KR100380604B1 - Method for manufacturing sprit using distillation waste - Google Patents

Abstract

PURPOSE: Provided is a method for manufacturing sprit using distillation waste, thereby reducing the cost and energy for the treatment of wastes, as well as the consumption of industrial water and the cost for the increase of the temperature of mashing water. CONSTITUTION: A method for manufacturing sprit using distillation waste comprises the steps of: liquifying the raw material of spirit, followed by saccharification, fermentation and mashing to give fermented mash; distilling the fermented mash; filtering the distillation waste using filter membrane; and recycling the filtrate as mashing water in liquefaction and saccharification processes.

Description

Manufacturing method of alcohol by reusing distillation waste liquid

[Industrial Applications]

More particularly, the present invention relates to a method for producing a high-economic-value alcohol by recycling a distillation waste liquid generated in the manufacture of alcohol.

BACKGROUND ART [0002]

The alcohol production process is one of the important fermentation processes and produces a million drums of alcohol per year in Korea. The alcohol production process of alcohol factory can be divided into brewing process and distillation process. First, the brewing process is a process from milling the raw material to making a fermentation sludge (containing 8 ~ 10% alcohol) through the process of liquification (liquefaction), saccharification and fermentation. In the distillation process, the fermentation sludge is subjected to several distillation processes to produce 95 It is the process of making alcohol products containing more than% alcohol. At this time, distillation of high temperature and high concentration occurs at the first distillation tower in the distillation process.

The characteristics of a typical distillation waste liquid according to the raw materials of the alcohol are shown in Table 1 below.

[Table 1]

Since the distillation waste liquid has a high concentration of solids and dissolved organic substances, it is difficult to effectively treat the distillation effluent by physicochemical treatment. Therefore, in most cases, anaerobic digestion (anaerobic digestion) and activated sludge In some cases, evaporative enrichment and incineration methods are being studied.

The anaerobic digestion method has been widely used for the treatment of the distillation waste liquid due to the stabilization of the wastewater and the advantage that the generated methane gas can be reused as fuel. However, when the raw materials of the alcoholic beverage industry are changed from tapioca or sweet potatoes to natto, the anaerobic digestion efficiency of the distillation effluent is greatly reduced. In order to solve this problem, it is necessary to reduce the amount of waste liquid generated (that is, to reduce the amount of alcohol produced), to add the flocculant before the distillation effluent enters the anaerobic digestion process, or to dilute the pre- It is true. However, these measures are problematic in that the anaerobic digester is excessively volumetric, the cost of dilute water and the cost of chemicals are increased.

In general, the activated sludge process is used for the secondary treatment of the primary treated distillation waste liquid or for the complete aerobic treatment of the distillation waste liquid not subjected to the primary treatment. Since the activated sludge process generates a considerable amount of waste sludge after the distillation waste liquid treatment, it has to be treated separately.

In order to effectively treat distillation pellets which have a considerably high concentration of organic matter, most of the alcohol factories currently use anaerobic digestion as the primary treatment and anaerobic treatment and aerobic treatment using the activated sludge as the secondary treatment. The wastewater treatment process of most of the state-of-the-art factories will now be described with reference to FIG. The distillation wastewater generated during the manufacture of alcohol is separated into a large particle by a screw decanter (9), an anaerobic digestion process (11 '), an activated sludge process (14') and a chemical flocculation and precipitation process (16 ' And discharges it. The above-mentioned wastewater treatment process has a problem that not only the problems of the anaerobic digestion method and the activated sludge method but also the wastewater treatment process site and treatment facility become large. In addition, since the energy required for the wastewater treatment process occupies 20-30% of the energy required for the entire spirits production process, there are many problems in the efficient use of energy.

Also, in the known method of producing alcohol, whenever a series of processes for producing the alcohol are carried out, the industrial water is re-supplied and used as the soaking water for the liquefaction process. In this case, the industrial water used is enormous. Therefore, an effective method of using the industrial water has been proposed.

It is an object of the present invention to solve the above-mentioned problems, and an object of the present invention is to provide a method and apparatus for recycling a distillation waste generated in a manufacturing process of a drinking water, The present invention aims to provide an economical method for manufacturing a spirits, which can greatly reduce site, facilities, and costs, and can significantly reduce the cost of heating up the soaking water and the amount of industrial water at the time of manufacturing the spirits.

FIG. 1 is a view showing a process of manufacturing a syringe according to an embodiment of the present invention.

FIG. 2 is a process chart showing a conventional preparation of a alcohol and a treatment of a distillation waste liquid. FIG.

3 is a process diagram of a membrane separation apparatus according to an embodiment of the present invention.

4 is a graph showing changes in flux according to pH at the time of the membrane separation process.

Description of the Related Art [0002]

1: raw material 2: crushing process 3: increase (liquefaction) process

4: Industrial water 5: Saccharification process 6: Fermentation process

7: distillation process 8: product (alcohol) 9: particle removal process

10: particle cake 11: membrane separation device 12: membrane separation filtrate

13: membrane separation concentrated water 11 ': anaerobic digestion tank 12': sedimentation tank

13 ': Carrier sludge 14': Activated sludge tank 15 ': Carrier sludge

16 ': First settling tank 17': Second settling tank 18 ': Discharged water

21: feed liquid 22: pump 23: inlet side pressure gauge

24: Membrane device 25: Pressure gauge on the outlet side 26: Pressure regulating valve

27: Filtration water control valve 28: Filtration water discharge valve 29: Filtration water

[MEANS FOR SOLVING THE PROBLEMS]

In order to accomplish the above object, the present invention provides a method for producing a fermentation product, which comprises a liquefaction process for liquefying a raw material of a raw material, a saccharification process and a fermentation process, a brewing process for producing a fermentation sludge, a distillation process for distilling the fermentation sludge, There is provided a method for preparing a spirit by reusing a distillation waste liquid comprising a membrane separation step of filtrating a waste solution using a filtration membrane and a step of re-introducing the filtrate obtained in the membrane separation step as a soaking water in the liquefaction step and / or the saccharification step .

The membrane separation process is preferably microfiltration or ultrafiltration. The cut-off molecular weight of the filtration membrane is preferably 10,000 to 50,000 daltons. It is preferable that the separation membrane is a ceramic membrane and that the ceramic membrane is selected from the group consisting of silicium carbide, zirconium dioxide (ZrO ₂ ), aluminum oxide (Al ₂ O ₃ ), and carbon . The membrane separation step preferably has a temperature of 50 to 80 DEG C, a flow rate of 1 to 6 m / sec, and a pressure of 1 to 6 atm. The distillation waste liquid preferably has a pH of 2 to 5 and a temperature of 60 to 80 ° C. It is preferable to adjust the pH to 5 to 8 before the filtered water is introduced into the liquefaction process and / or the saccharification process.

[Action]

The process of manufacturing a syrup by reusing the distillation waste liquid according to the present invention will be described with reference to the process drawing of FIG. After the raw material is pulverized (2), the industrial water (4) is added to carry out the liquefaction process (3), and the aging process is carried out through the saccharification process (5) and the fermentation process (6) Manufacture of spirits. The distillation wastewater generated in the distillation step is introduced into a particle removal device 9 such as a known screw decanter to remove large particles and then introduced into a membrane separation step 11 to remove the concentrate 13 and permeate And the concentrated water 13 is recirculated to the particle removing device 9 so as to be separated together with the large particles and the filtered water 12 which maintains a high temperature is separated into the dipping water .

The separation membrane may be any conventional separation membrane, but it is preferable to use a ceramic material which is suitable for application to a distillation waste liquid having a high temperature and a low pH and a high pressure, and a polymer separation membrane may also be used. Silicon carbide, zirconium dioxide, aluminum oxide, carbon and the like can all be used as a material of the ceramic membrane. Microfiltration or ultrafiltration can be used as the filtration method depending on the characteristics of the distillation waste liquid. The pore size of the membrane is effective for the ultrafiltration membrane, but a microfiltration membrane may be used. In the case of an ultrafiltration membrane having a fractional molecular weight of less than 10000 daltons, there is a problem in that the membrane is frequently washed due to the decrease of the flux due to clogging of the separation membrane. However, the fractional molecular weight of 10000 to 50000 daltons is similar to the water quality of the filtrate It is possible to reduce clogging of the membrane while giving a result. In the case of microfiltration membranes, organics smaller than the pore size may be recycled and enter the fermentation process, which may adversely affect the next fermentation process. At this time, it is preferable that the operating condition of the membrane separation apparatus is 60 ° C or higher and the pressure is 1-6 atmospheres.

When the filtered water generated in the membrane separation step is used as the soaking water in the liquefaction and / or glycation process, the pH of the soaking water greatly affects the liquefaction and the saccharification efficiency. Therefore, it is necessary to adjust the pH. It is preferable to adjust the pH to at least 6.5 so that it is poured into the above-mentioned immersion water.

In addition, since the filtration efficiency of the distillation wastewater and the appropriate temperature of the wastewater are 95 ° C in terms of energy, it is advantageous to filtrate the distillation wastewater at a high temperature in order to increase the efficiency of reusing the wastewater.

[Example]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The following will describe preferred embodiments in order to facilitate understanding of the present invention. However, it should be understood that the following examples are provided for a better understanding of the present invention, but the present invention is not limited to the following examples.

Example 1

Nutrient was used as a raw material of the alcoholic beverages, and the mixture was subjected to distillation process by grinding, liquefaction, saccharification and fermentation. After the distillation step was performed, a distillation waste liquid having a pH of 3.5 was obtained. The distillation waste liquid was introduced into the membrane separation step shown in Fig. The feed liquid (distillation waste liquid) 21 introduced into the membrane separation step was guided to the membrane separation device 24 and filtered to obtain filtered water 29. The membrane separation apparatus used was a Tech-Sep tubular module. The supporting layer of the filtration membrane was made of carbon and the skin layer was made of zirconium dioxide (ZrO ₂ ) The ultrafiltration method with a molecular weight of 20,000 daltons was used. Filtration conditions of the distillation waste liquid were 50 to 80 캜, flow rate of 1 to 6 m / sec, and permeation pressure of 1 to 6 atm. The filtered water produced in the above membrane separation step was adjusted to pH 6.5 and reused as a soaked water in the liquefaction process to prepare the alcohol.

Example 2

Example 1 was carried out in the same manner as in Example 1, except that the filtered water produced in the membrane separation step was adjusted to pH 5.5.

Example 3

In Example 1, the distillation waste liquid was adjusted to pH 6.5, and the filtrate was added to a membrane separation process. The resulting filtrate was charged into the liquor of the liquefaction process without adjusting the pH.

Comparative Example 1

Nutrient was used as a raw material of the alcoholic beverages, and the mixture was subjected to distillation process by grinding, liquefaction, saccharification and fermentation. The same procedures as in Example 1 were carried out except that the distillation waste liquid generated after the above distillation step was subjected to wastewater treatment and industrial water (pH 7.2 to 7.4) was used as the immersion water for the liquefaction process.

Comparative Example 2

The procedure of Example 1 was repeated, except that the distillation waste solution in Example 1 was adjusted to pH 6.5 without adding it to the membrane separation step and then added with immersion water.

Table 2 and Table 3 show the saccharification efficiency and the alcohol production efficiency according to the examples and comparative examples.

[Table 2]

The saccharification efficiency according to the pH of Examples 1 and 2 and Comparative Example

As can be seen from the above Table 2, it was found that pH of the immersion water greatly influences the liquefaction and saccharification efficiency when the distillation waste liquid was reused, and it is understood that more preferable saccharification is achieved when the pH is maintained at 6.5.

[Table 3]

The alcohol production efficiency of the fermentation process according to the kinds of the immersion liquids in the liquefaction processes of Examples 1 and 3 and Comparative Example

As can be seen from the results of Table 3, in Example 3, the alcohol yield was remarkably lowered at the alcohol fermentation time according to the fermentation time of 60 hours, which was the normal fermentation time, but the alcohol yield was lowered relatively in Example 1. This means that, when the distillation waste solution is reused as it is, the component which adversely affects the alcohol fermentation is considerably contained. However, when the distillation waste solution is treated with the separation membrane and reused, the components that adversely affect the alcohol fermentation can be substantially removed . In Example 1, the time for obtaining the final final ethanol yield of 87 to 90% is significantly different from that in Example 3. When the fermentation time is prolonged as described above, not only the lag time required for the growth of the microorganism is prolonged but also the fermentation rate is decreased. Therefore, the reuse of the distillation waste liquid is economically disadvantageous. The longer fermentation time is believed to be due to the fact that the organic matter present in the distillation wastewater flows into the fermentation process in the next step to inhibit yeast growth and fermentation. When the distilled waste solution of Example 1 was filtered through a filtration membrane and the filtered water was used as immersion water, only a slight decrease in the yield of alcohol was observed as compared with Example 3. As a result of the experiments conducted by the present inventors, when the filtrate was reused up to 8 times, the ethanol yield was decreased by 0.2% on average compared to the normal fermentation, but the fermentation process could be maintained stably. This indicates that the fermentation time delay was significantly reduced compared to the case of using the distillation wastewater without filtration and that the fermentation time delay was maintained within a certain range rather than gradually increasing as the filtration water reuse was repeated. This is because when the distillation wastewater is treated with a filtration membrane, the polymer organic substances that inhibit the fermentation are removed by the separation membrane, thereby inhibiting the cell growth or inhibiting the fermentation degree. Therefore, the water quality of the filtration water can be stably maintained, It is because.

The change in flux according to pH at the time of the membrane separation process of Example 1 and Example 3 was measured at a flow rate of 2.35 m / sec, a pressure of 1.4 bar and a temperature of 65 캜 using Membrane M8 (50 Kdalton) Respectively. When the pH was adjusted to 6.5 before the membrane separation process, the flux as the initial filtration capacity was high. However, since the membrane was contaminated with time, there was a problem that the flux as the filtration ability was lowered. However, In the case of performing the process, the flux as the filtration ability increased. Therefore, it can be seen that it is preferable to adjust the pH to 6.5 or more by adjusting pH after the membrane separation process.

The present invention reuses the distillation waste liquid generated in a distillation process as a soaked water in a liquefaction process and / or a saccharification process, so that the amount of wastewater generated is remarkably reduced and the amount of wastewater such as current anaerobic digestion, activated sludge, flocculation, The present invention provides an economical method for producing a spirulina that can reduce the total cost and energy consumed in the process without the need for wastewater treatment process sites and facilities. In addition, by reusing high-temperature filtered water as immersion water, it is possible to reduce the energy required for raising the temperature to 95 ° C, which is an appropriate temperature of immersion water when industrial water is used as immersion water, and the use of industrial water The effect can be remarkably reduced.

Claims (8)

The liquefaction process, the saccharification process and the fermentation process, A brewing process for preparing a ripening soup; A distillation step of distilling the aged sludge; A membrane separation step of filtering the distillation waste liquid generated in the distillation step using a filtration membrane; A step of re-introducing the filtered water obtained in the membrane separation step as a soaking water in the liquefaction step and / or the saccharification step; Wherein the distillation waste liquid is recycled. The method according to claim 1, wherein the membrane separation step is reusing a distillation waste liquid which is microfiltration or ultrafiltration. The method according to claim 1, wherein the fractionated molecular weight of the filtration membrane is 10000 to 50000 daltons. The method of claim 1, wherein the separation membrane is a ceramic membrane. 5. The method according to claim 4, wherein the ceramic film is selected from the group consisting of silicium carbide, zirconium dioxide, aluminum oxide and carbon. The method according to claim 1, wherein the membrane separation step is a method of reusing a distillation waste liquid having a temperature of 50 to 80 캜, a flow rate of 1 to 6 m / sec, and a pressure of 1 to 6 atm. The method according to claim 1, wherein the distillation waste liquid has a pH of 2 to 5 and a temperature of 60 to 80 ° C. The method according to claim 1, wherein the distilled waste liquid having a pH of 5 to 8 is reused before the filtered water is introduced into the liquefaction process and / or the saccharification process.