SU1070155A1 - Process for producing food vinegar - Google Patents

Abstract

1. Process for the preparation nHUlEBOGO VINEGAR by oxidation in the battery fermenters ethanol acetate bacteria in a medium consisting of ethyl alcohol, acetic acid, phosphate, or potassium sulfate, phosphate or ammonium sulfate and magnesium sulfate, clarified vinegar to obtain biomass-acetic acid the treatment of biomass, the separation of the liquid fraction from it and the introduction of the liquid fraction in the During the process, a fermenter, in contrast to the fact that, in order to increase the rate of formation of acetic acid and increase its yield, simultaneously with the liquid fraction, 0.5-1.0% of the volume is introduced into the first one during the process. nutrient medium 5% ammonia water, and as the liquid fraction using hydrolyzed biomass in the amount of 0.2-2.0% of the volume of the nutrient medium. 2. Method POP.1, distinguish ayu1D and also with the fact that the processing of biomass of acetic acid bacteria is carried out by its hydrolysis with 0, S-1.0% -HUM lysosubtilin POH solution at hydromodule 4-6, pH 6.8-8 , 5 and 36.5-37.5 C for 30-40 minutes. 3. Method POP.1, characterized in that the processing of biomass of acetic acid bacteria B (L is given by its hydrolysis with an 8-12% solution of acetic acid or 5-7% solution of hydrochloric or 9-12% growth using sulfuric acid, or 9-12% solution of orthophosphoric acid at a hydromodule 4-G and 110-140 ° C for 1-2 hours. 4. Method according to claim 1, characterized in that when brightening vinegar pasted over with bentonite, image Biomass of acetic acid bacteria is processed by hydrolysis in the presence of bentonite.

Description

The invention relates to the microbiological industry, in particular to methods for producing edible vinegar. A known method for producing edible vinegar by oxidizing ethyl alcohol with acetic acid bacteria in a fermenter battery, separating the acetic acid bacteria biome, extracting it, and returning the extract to the SP oxidation stage. The closest to the present invention is a method of obtaining food vinegar by oxidation in the battery of fermenters of ethyl alcohol with acetic acid bacteria in a nutrient medium consisting of ethyl alcohol, acetic acid, potassium phosphate or sulfate, ammonium phosphate or ammonium sulfate and magnesium sulfate, clarifying vinegar to obtain biomass-acetic acid bacteria, process the biomass, separate the liquid fraction from it and introduce the liquid fraction to the first fermenter during the process. The biomass is treated by extraction with alcohol 21. The disadvantage of this method is the low yield of the finished product and the insufficient oxidation rate, but this method does not provide for a more complete utilization of the potential possibilities of the bacterial cells. . The purpose of the invention is to increase the rate of formation of acetic acid and increase its yield. This goal is achieved in that according to the method of preparing food vinegar by oxidation in the battery of ethyl alcohol fermenters with acetic acid bacteria in a nutrient medium consisting of ethyl alcohol, acetic acid, potassium phosphate or sulfate, ammonium phosphate or magnesium sulfate and magnesium sulfate, clarifying the vinegar to obtain the biomass of acetic acid bacteria, processing the biomass of separating the liquid fraction from it and introducing the liquid fraction into the first during the process of the fermenter, simultaneously with the liquid fraction during the first ca fermenter administered 0.51, 0% of the volume of nutrient medium with 5% ammonia water, and as the liquid fraction of the biomass hydrolyzate used in an amount of 0.2-2.0% by volume of the nutrient medium. It is advisable to treat the biomass of acid-acid bacteria by its hydrolysis with O, 5% -1.0% solution of lysosubtilin POh with hydromodu 4-6, pH 6.8-8.5 and 36.5-37, in for 30-40 minutes Biomass treatment of acetic acid bacteria is carried out by hydrolizing it with an 8-12% solution of acetic acid or 5-7% solution of SALT - OR 9g12% solution of sulfuric or 9-12% solution of phosphoric acid at hydromodule 4-6 and 110140 C for 1-2 hours. It is recommended when brightening vinegar pasted over with bentonite, acetic acid bacteria should be treated with biomass by hydrolysis in the presence of bentonite. The proposed method is carried out as follows. Dietary vinegar is obtained by oxidizing ethyl alcohol by cultivating acetic acid bacteria on an alcohol-containing medium in a continuous, downhole manner in a battery of 3–4 fermenters using the flow chart for aeration of 0.20, 3, and 28–32 ° C. In the head apparatus of the battery simultaneously with a nutrient medium containing,%: alcohol 7.0-8.0, acetic acid 1.5-2.5. potassium mono- or bi-substituted phosphate or potassium sulphate 0.005–0.02 ammonium phosphate-one or disubstituted ammonium or ammonium sulfate 0.01–0.05, magnesium sulfate 0.00.5-0.2, urea 0, and 5% ammonia water 0.5-1 by volume, the hydrolyzate of biomass of acetic acid bacteria is fed in the amount of 0.2-2% of the volume of the incoming medium. The biomass hydrolyzate of acetic acid bacteria is obtained by processing the acetic acid biomass waste production of acetic acid bacteria separated from vinegar at the clarification stage. Biomass is separated by filtration through microporous filters or by centrifuging, or separation, or by using bentonite introduced into raw vinegar in an amount of 0.3-0.5%. After adding bentonite, the resulting suspension is stirred for 30-60 minutes, settled 4-6, h; II filter through filter paper. Biomass obtained by clarifying raw vinegar by centrifuging, filtering through microfilters or by separation, contains 17-21% solids, and the residue obtained by clarifying raw vinegar using bentonite contains 2035% solids, 3-8% of this amount is the actual biomass of acetic acid bacteria, the rest is bentonite. By acid or enzymatic hydrolysis of the biomass of acetic acid bacteria, it is possible to obtain products that are easily obtained by acetic acid bacteria — peptides, oligopentides, and amino acids. Acid hydrolysis of biomass or bentonite sediment with biomass of acetic acid bacteria is carried out with 8–12% acetic or 5–7% hydrochloric, or 9–12% sulfuric, or 9–12% orthophosphoric acid with the hydromodule 4-6, 110-140C for 1-2 hours. The degree of hydrolysis by the number of destroyed cells is 70-.80%, the hydrolyzate of pure biomas contains 7-9 mg / ml of amino acids, and the hydrolyzate of bentonite sediment contains 1- 2 mg / ml of amino acids, including,% of the sum of amino acids: lizin 11, histidine 5, arginine 7, aspartic acid 9, threonine 6, serine 4, glutamic acid that 11, pro ling 4, glycine 5, alanine 7, valine b, methionine 2, iisoleucine 5, leucine 8, tyrosine 3, phenylalanine 4, the sum of three ptophan, cysteine and cystine composition is 3%. Enzymatic hydrolysis is subjected to biomass without bintonite. Hydrolysis is carried out with a 0.5-1.0% solution of lysosubtilin riOxinpH in a hydronic unit 4-6, pH 6.8-8.5 and 3B, 5-37.5 in 30-40 minutes. The degree of hydrolysis is 100% by the number of destroyed cells. The hydrolyzate contains 3035% (by dry weight) of protein compounds, including 17–19% of proteins, 13–14% of peptides, and lower peptides of the no acid in trace amounts. The biomass hydrolyzate is directly fed to the head fermenter without further processing, the biomass hvdrolizat with bentonite must be separated from the bentonite sludge by filtration through filter paper, and then fed to the head fermenter battery. Bentonite sludge is sent for regeneration, which involves processing with neutralizing solution and water. . After regeneration, the bentonite is recycled to clarify the raw vinegar. The bentonite residue after acetic acid hydrolysis does not need regeneration. The addition of biomass hydrolyzate to the culture medium for the cultivation of acetic acid bacteria makes it possible to reduce the consumption of mineral salts by a factor of 2. to intensify the multiplication of bacteria 1.2-1.3 times and increase the rate of formation of acetic acid by 1.5-2 times. As a result of the addition of the hydrolyzate, the nutrient flow in the battery is increased by 1.5-2 times, and the number of fermenters decreases from 4-5 to 3. Equipment released as a result of process intensification can be used to increase the capacity of the plant. Table 1 shows the dependence of the degree of hydrolysis (hydromodule 5 on the temperature and duration of the process. From the data of Table 1 it follows that for acid hydrolysis, the optimum temperature range is 110140 ° C with a process duration of 1-2 hours, since further temperature rise and an increase in the duration of hydrolysis does not give positive results.For enzymatic hydrolysis, temperatures in the range 36.5-37.5 ° C are optimal for a duration of 30-40 minutes. Table 2 shows the dependence of the degree of hydrolysis on the end Concentrations of the hydrolyzing agent and hydromodule. From the data of Table 2 it follows that the hydromodules 4.5 and 6 are optimal. Increasing the hydromodule to 7 does not give a positive effect on the degree of hydrolysis, but leads to the dilution of extractive substances in the hydrolyzate, which is not economically profitable. The optimal concentrations of hydrolysing agents are as follows: acetic acid 8-12%, hydrochloric acid 5-7%, sulfuric acid 9-12%, phosphoric acid 9-12%, lysosubtilin 0.5-1,, 0%. A further increase in the concentration of hydrolyzing agents does not give a positive effect. Enzymatic hydrolysis should be carried out at a pH value corresponding to the optimum effect of the lysosubtilin enzyme. Full lysis of acetic acid bacteria cells is achieved in the pE 6.8-0.5 range. Deviations from these values lead to a decrease in the degree of hydrolysis. So, at pH 6.7 it is equal to 85%, and at pH 8.9 it is 9.5%. Data on the choice of optimal amounts of acetic acid bacteria biomass hydrolysates, which allow to intensify the process of obtaining biochemical vinegar, are presented in Table 3. The composition of the nutrient medium supplied to the 1st fermenter of the battery is as follows: ethyl alcohol 7.57 acetic acid 2.0; monobasic potassium phosphate 0.01; disubstituted ammonium phosphate 0.02 magnesium sulfate 0.01; Urea 0.05 5% ammonia water 0.5. Acetic acid formation rate and biomass concentration are determined in the 1st battery fermenter, where the process is most intense. All variants of hydrolysis can be considered alternative in their effect on the rate of formation of acetic acid and the development of biomass of acetic acid bacteria. The enzymatic hydrolyzate on the activating effect on the process of obtaining acetic acid is somewhat inferior to acid hydrolyzates, but the method of hydrolysis is faster and less laborious, this is an advantage of enzymatic hydrolysis. The optimal concentrations for applying pure biomass hydrolysates of 0.2-0.5% byproduct, for biomass hydrolysates with bentonite sediment 1-2%. .. PRI and measure 1. Carry out; the process of obtaining edible vinegar in the battery of 4 fermenters. The composition of the nutrient medium supplied to the head fermenter,%: ethyl alcohol 6.0, acetic acid 2.0 / potassium phosphate 0.05, phosphate ammonium 0.1, magnesium sulfate O, 05, urea 0.05 / 5% sinus water 1. In the 2nd fermenter serves additionally ethyl alcohol In an amount of 1.5% of the volume medium. The concentration of acetic acid in the battery increases as follows: 1st fermentor 5.6%, 2nd 2nd 7.5%; 3rd 8.5%; 4th 9.1%. The duct is 0.44 m / h, the amount of 100% acetic acid obtained from a battery is 750.0 kg / day, the rate of formation of acetic acid in the 1st oxide body is 16.0 kg / h, the biomass concentration is 0.15 g / l, the output of acetic acid 84,46%. ., .one .. --.- . With 2% hydrochloric acid biomass hydrolyzate of acetic acid bacteria with bentonite, the process is carried out in a battery of 3 fermenters. To obtain a hydrolyzate, a bentonite precipitate with biomass (1000 kg1 containing 35% solids is used. Hydrolysis is carried out in a reactor with 5% hydrochloric acid and hydrated b for 2 hours. After cooling, the suspension is filtered through a filter board. 1750 L are obtained hydrolyzate. When using this hydrolyzate, the concentration of neural and organic additives in the medium fed to the head fermenter is halved (potassium phosphate 0.020%; ammonium phosphate 0-, 05%; magnesium sulfate O., 020%; urine by 0.020% / 5% ammonia water 0.05%), ethyl alcohol concentration and increase to 7.5%, the concentration of acetic acid is 2.0%. The concentration of acetic acid in the battery will melt as follows: 1st farm, 6.0%; 2nd, 8.1%; 3rd, 9.2 %. Flow O, 71., / Amount of 100% acetic acid obtained from the battery, 1227, 1 kg / day, biomass formation rate 0.19 g / l. Output of acetic acid 87.2%. Example 2 The method was carried out: as in Example 1, only phosphoric acid hydrolyzate of acetic acid bacteria with bentonite 6 - RB-% is used instead of hydrochloric acid bentonite hydrolyzate. To obtain hydrolysis, a bentonite precipitate (flOOO kg) containing 30% of dry substances is used. The hydrolysis is carried out in a 12% phosphoric acid 99 reactor at a water ratio of 5, 120 C. for 1 hour. After cooling, the suspension is filtered through filter paper and 1000 l of gmdrolizate are obtained. When using this hydrolyzate, the concentration of mineral substances is reduced as compared with the experience without hydrolyzate and is,%: potassium phosphate 0.01, ammonium phosphate 0.02; magnesium sulfate 0.01. The concentration of acetic acid in the battery increases as follows: 1st fermenter 6.0%, 2nd 8.3%, 3rd 9.4%. Flow, O, 7 m- / h, amount of 100% acetic acid acid, obtained from the battery 1243.2 kg / day, the rate of formation of acetic acid in the 1st oxidizer is 28.0 kg / h, the biomass concentration is 0.19 g / l. The output of acetic acid. 87.9%. Example 3. The method is carried out analogously to example 1, except that bentonite sulfate is used to hydrolyze acetic acid bacteria (1% by volume). Hydrolyzate production day. Bentonite precipitate with biomass (1000 kg, containing 33% solids is used .. Hydrolysis is carried out in a reactor with 9% sulfuric acid. At hydromodule 4 for 2 hours at -30 ° C. After cooling and filtration, 650 l are obtained hydrolyzate. When using this hydrolyzate, the concentration of mineral and organic additives is, in%: potassium phosphate, 0.005, urea, 0.05, ammonium phosphate, 0.01, magnesium sulfate, 0.005, 5% ammonia water, 0.5. acid in the battery increases as follows: 1st fermenter 6.0%, 2nd 8.1%, 3rd 9.2%. The flow rate is 0.65 m / h, the amount of 100% acetic acid obtained from the battery is 1123 kg / day, the rate of formation of acetic acid in the 1st oxidizer is 26 kg / h, the biomass concentration is 0.17 g / l. The yield of acetic acid 87.7%. Example 4. The method is carried out analogously to Example 1.1, but using acetic acid bentonite hydrolyzate of acetic acid bacteria (1% by volume). Bentonite sediment with biomass (1000 kg) containing 30% dry matter is hydrolyzed in the 9% reactor. acid (raw vinegar) at the hydromodule 5, 120 ° C for 2 hours. After cooling and filtration, 950 l of hydrolyzate was obtained. When using this hydrolyzate, the concentration of mineral and organic additives is,%: potassium phosphate O ,, 02; ammonium phosphate 0.05; magnesium sulfate 0.02, urea 0.05; .-, (- 5% ammonia water 0.5. The concentration of acid with the acid in the battery increases as follows: 1st fermentor 6.0%; 2nd 8.4%; 3rd 9.4%. Duct 0 , 80, the amount of 100% acetic acid obtained from the battery is 1420.8 kg / day, the rate of formation of acetic acid in the 1st oxidizer is 32 kg / h, the biomass concentration is 0.18 g / l. The output of acetic acid is 87.2 %

EXAMPLE 5 The method is carried out analogously to example 1, but hydrochloric acid hydrolyzate of acetic acid bacteria is used (0.2 vol.% Obtained by the action of a 5% HC1 solution. To obtain a hydrolyzate of acetic acid bacteria 5.0 kg), separated from the crude vinegar by centrifugation, is hydrolyzed with 7% hydrochloric acid at hydronic unit b for 2 hours. Get 30 l gvdrolizat. The acid concentration in the battery increases as follows: 1st fermenter 6.0%; 2nd 8.0%; 3rd 9.0%. channel 0.7, the number. 100% acetic acid obtained from a battery is 1193 kg / day, the rate of formation of acetic acid in the 1st oxidizer is 28.4 kg / h, the biomass concentration is 0.18 g / l, the yield of acetic acid is 87.5%,

Example 6. The method is carried out analogously to example 1, but using 0.5% acetic acid hydrolyzate of acetic acid bacteria obtained by the action of 9% vinegar. To obtain biomass hydrolyzate, acetic acid bacteria (5.0 kg), separated from raw vinegar by separation, are hydrolyzed with 9% acetic acid (crude vinegar) at hydromodule 6, 12 OC for 2 hours. 32 L of hydrolyzate is obtained. The concentration of micronal and organic additives in the atomic experiment,%: potassium phosphate 0.01; ammonium phosphate 0.02, magnesium sulfate 0.01 j urea 0, .05; 5% ammonia water 0.5. The alcohol concentration is 7.0%, the acid concentration. 2.5%.

The concentration of acetic acid in the battery increases as follows: 1st fermentor 6.5%, 2nd 7.9; 3rd 9.3%. The flow channel was 0.76 m3 / h, the amount of 100% acetic acid obtained from a 12403 battery, 2 kg / day, the formation rate of acetic acid in the first oxidizer was 30.4 kg / h, the biomass concentration was 0.18 g / l, the yield acetic acid 87.0%.

Example 7 The process is carried out analogously to Example 1, but using 0.3% acetic acid biomass sulphate of biomass. To obtain a biomass hydrolyzate of acetic acid bacteria (6.5-g), separated from the crude vinegar by centrifugation, a guide), they were oxidized with 9% sulfuric acid at a hydromodule b, 120 ° C for 1.5 hours. 45 l of the hydrolyzate is obtained. Mineral concentration

and organic additives in the nutrient medium,%: potassium phosphate 0.01, ammonium phosphate 0.02, magnesium sulfate 0.01 urea 0.05 / 5% ammonia water 0.5. The concentration of acetic acid in the battery increases as follows: 1st fermentor 6.0%; 2nd 8.05%; 3rd 9.05%. The flow is 0.68 m / h, the amount of 100% acetic acid obtained from a battery is 1150.5 kg / day, the rate of formation of acetic acid in the 1st oxidizer is 27.0 kg / h, the biomass concentration is 0.20 g / l Acetic acid yield 87.1%

EXAMPLE 8 The method is carried out analogously to example 1, but using 0.2% phosphoric acid biomass hydrolyzate of acetic acid bacteria. To obtain a biomass hydrolyzate, acetic acid bacteria (G kg), separated from the raw vinegar by centrifugation, is hydrolyzed with 12% phosphoric acid at a hydronic module 6, 120 ° C for 1 hour. 40 liters of hydrolyzate are obtained. Concentration of mineral and organic additives to the nutrient medium,%: potassium phosphate 0.01, ammonium phosphate: 0.02; magnesium sulfate 0.01; Urea 0.05, 5% ammonia water 0.5. The concentration of alcohol in the environment of 8.0%, acetic acid 1.5%. The concentration of acetic acid in the battery increases as follows: 1st fermenter 6, 0.2th 8.15%; 3rd 9.10%, flow 0.62, the amount of 100% acetic acid obtained from a battery is 1160.6 kg / day, the rate of formation of acetic acid in one oxidizer is 27.3 kg / h, the biomass concentration is 0.18 g / l. The output of acetic acid 87,5

An example. The method is carried out analogously to example 1, but using 0.2% acetic acid bacteria hydrolyzate obtained by the action of lysosubtilin G 10x. To obtain a biomass hydrolyzate, acetic / acidic bacteria, separated from the raw vinegar by centrifugation (5 kg), are neutralized with 10% NaOH solution to pH 7.5, then diluted 5 times with water and added 125 g of lysosubstilin 10x, t. e. 0.5%. The mixture is kept in a thermostat for 30 minutes. 25 liters of hydrolyzate are obtained. A nutrient medium containing,%: potassium phosphate, 0.005; ammonium phosphate 0.01; magnesium sulfate 0.005; Urea 0.05, 5% ammonia water 0.5. The concentration of acetic acid in the battery increases as follows: 1st fermenter 6.0%, 2nd 8.0%; 3rd 9.2%. The duct is 0.60 the amount of 100% acetic acid obtained from the battery is 1036.8 kg / day, the rate of formation of acetic acid in the 1st oxide

 24 kg / h biomass concentration 0.18 g / p, acetic acid yield 88.2%.

Table 4 shows the potential | Characteristic proposed and known methods.

Thus, the proposed method, compared with the prototype, increases the yield of the finished product by 2%, the process is accelerated -V 1.5-2 times due to an increase in the oxidative activity of the culture.

Table

table 2

Continuation of the tabl., 3 Guides) olieat Amount of hydrocollate, introduced into the fermenter,% vol. Fliva ' 1B (-I Enzymatic 0.1 0.2 0.5 0.6 Indicators I Prototype Formation rate of acetic acid in the first oxidizer, kg / h 14 The yield of acetic acid,% 85-86

Continued table. 3 centrations Obramass velocity, calling VKj, / jj hydrochloric acid, kg / h 0.15 16.6 0.18 24.0 0.18 22.4 0.18 20.2. Table. 4. I The proposed method i 24-32, J 87-88

Claims (4)

1. METHOD FOR PRODUCING FOOD VINEGAR by oxidizing ethyl alcohol in the battery of fermenters with acetic acid bacteria in a nutrient medium consisting of ethyl alcohol, acetic acid, potassium phosphate or sulfate, ammonium phosphate or sulfate and magnesium sulfate, clarifying vinegar to obtain biomass uk- ⁴ acid bacteria, processing biomass, separating the liquid fraction from it and introducing the liquid fraction into the first fermenter along the process, characterized in that, in order to increase the rate of formation of acetic acid and increase it in yield, simultaneously with the liquid fraction in the first during the process of the fermenter enter 0.5-1.0% of the volume. the nutrient medium is 5% ammonia water, and a biomass hydrolyzate in an amount of 0.2-2.0% of the volume of the nutrient medium is used as the liquid fraction. 2. The method according to claim 1, characterized in that the biomass of acetic acid bacteria is processed by hydrolysis of it with a 0.8-1.0% solution of lysosubtilin G10x at a hydromodule of 4-6, pH 6.8- 8.5 and 36.5-37.5 ° C for 30-40 minutes. 3. The method according to claim 1, wherein the treatment of the biomass of acetic acid bacteria is carried out by hydrolysis of it with an 8-12% solution of acetic or 5-7% solution of hydrochloric or 9 -12% sulfuric solution, or 9-12% phosphoric acid solution with a hydromodule of 4-6 and 110-140 ° C for 1-2 hours 4. The method according to claim 1, characterized in that when bleaching vinegar glued with bentonite, the biomass of acetic acid bacteria is processed by hydrolysis in the presence of bentonite. Xia>