time lower and one time higher in the lactic acid fermentation production.
In order to solve the technical problems, the invention provides the following technical scheme:
the sectional pH control method in the lactic acid fermentation production comprises the following steps:
(1) Adding an acid releasing agent into the fermentation liquid at the end stage of the rapid growth stage of the lactobacillus;
(2) And adding an alkali releasing agent into the fermentation liquid at the terminal stage of the growth inhibition stage of the lactic acid bacteria.
The stage pH control method in the lactic acid fermentation production comprises the following steps of (1): the time for the acid releasing agent to release the acid completely is less than 5 hours.
The stage pH control method in the lactic acid fermentation production comprises the following steps of (1): the time for the acid releasing agent to release the acid completely is less than or equal to 3 hours.
The stage pH control method in the lactic acid fermentation production comprises the following steps of (1): the acid releasing agent is water-soluble organic acid ester.
In the segmented pH control method in the lactic acid fermentation production, the water-soluble organic acid ester is glucolactone.
The stage pH control method in the lactic acid fermentation production comprises the following steps of (2): the time for the alkali releasing agent to completely release the alkali is less than 5 hours.
The stage pH control method in the lactic acid fermentation production comprises the following steps of (2): the time for the base releasing agent to completely release the base is less than or equal to 30 minutes.
The stage pH control method in the lactic acid fermentation production comprises the following steps of (2): the alkali releasing agent is hydrophobic calcium oxide.
The preparation method of the hydrophobic calcium oxide comprises the following steps:
(A) Adding tert-butyldimethylsilyl chloride powder into ethyl acetate, and stirring to obtain a solution A;
(B) Adding polydimethylsiloxane into the solution A obtained in the step (A), and stirring to obtain a solution B;
(C) Adding calcium oxide powder into the solution B obtained in the step (B), stirring, and performing calcium oxide surface hydrophobic modification;
(D) Filtering to obtain the surface hydrophobic modified calcium oxide, and vacuum drying to obtain the neutralizer for fermentation production of lactic acid.
The stage pH control method in the lactic acid fermentation production comprises the following steps: the mass fraction of the tert-butyldimethylsilyl chloride in the solution A is 5-15%, and the stirring time is more than or equal to 1 hour; in step (B): the adding amount of the polydimethylsiloxane is 5-10 times of the mass of the tert-butyldimethylsilyl chloride, and the stirring time is more than or equal to 0.5 hour; in step (C): the adding amount of the calcium oxide powder is 15-20% of the mass of the solution B, the granularity of the calcium oxide powder is 100-200 meshes, the stirring time is 48-72 hours, a saturated tyramine ethanol solution can be dropwise added in the stirring process, and the dropwise adding amount of the saturated tyramine ethanol solution is 10-30% of the mass of the solution A; the vacuum drying time is more than or equal to 10 hours, and the drying temperature is 50-100 ℃.
The technical scheme of the invention achieves the following beneficial technical effects:
since the acid releasing agent slowly releases the acid, the target pH can be adjusted according to the current pH Inhibition of bacterial growth And the amount of the fermentation liquid in the fermentation tank, the needed acid releasing agent is added into the fermentation liquid at one time, the local acidity of the fermentation liquid is not too strong to kill lactic acid bacteria, the acid releasing agent is uniformly distributed in the fermentation liquid under the stirring condition, the acid releasing agent slowly releases acid, the acidity of the fermentation liquid is gradually enhanced until the release of the acid releasing agent is finished, so that the pH value of the fermentation liquid is adjusted to the pH value Inhibition of bacterial growth By selecting an acid releasing agent that releases acid at a faster rate, "one low" pH adjustment time can be greatly shortened. Similarly, since the alkali releasing agent slowly releases the alkali, the target pH can be adjusted according to the current pH Growth and acid production balance And the amount of the fermentation liquid in the fermentation tank, the needed alkali releasing agent is added into the fermentation liquid at one time, so that the local alkalinity of the fermentation liquid is not too strong to kill lactic acid bacteria, the alkali releasing agent is uniformly distributed in the fermentation liquid under the stirring condition, the alkali releasing agent slowly releases alkali, the alkalinity of the fermentation liquid is gradually enhanced until the alkali releasing agent is completely released, and the pH of the fermentation liquid is adjusted to the pH value Growth and acid production balance By selecting an alkali releasing agent with a faster alkali releasing speed, the 'one-high' pH adjustment time can be greatly shortened.
When the neutralizer for producing lactic acid by fermentation, which is prepared by the invention, is used for adjusting the pH of the fermentation liquid, the pH of the fermentation liquid is not too high locally, the pH fluctuation during the adjustment period is small, and the fluctuation time during the adjustment is short. The reaction of the tert-butyldimethylsilyl chloride and the calcium oxide enables the tert-butyldimethylsilyl chloride to be coupled to the surface of calcium oxide particles, so that the hydrophobic modification of the surface of the calcium oxide is realized, the reaction speed of the calcium oxide and water is greatly delayed, the reaction time of the calcium oxide and the water is prolonged, heat is released in the reaction process of the calcium oxide and the water, the temperature stability of fermentation feed liquid is favorably maintained, and the power consumption is reduced. When the hydrophobic modified calcium oxide powder is added into the fermentation liquid, the hydrophobic modified calcium oxide powder reacts with water slowly in the initial stage, so that the local pH of the fermentation liquid is not temporarily overhigh, the hydrophobic modified calcium oxide powder is uniformly dispersed into the fermentation liquid along with continuous stirring in a fermentation tank, the reaction of calcium oxide and water is gradually accelerated, the pH of the fermentation liquid is uniformly increased everywhere, the adding frequency of the hydrophobic modified calcium oxide powder is controlled, the superposition of wave troughs and wave crests of the hydrophobic modified calcium oxide powder added twice and reacted with water can be realized, and the pH fluctuation is smaller and the fluctuation time is shorter in the process of adjusting the pH of the fermentation liquid. The polydimethylsiloxane has good permeability, can permeate the surfaces of calcium oxide particles, can improve the coupling depth of tert-butyldimethylsilane on the surfaces of the calcium oxide particles, can play a role in coating the surfaces of the calcium oxide particles and certain depth of the surfaces of the calcium oxide particles, and delays the reaction speed of calcium oxide and water. Tyramine is used for restraining HCl generated in the process that tert-butyldimethylsilane is coupled to the surfaces of the calcium oxide particles, and the coupling degree of the surfaces of the calcium oxide particles is improved.
Drawings
FIG. 1 shows that the pH value of the fermentation liquid is adjusted twice when the fermentation liquid is lower and higher in the lactic acid fermentation production.
FIG. 2 pH profiles of two neutralizing agents added to lactic acid solutions in example 1 and example 2.
Detailed Description
Example 1
The segmented pH control method in the lactic acid fermentation production is characterized by comprising the following steps:
(1) Adding an acid releasing agent into the fermentation liquid at the end stage of the rapid growth stage of the lactobacillus; the acid releasing agent is water-soluble organic acid ester, and the water-soluble organic acid ester is gluconolactone; the gluconolactone can be hydrolyzed in the fermentation liquid within 3 hours, the added amount of the gluconolactone is controlled according to the size of a fermentation tank in production and the amount of the fermentation material in the fermentation tank, so that the pH value of the fermentation liquid is reduced from about 5.8 to about 5.4, and the pH value is reduced from 5 hours to 3 hours in the 'one low' adjustment; gluconic acid and lactic acid may be separated in a subsequent molecular distillation process.
(2) Adding an alkali releasing agent into the fermentation liquid at the terminal stage of the growth inhibition stage of the lactic acid bacteria, wherein the alkali releasing agent is hydrophobic calcium oxide; the preparation method comprises the following steps:
(A) Adding 10kg of tert-butyldimethylsilyl chloride powder into 100kg of ethyl acetate, and stirring for 2 hours to obtain a solution A;
(B) Adding 50kg of polydimethylsiloxane into the solution A obtained in the step (A), and stirring for 1 hour to obtain a solution B;
(C) Adding 32kg of calcium oxide powder with the granularity of 100-200 meshes into the solution B obtained in the step (B), and stirring for 48 hours to perform surface hydrophobic modification on the calcium oxide;
(D) Filtering to obtain surface hydrophobic modified calcium oxide, washing with ethyl acetate for 3-5 times, vacuum drying at 100 deg.C for 15 hr to obtain neutralizing agent for fermentation production of lactic acid.
A50 g/L lactic acid solution (pH 5.68) was prepared, and the neutralizing agent prepared in this example was added in an amount of 0.5 times the amount of lactic acid in the solution, calculated as calcium oxide (other substances in the neutralizing agent were ignored). The agitation was turned on and the water bath maintained the solution temperature at 40 c and the pH of the solution was measured every two minutes, the results are shown in figure 2.
As can be seen from fig. 2, the calcium oxide in the neutralizing agent obtained in this example started to accelerate the reaction with water at around 16 minutes, and the pH of the solution reached 6.46 at 30 minutes, indicating that the lactic acid in the solution had completely reacted (the pH of 60.6g/L calcium lactate aqueous solution at 40 ℃ c was around 6.46) from the time the neutralizing agent was added to 30 minutes, and the pH of the solution did not change any more with time. According to the size of a fermentation tank in production and the amount of fermentation materials in the fermentation tank, the amount of the added surface hydrophobic modified calcium oxide is controlled to realize that the pH value of the fermentation material liquid is increased from about 5.4 to about 5.6, and is shortened from the original 5 hours to within 1 hour in the 'one-high' adjustment.
Example 2
The segmented pH control method in the lactic acid fermentation production comprises the following steps:
(1) Adding an acid releasing agent into the fermentation liquid at the end stage of the rapid growth stage of the lactobacillus; the acid releasing agent is water-soluble organic acid ester, and the water-soluble organic acid ester is gluconolactone; the gluconolactone can be hydrolyzed in the fermentation liquid within 3 hours, the added amount of the gluconolactone is controlled according to the size of a fermentation tank in production and the amount of the fermentation material in the fermentation tank, so that the pH value of the fermentation liquid is reduced from about 5.8 to about 5.4, and the pH value is reduced from 5 hours to 3 hours in the 'one low' adjustment; gluconic acid and lactic acid may be separated in a subsequent molecular distillation process.
(2) Adding an alkali releasing agent into the fermentation liquid at the final stage of the growth inhibition stage of the lactobacillus, wherein the alkali releasing agent is hydrophobic calcium oxide; the preparation method comprises the following steps:
(1) Adding 10kg of tert-butyldimethylchlorosilane powder into 100kg of ethyl acetate, and stirring for 2 hours to obtain a solution A;
(2) Adding 50kg of polydimethylsiloxane into the solution A obtained in the step (A), and stirring for 1 hour to obtain a solution B;
(3) Adding 32kg of calcium oxide powder with the granularity of 100-200 meshes into the solution B obtained in the step (B), stirring for 48 hours, dropwise adding a saturated tyramine ethanol solution at a constant speed in the stirring process (adding tyramine into absolute ethyl alcohol, stirring until tyramine is not dissolved any more to obtain the saturated tyramine ethanol solution), wherein the dropwise adding amount of the saturated tyramine ethanol solution is 22kg, and performing calcium oxide surface hydrophobic modification;
(4) Filtering to obtain surface hydrophobic modified calcium oxide, sequentially washing with ethyl acetate and anhydrous ethanol for 3-5 times, vacuum drying at 100 deg.C for 15 hr to obtain neutralizing agent for fermentation production of lactic acid.
A50 g/L solution of lactic acid (pH 5.68) was prepared and the neutralizing agent prepared in this example was added in an amount of 0.5 times the amount of the lactic acid in the solution, calculated as calcium oxide (other substances in the neutralizing agent were ignored). The agitation was turned on and the water bath maintained the solution temperature at 40 c and the pH of the solution was measured every two minutes, the results are shown in figure 2.
The calcium oxide in the neutralizer obtained in this example started to accelerate the reaction with water in about 23 minutes, and the solution pH reached 6.47 by 30 minutes, indicating that the lactic acid in the solution had completely reacted (60.6 g/L calcium lactate aqueous solution had a pH of about 6.46 at 40 ℃) from the time the neutralizer was added to 30 minutes, and the solution pH did not change any more with time. Compared with example 1, the neutralizing agent obtained in example 2 is more suitable for adjusting pH in lactic acid fermentation production, because about 25 minutes is needed for a hundred ton grade fermentation tank from material addition to uniform mixing, and calcium oxide starts to accelerate reaction with water at 23 minutes in the neutralizing agent obtained in example 2, so that local pH in the fermentation liquor is more effectively prevented from being too high to inhibit propagation of lactic acid bacteria or cause death of lactic acid bacteria, and the adjustment of the pH of the fermentation liquor is completed in a short time.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. This need not be, nor should it be exhaustive of all embodiments. And obvious variations or modifications are possible which remain within the scope of the appended claims.
Claims (7)
1. The segmented pH control method in the lactic acid fermentation production is characterized by comprising the following steps:
(1) Adding an acid releasing agent into the fermentation liquid at the end stage of the rapid growth stage of the lactobacillus;
(2) Adding an alkali releasing agent into the fermentation liquid at the terminal stage of the growth inhibition stage of the lactic acid bacteria;
the alkali releasing agent is hydrophobic calcium oxide;
the preparation method of the hydrophobic calcium oxide comprises the following steps:
(A) Adding tert-butyldimethylsilyl chloride powder into ethyl acetate, and stirring to obtain a solution A;
(B) Adding polydimethylsiloxane into the solution A obtained in the step (A), and stirring to obtain a solution B;
(C) Adding calcium oxide powder into the solution B obtained in the step (B), stirring, and performing calcium oxide surface hydrophobic modification;
(D) Filtering to obtain surface hydrophobic modified calcium oxide, and vacuum drying to obtain neutralizer for fermentation production of lactic acid;
in step (a): the mass fraction of the tert-butyldimethylsilyl chloride in the solution A is 5-15%, and the stirring time is more than or equal to 1 hour; in step (B): the adding amount of the polydimethylsiloxane is 5-10 times of the mass of the tert-butyldimethylsilyl chloride, and the stirring time is more than or equal to 0.5 hour; in step (C): the addition amount of the calcium oxide powder is 15-20% of the mass of the solution B, the particle size of the calcium oxide powder is 100-200 meshes, the stirring time is 48-72 hours, a saturated tyramine ethanol solution can be dropwise added in the stirring process, and the addition amount of the saturated tyramine ethanol solution is 20% of the mass of the solution A; the vacuum drying time is more than or equal to 10 hours, and the drying temperature is 50-100 ℃.
2. The stepwise pH control method according to claim 1, wherein in step (1): the time for the acid releasing agent to release the acid completely is less than 5 hours.
3. The method for staged pH control in lactic acid fermentation production according to claim 1, wherein in step (1): the time for the acid releasing agent to completely release the acid is less than or equal to 3 hours.
4. The method for staged pH control in lactic acid fermentation production according to claim 1, wherein in step (1): the acid releasing agent is water-soluble organic acid ester.
5. The stepwise pH control method according to claim 4, wherein the water-soluble organic acid ester is gluconolactone.
6. The stepwise pH control method according to claim 1, wherein in step (2): the time for the alkali releasing agent to completely release the alkali is less than 5 hours.
7. The stepwise pH control method according to claim 1, wherein in step (2): the time for the base releasing agent to completely release the base is less than or equal to 30 minutes.
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