CN112795461B - Efficient recovery method of effective components in solid-state fermentation vinegar frying process - Google Patents
Efficient recovery method of effective components in solid-state fermentation vinegar frying process Download PDFInfo
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Abstract
An efficient recovery method of effective components in the process of solid-state fermentation of aromatic vinegar and fried vinegar. Relates to the field of edible vinegar fermentation production. The vinegar frying pot is characterized in that a secondary steam outlet is formed in the top of the vinegar frying pot, and the temperature of secondary steam discharged from the secondary steam outlet is 98-102 ℃; introducing the secondary steam into a shell and tube condenser; the shell-and-tube condenser comprises a tube side and a shell side, wherein a secondary steam inlet is formed in the middle of the shell side, a secondary steam condensate outlet is formed in the bottom of the shell side, and a non-condensable gas outlet is formed in the top of the shell side; the tube side is provided with a cooling water inlet and a cooling water outlet; the secondary steam condensate outlet is connected with a condensate storage tank; after the secondary steam passes through the shell-and-tube condenser, condensing the secondary steam to obtain condensed vinegar with the acetic acid content of 4.5-5.5 g/100mL, and discharging the rest non-condensable gas in the secondary steam through the non-condensable gas outlet. The invention has simple process, easy production and high recovery efficiency.
Description
Technical Field
The invention relates to the field of fermented edible vinegar production, in particular to improvement of a steam residual vinegar recovery technology in a vinegar frying process in the traditional solid-state fermented aromatic vinegar processing.
Background
The traditional aromatic vinegar production in China mostly adopts a solid state fermentation process, and the general process adopts the processes of rice → soaking → cooking → drenched rice → mixed koji → saccharification → wine making → vinegar making → drenched vinegar → fried vinegar → aged wine → filling and the like. The fried vinegar has several purposes, firstly, most of mixed bacteria in the raw vinegar are killed by frying the vinegar, the vinegar is beneficial to preservation, and secondly, organic matters such as protein and the like in the raw vinegar are heated, denatured and solidified by frying the vinegar, the turbidity is reduced by precipitation, and the brightness and the posture of the vinegar are improved; thirdly, Maillard reaction easily occurs at higher temperature, and the color of the vinegar is improved. Fourthly, the content of volatile acid and moisture is reduced by frying the vinegar. Due to the above functions, the conventional process is used in the production process of the prior aromatic vinegar. Taking 6 tons of raw vinegar in one pot as an example, after boiling, the boiling is maintained for 30-40 min, the evaporated feed liquid accounts for about 300kg of raw materials, and the evaporated feed liquid takes away water and simultaneously evaporates and takes away the corresponding acetic acid. Although acetic acid is generally considered to have a higher boiling point than water and to evaporate most of the water, the amount of acetic acid volatilized is actually considerable for a low-concentration acetic acid aqueous solution. Through our research, the acetic acid content in the steam in the tail gas is about 80% of the acetic acid content of the primary vinegar.
CN210367630U of national intellectual property office 2020-4-21 announcement, the name "a fry in shallow oil vinegar jar with waste gas recycle" for avoiding frying in shallow oil vinegar in-process "vinegar steam" directly discharging, lead to acid gas polluted environment to and the purpose of cooling liquefaction recovery to the vinegar steam that can volatilize, disclose a fry in shallow oil vinegar jar with waste gas recycle, its technical scheme includes: including a jar body (1), this jar body (1) inboard lower extreme is equipped with heating coil (2), the upper end of the jar body (1) is toper structure (3), and toper structure (3) upper end is connected with exhaust outlet (4), the top level of the jar body (1) is provided with condensing coil (5), toper structure (3) and exhaust outlet (4) are bilayer structure, establish intermediate layer (6) in and, the interior winding of intermediate layer (6) of exhaust outlet (4) is equipped with cooling shower (7). Finally, the condenser coil that jar body top level set up, with the vinegar steam direct contact condensation of tank deck portion become liquid, can effectively avoid vinegar steam to directly discharge in the air, also can retrieve volatile vinegar steam cooling liquefaction simultaneously, just toper structure and exhaust outlet are bilayer structure, establish the intermediate layer in and the intermediate layer of exhaust outlet surrounds being equipped with the cooling shower in the intermediate layer of exhaust outlet for to the cooling of exhaust outlet's intermediate layer inner wall, guarantee not have the vinegar steam of condensation in condenser coil department to carry out the secondary condensation liquefaction, further carry out recovery processing to vinegar steam, reach the standard of exhaust gas zero release basically, and can practice thrift 100 kg's vinegar in every 5 tons of raw vinegar heating processes, improved the output of vinegar. We note that this case has several problems:
firstly, cooling device does not carry out effective control to the condensation effect, and direct open discharges, and vinegar is difficult to obtain guaranteeing to high-efficient recovery vinegar, according to it vinegar technology is fried in shallow oil to the tradition of case calculates, and actual evaporation capacity is vinegar volume for 200~250kg, and its vinegar of retrieving is only 100kg, and recovery efficiency is lower.
Secondly, the evacuation port is directly arranged at the top of the condensing structure at the upper part of the tank body, so that the tank body is of an open structure, although the exhaust gas outlet is in an outward positive pressure state in the vinegar frying process, when the vinegar frying process is finished and cooked vinegar is transferred, external air can enter to pollute the cooked vinegar.
And thirdly, the space of the tank top is limited, and the space of a heat transfer area required by sufficient heat exchange is not provided. The full condensation of steam is difficult to be guaranteed, and the vinegar recovery efficiency is influenced.
In conclusion, the document does not consider the change of the cooling water consumption required by the condensing steam caused by the change of the actual feeding amount, the heating steam temperature and the pressure, so that the condensing effect of the process is difficult to ensure, and the cooling water consumption is difficult to accurately and efficiently control. The technical scheme of the reference is difficult to meet the requirement of high efficiency for effectively recycling the residual steam vinegar in the vinegar frying process, and the recycling efficiency is insufficient.
Disclosure of Invention
Aiming at the problems, the invention provides the efficient recovery method of the effective components in the solid-state fermentation aromatic vinegar fried vinegar process, which has high recovery efficiency and can ensure the quality of cooked vinegar.
The technical scheme of the invention is as follows: filling raw vinegar with acetic acid content of 5.0-5.5 g/100mL into a vinegar frying tank, heating the vinegar frying tank to 98-105 ℃, maintaining boiling vinegar frying temperature for 30-40 minutes,
a secondary steam outlet is formed in the top of the vinegar frying tank, and the temperature of secondary steam discharged from the secondary steam outlet is 98-102 ℃;
introducing the secondary steam into a shell and tube condenser; the shell-and-tube condenser comprises a tube side and a shell side, wherein a secondary steam inlet is formed in the middle of the shell side, a secondary steam condensate outlet is formed in the bottom of the shell side, and a non-condensable gas outlet is formed in the top of the shell side;
the tube side is provided with a cooling water inlet and a cooling water outlet; the secondary steam condensate outlet is connected with a condensate storage tank;
after the secondary steam passes through the shell-and-tube condenser, condensing the secondary steam to obtain condensed vinegar with the acetic acid content of 4.5-5.5 g/100mL, and discharging the rest non-condensable gas in the secondary steam through the non-condensable gas outlet.
The temperature of the cooling water inlet is 10-30 ℃, and the temperature of the cooling water outlet is controlled to be less than or equal to 50 ℃.
And the cooling water outlet is connected with a cooling water elevated tank.
And a liquid seal pipeline structure is arranged between the condensate storage tank and the secondary steam condensate outlet.
The vinegar frying tank, the tube array condenser, the condensate storage tank and the (gas, liquid) pipeline are made of 316L stainless steel materials.
The shell and tube condenser be vertical structure, the cooling water inlet set up in shell and tube condenser bottom, intercommunication shell and tube condenser's tube side, the cooling water outlet set up in shell and tube condenser top, communicate again the cooling water elevated tank.
The non-condensable gas discharge port is provided with a non-condensable gas discharge valve for regulating the discharge amount of non-condensable gas.
The device is characterized in that a controller is further arranged, a cooling water inlet regulating valve is further arranged at the cooling water inlet, a pressure sensor is further arranged at the non-condensable gas outlet, and the pressure sensor, the non-condensable gas discharge valve and the cooling water inlet regulating valve are connected with the controller.
After the vinegar frying is finished (namely, the boiling temperature of the fried vinegar is maintained for 30-40 minutes), the vinegar frying pot is naturally cooled to 60-72 ℃, the non-condensable gas discharge valve is opened, the outer end of the discharge port is sleeved with a 0.1 mu m air filter, and then the cooked vinegar in the vinegar frying pot is discharged, so that the secondary pollution of the cooked vinegar is avoided.
Compared with the prior art, the invention adopts the tubular condensing device separated from the vinegar frying tank body, and forms an independent condensing environment of secondary vinegar steam in the shell pass of the tubular condensing device. The non-condensable gas can be effectively limited to be discharged by adjusting the opening degree and pressure control of the non-condensable gas discharge valve; and a high-precision pressure sensor is arranged on the tail gas discharge pipe to detect the pressure of the exhaust port, and the flow of cooling water is automatically adjusted through a PLC control system (controller), so that the aim of effectively condensing and recycling evaporated vinegar under the condition of saving the flow of the cooling water at most is finally achieved. The vinegar frying process improves the secondary steam recovery process, reduces the amount of volatile acetic acid discharged into the atmosphere by more than 95 percent, and effectively protects the environment. The cooling water realizes the internal circulation of the process without increasing consumption or discharge. The method has the advantages of simple process, less investment, easy implementation in production and remarkable economic benefit. The vinegar frying pot realizes the isolation state with the outside, avoids the defect of direct communication of air, and improves the safety of the final cooked vinegar.
The vinegar frying pot realizes the isolation state with the outside, avoids the defect of direct communication of air, and improves the safety of the final cooked vinegar. The invention carries out a separated condensation treatment process on steam generated in the decoction process, collects acetic acid and flavor component condensate with higher boiling point relative to water, has the recovery rate of evaporated acetic acid of more than 95 percent, produces more edible vinegar of 4 percent, has simple process, less investment, easy implementation in production, high safety of prepared food and has obvious economic benefit.
Drawings
Figure 1 is a schematic diagram of the operation of the present invention,
in the figure, 1 is a heating device, 2 is a vinegar frying tank, 21 is raw vinegar, 22 is vinegar steam, 3 is a secondary steam outlet, 4 is a cooling water elevated tank, 5 is a cooling water outlet, 6 is a non-condensable gas discharge valve, 7 is a non-condensable gas discharge port, 8 is a secondary steam condensate discharge port, 9 is a condensate storage tank, 10 is a shell and tube condenser, 11 is a cooling water inlet, 12 is a cooling water inlet regulating valve, 13 is a cooked vinegar discharge port, 14 is a secondary steam inlet, and 15 is a liquid seal pipeline structure.
Detailed Description
In order to reveal the importance of acetic acid recovery from steam during vinegar frying, the inventors tested the amount of acetic acid volatilization carried away in the steam. For 500mL of raw vinegar with acidity of 5.5g/100mL, simulating the water evaporation amount of the existing vinegar decocting process, collecting 25mL of steam complete condensate, analyzing that the acidity of acetic acid in the steam is about 5.2g/100mL and accounts for about 4.73% of the original vinegar, proving that considerable acetic acid is carried away in the raw vinegar decoction steam with low-concentration acetic acid content, and the recovery is meaningful.
The technical scheme of the invention is as follows: filling raw vinegar 21 with acetic acid content of 5.0-5.5 g/100mL into a vinegar decocting pot 2, heating the vinegar decocting pot 2 to 98-105 ℃ by a heating device 1, maintaining boiling vinegar decocting temperature for 30-40 minutes, forming vinegar steam 21 at the top of the vinegar decocting pot 2,
a secondary steam outlet 3 is formed in the top of the vinegar frying pot, and the temperature of secondary steam discharged from the secondary steam outlet is 98-102 ℃; then introducing the secondary steam into the shell and tube condenser 10 through a pipeline; the shell-and-tube condenser 10 comprises a tube side and a shell side, wherein the middle part of the shell side is provided with a secondary steam inlet 14, the bottom of the shell side is provided with a secondary steam condensate outlet 8, and the top of the shell side is provided with a non-condensable gas outlet 7; the inner diameter of the non-condensable gas outlet 7 is 12-18 mm, and a small amount of volatile gas is discharged; the tube pass is provided with a cooling water inlet 11 and a cooling water outlet 5; the secondary steam condensate outlet 8 is connected with a condensate storage tank 9 (in which condensed vinegar is collected, the quality of which is basically equal to that of cooked vinegar);
after the secondary steam passes through the shell-and-tube condenser, the secondary steam is condensed to prepare condensed vinegar with the acetic acid content of 4.5-5.5 g/100mL, and the rest non-condensable gas in the secondary steam is discharged through a non-condensable gas outlet 7. The recovery rate of the effective components of the vinegar is more than 95 percent
The temperature of the cooling water inlet is 10-30 ℃, and the temperature of the cooling water outlet is controlled to be less than or equal to 50 ℃.
The cooling water outlet 5 is connected with a cooling water elevated tank 4. The cooling water inlet regulating valve 12 can realize self-regulation of flow according to the magnitude of heat load. That is, when the temperature of the cooling water outlet 5 exceeds the threshold value, the flow rate is increased to control the outlet temperature.
A liquid seal pipeline structure 15 is arranged between the condensate storage tank 9 and the secondary steam condensate outlet 8. The function of the secondary steam condensate discharge port 8 is to prevent the non-condensed gaseous components in the secondary steam from overflowing.
The vinegar frying tank 2, the tubular condenser 10, the condensate storage tank 9 and the (gas, liquid) pipeline are made of 316L stainless steel materials. And manufacturing and processing equipment for the chlorine ion resistant materials such as 316L stainless steel with low carbon content. Other materials, such as steel, 304 stainless steel, etc., do not have this characteristic.
The shell and tube condenser 10 is of a vertical structure, a cooling water inlet 11 is arranged at the bottom of the shell and tube condenser 10 and communicated with a tube pass of the shell and tube condenser 10, and a cooling water outlet 5 is arranged at the top of the shell and tube condenser 10 and communicated with the cooling water elevated tank 4. In order to ensure the heat conduction effect, the heat exchange area is 1.5 times of the theoretical calculation area, the effective condensation of secondary steam is ensured, and water is saved to the maximum extent.
A non-condensable gas discharge valve 6 is provided at the non-condensable gas discharge port 7 to adjust the discharge amount of the non-condensable gas.
The device is also provided with a controller, a cooling water inlet regulating valve 12 is also arranged at the cooling water inlet 11, a pressure sensor (PT) is also arranged at the non-condensable gas outlet 7, and the pressure sensor and the cooling water inlet regulating valve 12 are connected with the controller. A non-condensable gas discharge valve 6 arranged at the discharge port can adjust the discharge amount of non-condensed gas; the tail gas discharge pipe is provided with a high-precision pressure sensor for detecting the pressure of the exhaust port, the pressure sensor transmits the pressure to the controller, the error between the set value and the feedback value is automatically calculated, the output value is calculated and sent to the cooling water regulating valve, the flow of the cooling water is automatically regulated, and finally the purpose of realizing effective condensation and recovery of evaporated vinegar under the condition of saving the flow of the cooling water to the utmost extent is achieved.
After the vinegar frying is finished (namely, the boiling temperature of the fried vinegar is maintained for 30-40 minutes), the vinegar frying tank 2 is naturally cooled to 60-72 ℃, the non-condensable gas discharge valve 6 is opened, the outer end of the discharge port is sleeved with a 0.1 mu m air filter, and the cooked vinegar in the vinegar frying tank 2 is discharged, so that the secondary pollution of the cooked vinegar is avoided.
The method comprises the following specific steps:
1) introducing secondary steam into a tubular condenser 10 at a secondary steam outlet 3 at the top end of a traditional vinegar frying tank, opening cooling water after raw vinegar is heated to boil, collecting condensed liquid, maintaining decoction for 30-40 minutes, merging the collected condensate into the vinegar frying tank to serve as a cooked vinegar finished product, and effectively recovering acetic acid and volatile flavor substances in the secondary steam.
2) During the secondary steam condensation operation, and set up noncondensable gas discharge port 7 on the top, during the operation, control cooling water flow adjusts 6 apertures of noncondensable gas discharge valve, lets a small amount of gas directly discharge in the atmosphere (the emission is about 0.1~0.3% of throwing the raw vinegar), during the operation, according to the pressure in the tail gas discharge pipe, through the flow of controlling cooling water inlet governing valve 12 and adjusting cooling water inlet 11, makes the abundant condensation of secondary steam. The non-condensable gas is mainly rich in alcohols, aldehydes, acids and other volatile substances with lower boiling points. Meanwhile, non-condensable gas dissolved in the raw material is removed, and the heat transfer efficiency is improved.
3) The cooling water for secondary steam is introduced into the elevated tank 4 and is used for the procedures of washing rice, soaking rice, showering rice, washing the ground and the like in the traditional vinegar production, and the water consumption cannot be increased due to the recycling of the secondary steam vinegar.
4) The condenser adopts a vertical heat exchanger 10, secondary steam flows through a shell pass, so that non-condensable gas discharge ports 7 at the upper end of the shell pass are convenient for discharging the non-condensable steam, and secondary steam condensate discharge ports 8 are arranged at the bottom of the shell pass and are convenient for recovering acetic acid; the cooling water condenser is internally provided with a cooling water outlet, the temperature of the cooling water outlet does not exceed 50 ℃, the scale accumulation of tap water is effectively reduced, and the tube pass is more convenient for scale mechanical cleaning.
5) After the vinegar is naturally cooled to less than 70 ℃, an air filter with the diameter of 0.1 mu m is sleeved on a discharge port behind the non-condensable gas discharge valve 6, the non-condensable gas discharge valve 6 is opened to ensure the discharge and respiratory balance, the cooked vinegar is conveyed to a subsequent mature vinegar working section, and the secondary pollution of the cooked vinegar is avoided.
Examples
Raw vinegar decoction and feeding of 5m3Placing in a vinegar decocting pot 2 with acidity of 5.5g/100mL and heating steam pressure of 0.2MPa, heating to boiling time of 42min, opening cooling water valve after boiling, and setting the initial flow of cooling water to 8m3H, collecting condensate, and continuously adjusting the opening of the non-condensing steam discharge valve 6 to make the condensate present a small amount of steamAnd (4) excluding. The heat exchange area of the condenser is 8m2When the pressure sensor (PT) in the condenser discharge pipe reaches 100mmH2When O is detected, the regulator will automatically regulate the inlet cooling water inlet valve (12) to increase the water flow by 1m3After each 50mmH increase or decrease in the pressure signal2The O system can automatically increase or decrease the flow of inlet cooling water by 1m3H is used as the reference value. The boiling was maintained for 33min, the collected condensate was 251.5 liters, the acidity was 4.6g/100mL, and the recovered acetic acid accounted for 4.2% of the total charge. And condensing and cooling the non-condensed exhaust gas discharged to the atmosphere, collecting and measuring 5.4 liters of volume and 3.08g/100mL of acidity, and calculating to obtain the acetic acid recovery rate in secondary steam to reach 98.4%. The amount of cooling water is 4.8m3The cooling water stored in the head tank 4 is used as supplementary water for washing rice, soaking rice and showering rice in the wine making section, and is used completely.
Claims (5)
1. A method for efficiently recovering active ingredients in a solid-state fermentation aromatic vinegar frying process includes the steps of filling raw vinegar with the acetic acid content of 5.0-5.5 g/100mL into a vinegar frying tank, heating the vinegar frying tank to 98-102 ℃, maintaining the boiling vinegar frying temperature for 30-40 minutes, and is characterized in that,
a secondary steam outlet is formed in the top of the vinegar frying tank, and the temperature of secondary steam discharged from the secondary steam outlet is 98-102 ℃;
introducing the secondary steam into a shell and tube condenser; the shell-and-tube condenser comprises a tube side and a shell side, wherein a secondary steam inlet is formed in the middle of the shell side, a secondary steam condensate outlet is formed in the bottom of the shell side, and a non-condensable gas outlet is formed in the top of the shell side;
the tube side is provided with a cooling water inlet and a cooling water outlet; the secondary steam condensate discharge port is connected with a condensate storage tank; the temperature of the cooling water inlet is 10-30 ℃, and the temperature of the cooling water outlet is controlled to be less than or equal to 50 ℃; the cooling water outlet is connected with a cooling water head tank; the shell and tube condenser is of a vertical structure, the cooling water inlet is arranged at the bottom of the shell and tube condenser and communicated with a tube pass of the shell and tube condenser, and the cooling water outlet is arranged at the top of the shell and tube condenser and communicated with the cooling water head tank;
after the secondary steam passes through the shell-and-tube condenser, condensing the secondary steam to prepare condensed vinegar with the acetic acid content of 4.5-5.5 g/100mL, and discharging the rest non-condensable gas in the secondary steam through the non-condensable gas outlet;
after the vinegar frying is finished, naturally cooling the vinegar frying tank to 60-72 ℃, opening the non-condensable gas discharge valve, sleeving an air filter with the diameter of 0.1 mu m on the outer end of the discharge port, and discharging the cooked vinegar in the vinegar frying tank to avoid secondary pollution of the cooked vinegar.
2. The method for efficiently recovering active ingredients in the vinegar frying process through solid state fermentation of aromatic vinegar as claimed in claim 1, wherein a liquid seal pipeline structure is arranged between the condensate storage tank and the secondary steam condensate outlet.
3. The method for efficiently recovering active ingredients in the solid-state fermentation aromatic vinegar-fried vinegar process according to claim 1, wherein the vinegar-frying tank, the tubular condenser, the condensate storage tank and the pipeline are made of 316L stainless steel.
4. The method for recovering effective components of vinegar during the course of vinegar-frying through solid-state fermentation as claimed in claim 1, wherein a non-condensable gas discharge valve is provided at the non-condensable gas discharge port to adjust the discharge amount of non-condensable gas.
5. The method for efficiently recovering active ingredients in the vinegar frying process through solid state fermentation of vinegar as claimed in claim 4, wherein a controller is further provided, a cooling water inlet regulating valve is further provided at the cooling water inlet, a pressure sensor is further provided at the non-condensable gas discharging port, and the pressure sensor, the non-condensable gas discharging valve and the cooling water inlet regulating valve are connected with the controller.
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| CN102352302A (en) * | 2011-10-13 | 2012-02-15 | 江苏恒顺醋业股份有限公司 | Heating device for frying pan |
| CN206995905U (en) * | 2017-06-06 | 2018-02-13 | 南昌金轩科技有限公司 | A kind of Acetic Acid Recovering Column |
| CN110172388A (en) * | 2019-06-25 | 2019-08-27 | 江苏恒顺醋业云阳调味品有限责任公司 | A kind of pan-fried vinegar tank utilized with waste gas recovery |
| CN210367630U (en) * | 2019-06-25 | 2020-04-21 | 江苏恒顺醋业云阳调味品有限责任公司 | Fry in shallow oil vinegar jar with waste gas recovery utilizes |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102352302A (en) * | 2011-10-13 | 2012-02-15 | 江苏恒顺醋业股份有限公司 | Heating device for frying pan |
| CN206995905U (en) * | 2017-06-06 | 2018-02-13 | 南昌金轩科技有限公司 | A kind of Acetic Acid Recovering Column |
| CN110172388A (en) * | 2019-06-25 | 2019-08-27 | 江苏恒顺醋业云阳调味品有限责任公司 | A kind of pan-fried vinegar tank utilized with waste gas recovery |
| CN210367630U (en) * | 2019-06-25 | 2020-04-21 | 江苏恒顺醋业云阳调味品有限责任公司 | Fry in shallow oil vinegar jar with waste gas recovery utilizes |
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