CN116425293A - Resource utilization method of pit bottom water in Maotai-flavor liquor production - Google Patents

Resource utilization method of pit bottom water in Maotai-flavor liquor production Download PDF

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CN116425293A
CN116425293A CN202310422773.8A CN202310422773A CN116425293A CN 116425293 A CN116425293 A CN 116425293A CN 202310422773 A CN202310422773 A CN 202310422773A CN 116425293 A CN116425293 A CN 116425293A
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bottom water
pit bottom
maotai
production
water
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周小农
张迪
张琴
代吉华
顾富宽
杜家绪
王文涛
唐启
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Henan Junhe Environmental Protection Technology Co ltd
Guizhou Maotai Distillery Group Circular Economy Industry Investment And Development Co ltd
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Henan Junhe Environmental Protection Technology Co ltd
Guizhou Maotai Distillery Group Circular Economy Industry Investment And Development Co ltd
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Priority to CN202311305595.7A priority patent/CN117550992A/en
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Abstract

The invention belongs to the field of treatment of white spirit production wastewater, and particularly relates to a method for recycling pit bottom water in Maotai-flavor white spirit production. The resource utilization method comprises the following steps: (1) Reacting ammonium bicarbonate with organic acid in the pit bottom water to generate pit bottom water containing organic ammonium salt; (2) Rectifying and separating the pit bottom water obtained in the step (1) to obtain ethanol fraction and rectifying residual liquid; (3) Evaporating and separating the rectification residual liquid to obtain concentrated solution containing amino acid. The recycling method of the pit bottom water in the production of the Maotai-flavor white spirit reduces the heat-sensitive solidification and denaturation degree of protein in the subsequent evaporation and concentration process section, reduces the loss of total amino acid quantity, neutralizes acidity, and reduces the corrosion resistance requirement of rectification and evaporation equipment; the ethanol fraction and the concentrated solution containing amino acid are respectively recovered, thereby realizing the comprehensive utilization of the water resource at the bottom of the cellar, reducing the burden of a sewage treatment system and being suitable for popularization and application of white spirit production enterprises.

Description

Resource utilization method of pit bottom water in Maotai-flavor liquor production
Technical Field
The invention belongs to the field of treatment of white spirit production wastewater, and particularly relates to a method for recycling pit bottom water in Maotai-flavor white spirit production.
Background
The Maotai-flavor liquor is prepared from cereal grains as main raw material by solid or semi-solid saccharification, fermentation, distillation to obtain base liquor, aging, and blending to obtain the final product liquor. The fermentation period of fermented grains is long in the production process of the Maotai-flavor white spirit, and percolate generated by fermenting the fermented grains in the pit, namely pit bottom water (also called yellow water), has the concentration of organic matters, nitrogen, phosphorus and other substances which are remarkably high in the pit bottom water, namely Yu Nong-flavor and faint scent type white spirit production pit bottom water. The quality index of the pit bottom water of the Maotai-flavor liquor production enterprise is as follows: the pH is 3-5, the total organic matter is 80-180g/L, the total nitrogen is 3.5-6.0g/L, the ammonia nitrogen is 1.5-3.0g/L, the total amino acid amount is 15-30g/L, wherein the nitrogen-containing compound is ammonium salt, free amino acid and protein, the amino acid is complete in variety (comprising 17 amino acids of aspartic acid, glutamic acid, proline, alanine, lysine, leucine, serine, arginine, glycine, threonine, valine, isoleucine, phenylalanine, histidine and the like), the total phosphorus is 0.8-3.0g/L, the total nutrient (N+P) 2 O 5 +K 2 O) is more than 10g/L, and the ethanol content is 2-5%.
The basic characteristics of the brewing process of Maotai-flavor liquor "12987", namely 1 year production period, 2 times of feeding, 9 times of steaming, 8 times of fermentation and 7 times of liquor taking, cause the obvious difference of the quality of the pit bottom water in different production stages. The traditional treatment mode of the pit bottom water is that the pit bottom water is used as production wastewater, and is mixed with the pit bottom water, workshop and equipment flushing water, bottle washing water, cooling tower sewage and the like and then is sent to a sewage treatment system for treatment, and as the pit bottom water has high organic matter, nitrogen and phosphorus content and large fluctuation along with the production period, the pit bottom water has complex components, the drainage after treatment is designed according to the concentration peak value of the organic matter, nitrogen and phosphorus to ensure that the drainage after treatment stably reaches the standard, a large amount of capital investment is consumed, a large amount of chemical agents and energy are consumed in the treatment process, and the treatment cost is high.
The pit bottom water contains low-boiling-point organic matters such as alcohol, ester, acid and aldehyde, and also contains rich sugar, protein, humic acid, amino acid, macromolecular organic matters and the like, so that the pit bottom water is rich in nutrient species, has extremely high resource utilization value, and is used as wastewater treatment to increase the burden of a sewage treatment system, is difficult to treat and reaches the standard, and also causes the waste of resources.
Disclosure of Invention
The invention aims to provide a method for recycling pit bottom water in the production of Maotai-flavor liquor, which solves the problems that the pit bottom water is directly treated as wastewater, the burden of a sewage treatment system is increased, the resource waste is caused and the like in the prior art.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the method for recycling the pit bottom water in the production of the Maotai-flavor white spirit comprises the following steps:
(1) Reacting ammonium bicarbonate with organic acid in the pit bottom water to generate pit bottom water containing organic ammonium salt;
(2) Rectifying and separating the pit bottom water obtained in the step (1) to obtain ethanol fraction and rectifying residual liquid;
(3) Evaporating and separating the rectification residual liquid to obtain concentrated solution containing amino acid.
According to the recycling method for the pit bottom water in the production of the Maotai-flavor white spirit, ammonium bicarbonate is added into the pit bottom water to generate the organic ammonium salt amino acid protecting agent mainly containing ammonium acetate, so that proteins are protected, the heat-sensitive solidification and denaturation degree of the proteins in the subsequent evaporation and concentration process section are reduced, the loss of total amino acid is reduced, meanwhile, the acidity is neutralized, and the corrosion resistance requirements of rectification and evaporation equipment are reduced; the ethanol fraction and the concentrated solution containing amino acid are respectively recovered, thereby realizing the comprehensive utilization of the water resource at the bottom of the cellar, reducing the burden of a sewage treatment system and being suitable for popularization and application of white spirit production enterprises.
In the step (1), through the generation reaction of organic ammonium salt, the protein in the pit bottom water is protected, the heat-sensitive denaturation and solidification degree of the protein in the rectification and evaporation section is reduced, the loss of total amino acid is reduced, preferably, in the step (1), the adding amount of ammonium bicarbonate is 5-30 kg/m 3 Stirring and reacting for 40-60 min.
Preferably, in step (1), the pit bottom water is stored for no more than 3 days. Anaerobic microorganisms are arranged in the water at the bottom of the cellar, the storage time is controlled, the amount of ethanol in the water hydrolyzed into acetic acid under the action of the microorganisms can be obviously reduced, and the ethanol yield of the rectification section is improved.
The purpose of the rectification separation is to separate an ethanol fraction which can be used for wine distillation in a production plant to improve the yield of base wine. Preferably, in the step (2), the vacuum degree is-0.07 to-0.08 MPa during rectification separation, and the rectification temperature is 65 to 75 ℃; and the alcohol content of the distillate at the top of the tower is received at 55-65 degrees, and the ethanol fraction is obtained and used for steaming wine in a production workshop, so that the yield of base wine is improved.
The purpose of evaporation separation is to realize effective concentration and enrichment of amino acid, preferably, in the step (3), the vacuum degree is-0.07 to-0.09 MPa, the evaporation temperature is 50 to 90 ℃, and the concentration multiple is 3.0 to 5.0 times during evaporation separation.
Preferably, the pH value of the pit bottom water is 3-5, the total organic matters are 80-180g/L, the total nitrogen is 3.5-6.0g/L, the ammonia nitrogen is 1.5-3.0g/L, the total amino acid amount is 15-30g/L, the total phosphorus is 0.8-3.0g/L, the total nutrients are more than 10g/L, and the ethanol content is 2-5%.
On the basis, a concentrated solution rich in amino acids and total nutrients and a condensate suitable for anaerobic fermentation can be obtained by evaporation separation, preferably, in the step (3), the concentrated solution and the condensate are obtained by evaporation separation; in the concentrated solution, the organic matter content is more than 300g/L, the total nutrient is more than 60g/L, and the total amino acid content is more than 70g/L; in the condensate liquid, COD is 10000-40000 mg/L, ammonia nitrogen is less than 20mg/L, total nitrogen is less than 50mg/L, and total phosphorus is less than 10mg/L.
In order to further improve the added value of the product of the concentrated solution containing the amino acid, preferably, the concentrated solution containing the amino acid is used for preparing an organic water-soluble fertilizer, and the organic water-soluble fertilizer comprises the following components in parts by weight: 994-1000 parts of concentrated solution, 1-2 parts of potassium fulvate, 0.1-0.3 part of polyethylene glycol and 2-4 parts of EDTA.
In order to further realize the recycling of condensate, preferably, in the step (3), the concentrated solution and the condensate are obtained through evaporation and separation, and the condensate is subjected to anaerobic fermentation to produce methane.
Further preferably, the biogas produced is used for producing steam for a gas boiler, and the steam produced is used as heat energy for the rectification section in step (2) and the evaporation section in step (3). By utilizing the mode, the resource utilization of methane can be realized, and the energy consumption of the rectification and evaporation section can be reduced.
In a comprehensive view, compared with the existing method for disposing the pit bottom water of the Maotai-flavor white spirit production enterprise, the method has the following beneficial effects:
(1) After the pit bottom water is collected independently, ammonium bicarbonate is added to generate an organic ammonium salt protective agent mainly containing ammonium acetate, so that the loss of nutrient substances in the pit bottom water is reduced, the corrosion resistance requirements of materials of rectification and evaporation equipment are reduced, and the equipment investment is saved.
(2) The ethanol recovered by rectification is used for improving the yield of base wine, and the concentrated solution is used as a raw material for producing organic water-soluble fertilizer, thereby creating additional economic value for enterprises;
(3) Evaporating condensate to produce methane by anaerobic fermentation, and using the methane as heat energy for rectification and evaporation sections to realize 'clean and recycling' of pit bottom water;
(4) The invention provides a process for recycling pit bottom water of a Maotai-flavor liquor production enterprise, which realizes resource recovery, reduces the difficulty of pit bottom water treatment and has the advantages of reasonable route, low investment cost, stable and reliable operation and the like.
Drawings
Fig. 1 is a process flow diagram for recycling pit bottom water of a Maotai-flavor liquor enterprise.
Detailed Description
The pit bottom water produced in pit in the production process of Maotai-flavor liquor contains saccharides, rich amino acids, nitrogen, phosphorus, potassium, various organic acids mainly including acetic acid, alcohols mainly including ethanol, various esters and other substances which can be used as resources. When the wastewater is used for wastewater treatment, the burden of a sewage treatment system is increased, the wastewater is difficult to treat and reaches the standard, and the waste of resources is caused.
If the method of evaporation concentration recycling is adopted for recycling, the problem of temperature solidification denaturation of nutrients such as amino acid in pit bottom water in the concentration process and reduced nutritive value exists. The pit bottom water of certain Maotai-flavor liquor production enterprises adopts evaporation concentration to enrich nutrients, the concentration multiple is 3.5 times, the contents of various amino acids in the stock solution before and after concentration and the evaporation concentration solution are shown in table 1, and the amino acid loss during the evaporation concentration process is 32.78%.
TABLE 1 amino acid content before and after Evaporation concentration of pit bottom Water in Soy sauce-flavor liquor production enterprises
Figure BDA0004188910310000031
Figure BDA0004188910310000041
The invention provides a process for recycling pit bottom water of a Maotai-flavor white spirit production enterprise according to the component characteristics of the pit bottom water. The invention adopts the processes of separately collecting pit bottom water, adding ammonium bicarbonate, rectifying and recovering ethanol and evaporating and separating; rectifying the recovered ethanol for improving the yield of the base wine in a production workshop; evaporating the concentrated solution to be used as the raw material of the organic water-soluble fertilizer, and adding a certain proportion of potassium fulvate, polyethylene glycol and EDTA to produce the special organic water-soluble fertilizer; the method comprises the steps of performing anaerobic fermentation on evaporation condensate to generate clean energy biogas, using the biogas to produce steam by a gas boiler, recycling the steam as heat energy to a rectifying and evaporating section, discharging anaerobic fermentation effluent into a sewage treatment system, and treating the sewage together with bottom water and other low-concentration production wastewater discharged in brewing production. At this time, the effluent can meet the direct discharge standard of Table 3 of the emission standard of industrial water pollutants for fermented alcohol and white spirit (GB 27631-2011) by adopting a conventional wastewater treatment flow.
The invention further provides a process for recycling pit bottom water of a Maotai-flavor liquor production enterprise, and the process flow chart is shown in figure 1 and comprises the following steps:
(1) The pit bottom water is singly collected and then enters a storage tank for storage, is pumped to a stirring tank, and is added with ammonium bicarbonate to react with organic acid in the pit bottom water to generate organic ammonium salt mainly containing ammonium acetate, so that protein in the pit bottom water is protected, the heat-sensitive denaturation and solidification degree of protein in a rectification and evaporation section is reduced, and the total amino acid loss is reduced;
(2) Recovering low boiling point substances which are mainly ethanol in the water at the bottom of the cellar by adopting a rectifying device, and steaming wine in a production workshop;
(3) Evaporating and secondarily separating the bottom solution of the rectifying still to obtain condensate and concentrated solution;
(4) The evaporating concentrated solution is used as the raw material for producing the organic water-soluble fertilizer, and a certain proportion of potassium fulvate, polyethylene glycol and EDTA are added to produce the special organic water-soluble fertilizer.
(5) The condensate is evaporated for anaerobic fermentation to produce methane, the methane is used for producing steam by a gas boiler and used as heat energy for rectification and evaporation sections, anaerobic fermentation effluent is discharged into a sewage treatment system, and the sewage is treated with bottom water discharged in brewing production and other low-concentration production wastewater.
Wherein, the pit bottom water of the soy sauce type white spirit production enterprise is percolate generated in the fermentation process of soy sauce type white spirit production fermented grains, and the water quality indexes are as follows: the pH is 3-5, the total organic matter is 80-180g/L, the total nitrogen is 3.5-6.0g/L, the ammonia nitrogen is 1.5-3.0g/L, the total amino acid amount is 15-30g/L, wherein the nitrogen-containing compound is ammonium salt, free amino acid and protein, the amino acid is complete in variety (comprising 17 amino acids of aspartic acid, glutamic acid, proline, alanine, lysine, leucine, serine, arginine, glycine, threonine, valine, isoleucine, phenylalanine, histidine and the like), the total phosphorus is 0.8-3.0g/L, the total nutrient (N+P2O5+K2O) is more than 10g/L, and the ethanol content is 2-5%.
After the pit bottom water is treated in the steps (1), (2) and (3), recovering low boiling point components mainly comprising ethanol to obtain concentrated solution and condensate, and treating the concentrated solution and the condensate in the steps (4) and (5) to realize the recycling of the pit bottom water with high added value and reduce environmental pollution.
In the step (1), the pit bottom water is singly collected by adopting a food-grade stainless steel storage tank and pumped to a stirring reaction tank, and ammonium bicarbonate is added under the control conditions that: the storage time is not longer than 3 days, and the addition amount of ammonium bicarbonate is 5-30 kg/m 3 Mechanical stirring time is 40-60 min; anaerobic microorganisms are arranged in the water at the bottom of the cellar, the storage time is controlled, the amount of ethanol in the water hydrolyzed into acetic acid under the action of the microorganisms can be obviously reduced, and the ethanol yield of the rectification section is improved. The pit bottom water is acidic, contains various organic acids mainly containing acetic acid, and is added with ammonium bicarbonate to react with the organic acids in the pit bottom water to generate organic ammonium salt mainly containing ammonium acetate, so that protein in the pit bottom water is protected, the heat-sensitive denaturation and solidification degree of protein in a rectification and evaporation section is reduced, meanwhile, the acidity is neutralized, the corrosion resistance requirement of rectification and evaporation equipment is reduced, SUS304 materials with the cost greatly reduced relative to titanium materials or 2205 duplex stainless steel can be adopted as main materials of the evaporation equipment, and the construction investment is saved.
Under the working condition that the liquid phase temperature is higher than 65 ℃, the protein is subjected to heat-sensitive denaturation and solidification, so that the nutritive value of the concentrated solution is reduced, ammonium bicarbonate is added in the step (1), an organic ammonium salt protective agent mainly containing ammonium acetate is generated by reaction, the denaturation and solidification degree of the protein under the high-temperature working condition is reduced, and the loss amount of amino acid before and after rectification and evaporation is reduced to be within 10%.
In the step (2), a rectifying device is adopted to recycle low boiling point substances which are mainly ethanol in the pit bottom water and are used for steaming wine in a production workshop. The control conditions of the rectifying device are as follows: preheating the materials to 45-55 ℃, then entering a rectifying device, wherein the vacuum degree of the rectifying device is minus 0.07-minus 0.08MPa, the rectifying temperature is 65-75 ℃, the alcohol content of distillate is 55-65 ℃, and the appearance is clear and transparent; the material of the part of equipment contacted with the material and the secondary steam is food grade stainless steel; the materials are preheated in a gradient heating way, so that foam generated by the rapid heating of the materials is avoided, the impurity content in distillate is reduced, the alcoholic strength of the distillate is controlled to be 55-65 degrees, the distilled liquor is used for steaming wine in a production workshop, and the yield of base liquor is improved.
In the step (3), the secondary separation is carried out on the bottom liquid of the rectifying still in the step (2) by adopting an evaporation device (such as an MVR evaporator, a multi-effect evaporator, a TVR evaporator and the like), and the control conditions are as follows: the vacuum degree is-0.07 to-0.09 MPa, the evaporation temperature is 55-90 ℃, the concentration multiple is 3.0-5.0 times, and the specific gravity of the finished product is 1.15-1.35, so the product has fluidity. The steam is used as heat energy to evaporate and separate the bottom liquid of the rectifying still, and the organic matters, nitrogen, phosphorus, potassium nutrients, amino acids and other nutrients in the water are enriched in the concentrated solution, and other organic matters and water are separated in the form of evaporating condensate.
The condensate water quality index generated in the step (3) is as follows: COD is 10000-40000 mg/L, ammonia nitrogen is less than 20mg/L, total nitrogen is less than 50mg/L, and total phosphorus is less than 10mg/L; the pH is 6.0-6.5.
In the step (4), the organic matter content of the evaporating concentrated solution is more than 300g/L, and the total nutrient (N+P) 2 O 5 +K 2 O) is more than 60g/L, the total amount of amino acid is more than 70g/L, the water insoluble substance is less than 10g/L, and the heavy metal content is lower than the limit requirement of mercury, arsenic, cadmium, lead and chromium of water soluble fertilizer (NY 1110-2010), and the water soluble fertilizer is used as the raw material for producing the organic water soluble fertilizer, and potassium fulvate, polyethylene glycol and EDTA are added to produce the special organic water soluble fertilizer, wherein the adding proportion is as follows by weight: 994-1000 parts of concentrated solution, 1-2 parts of potassium fulvate, 0.1-0.3 part of polyethylene glycol and 2-4 parts of EDTA.
In general, the evaporative concentrate may achieve the following criteria: the organic matter content is 350-450 g/L, and the total nutrient (N+P) 2 O 5 +K 2 O) 62-70 g/L and 75-85 g/L of total amino acid.
In the step (5), evaporating condensate for anaerobic fermentation, wherein the control conditions are as follows: the temperature is 30-37 ℃, the continuous fermentation process is adopted, the fermentation time is 3-4 days, the pH of the inlet water is 6.0-6.5, and the reactor type adopts an internal circulation anaerobic reactor or an upflow anaerobic sludge blanket reactor. COD removal rate of evaporated condensate in anaerobic fermentation process is 90% -95%, and biogas yield is 0.45-0.50Nm 3 And (3) the COD (chemical oxygen demand) of the anaerobic fermentation effluent is smaller than 2000mg/L, and the effluent is discharged into a sewage treatment system to be combined with bottom water and other low-concentration production wastewater for treatment.
The following describes the practice of the invention in detail with reference to specific examples.
Example 1
The method for recycling pit bottom water in Maotai-flavor liquor production of this embodiment takes the Guizhou-flavor liquor production enterprise as an example, and the enterprise daily produces pit bottom water of 200m 3 The water quality is as follows: 150g/L of total organic matters, 2.5g/L of ammonia nitrogen, 5.8g/L of total nitrogen, 2.7g/L of total phosphorus, pH3.5 and total nutrient (N+P) 2 O 5 +K 2 O) 15.60g/L, total amino acid amount 27.77g/L, ethanol content 4.8%, and amino acid content in water as shown in Table 2.
Table 2 example 1 amino acid content (Unit: g/L) in pit bottom water of Guizhou Maotai-flavor liquor manufacturing enterprises
Asparagin acid Arginine (Arg) Proline (proline) Methionine Lysine Glutamic acid
1.91 0.74 2.62 0.24 1.36 9.39
Glycine (Gly) Alanine (Ala) Cystine (cystine) Phenylalanine (Phe) Tryptophan Serine (serine)
1.47 2.41 0.18 0.72 0.17 1.03
Threonine (Thr) Valine (valine) Isoleucine (Ile) Leucine (leucine) Histidine Tyrosine
1.04 1.22 0.89 1.26 0.75 0.37
The method for recycling the pit bottom water comprises the following steps:
(1) The pit bottom water is singly collected to a stainless steel storage tank, and the storage time is 2 days.Pumping the pit bottom water to a stainless steel stirring tank, and adding 30kg/m ammonium bicarbonate 3 Stirring for 60min, and ending the reaction.
In the step, the pit bottom water is collected independently, a storage tank is made of corrosion-resistant food-grade materials, the storage time of the pit bottom water is not longer than 3 days, and ethanol in the pit bottom water is prevented from being fermented and converted into acetic acid; and then pumping the mixture to a stirring reaction tank, adding ammonium bicarbonate, and reacting the ammonium bicarbonate with organic acid in the pit bottom water to generate organic ammonium salt mainly containing ammonium acetate, so as to protect protein in the pit bottom water, reduce the heat-sensitive denaturation and solidification degree of protein in the rectification and evaporation section, reduce the total amino acid loss, and simultaneously raise the pH value of the pit bottom water and reduce the corrosion resistance requirements of materials of rectification and evaporation equipment.
(2) The feed liquid added with ammonium bicarbonate is pumped to a rectifying section, is heated to 48 ℃ through a heat exchanger, enters a rectifying tower, has the vacuum degree of-0.08 MPa, has the rectifying temperature of 68 ℃, has the distillate alcohol degree of 60 DEG, the methanol content of less than 0.2g/L, has lead undetected, has the daily distillate output of 13.80t, and is used for distilling wine in a production workshop, and the yield of base wine is improved.
By utilizing the step, the distillate which takes ethanol as a main component and contains a small amount of esters can be recovered from the cellar bottom liquid and used for steaming wine in a production workshop, and the yield of base wine is improved.
(3) The bottom liquid of the rectifying still is pumped to a five-effect evaporation device, the vacuum degree of the effect body is-0.07 to-0.09 MPa, the evaporation temperature is 85-50 ℃, and the concentration multiple is 3.2 times. The organic matter content of the concentrated solution is 400g/L, and the total nutrient (N+P) 2 O 5 +K 2 O) 65g/L, 7g/L of water insoluble matter, and amino acid content as shown in Table 3; the COD of the evaporated condensate is 35000mg/L, ammonia nitrogen is 18mg/L, total nitrogen is 25mg/L, and total phosphorus is 3mg/L.
TABLE 3 example 1 amino acid content (Unit: g/L) in a pit bottom water evaporative concentrate of a Guizhou Maotai-flavor liquor manufacturing enterprise
Asparagin acid Arginine (Arg) Proline (proline) Methionine Lysine Glutamic acid
5.81 2.16 7.77 0.71 4.03 27.65
Glycine (Gly) Alanine (Ala) Cystine (cystine) Phenylalanine (Phe) Tryptophan Serine (serine)
4.31 6.96 0.55 2.12 0.49 2.98
Threonine (Thr) Valine (valine) Isoleucine (Ile) Leucine (leucine) Histidine Tyrosine
2.96 3.60 2.61 3.65 2.12 1.10
Evaporating and concentrating the pit bottom water for 3.2 times, and then concentrating the total amount of amino acid in the concentrated solution to 81.58g/L; amino acid loss during evaporation concentration was 8.20%.
(4) The evaporating concentrated solution is used as the raw material for producing the organic water-soluble fertilizer, and the potassium fulvate, the polyethylene glycol and the EDTA are added to produce the special organic water-soluble fertilizer. The weight ratio is as follows: 994.80kg of evaporation concentrate, 2.00kg of potassium fulvate, 0.20kg of polyethylene glycol and 3.00kg of EDTA3.
(5) The evaporated condensate is cooled by a heat exchanger and then pumped to an up-flow anaerobic sludge blanket fermentation device for anaerobic fermentation, the anaerobic fermentation time is 4.0d, the temperature is 30 ℃, and the anaerobic fermentation COD removal rate is 90%. The biogas generated by anaerobic fermentation enters a gas boiler to produce steam, the steam yield is 16.80t/d at 0.8MPa, the steam is used as heat energy for a rectification and evaporation section, and the heat energy is saved by 42% compared with the whole use of fresh steam. Anaerobic fermentation effluent is mixed with boiler bottom water and other low-concentration production wastewater discharged by enterprises, and the process treatment of pretreatment, anaerobism, aerobiotic and advanced treatment is adopted, wherein the effluent meets the direct discharge standard of the wastewater pollutants in the fermented alcohol and white spirit industry (GB 27631-2011) in table 3.
Example 2
The method for recycling pit bottom water in Maotai-flavor liquor production of this embodiment is exemplified by a Sichuan certain Maotai-flavor liquor production enterprise which produces 120m pit bottom water daily 3 The water quality is as follows: 115g/L of total organic matters, 2.2g/L of ammonia nitrogen, 5.0g/L of total nitrogen, 2.2g/L of total phosphorus, pH3.8 and total nutrient (N+P) 2 O 5 +K 2 O) 14.50g/L, total amino acid 2418g/L, ethanol content 4.1%, and amino acid content in water as shown in Table 4.
TABLE 4 example 2 Sichuan Maotai-flavor liquor production enterprises pit bottom water amino acid content (unit: g/L)
Asparagin acid Arginine (Arg) Proline (proline) Methionine Lysine Glutamic acid
2.15 0.52 2.58 0.26 1.51 6.67
Glycine (Gly) Alanine (Ala) Cystine (cystine) Phenylalanine (Phe) Tryptophan Serine (serine)
0.92 1.55 0.21 0.57 0.15 0.97
Threonine (Thr) Valine (valine) Isoleucine (Ile) Leucine (leucine) Histidine Tyrosine
0.77 1.34 0.93 1.88 0.62 0.58
The method for recycling the pit bottom water comprises the following steps:
(1) Separately collecting the pit bottom water into a storage pool for 2 days, pumping into a stirring tank, and adding 15kg/m ammonium bicarbonate 3 The reaction was stirred for 50min and ended.
(2) The feed liquid added with ammonium bicarbonate is pumped to a rectifying tower, and is primarily heated to 45 ℃ through a heat exchanger, the vacuum degree of the rectifying tower is-0.078 MPa, the rectifying temperature is 70 ℃, the alcoholic strength of distillate is 58 degrees, the methanol content is less than 0.2g/L, lead is not detected, the daily yield of the distillate is 7.6t, and the feed liquid is used for steaming wine in a production workshop and improving the yield of base wine.
(3) The bottom liquid of the rectifying still is pumped to an MVR evaporation device, the vacuum degree of the evaporation device is controlled to be-0.085 MPa, the evaporation temperature is 85 ℃, and the concentration multiple is 3.8 times. The organic matter content of the concentrated solution is 410g/L, and the total nutrient (N+P) 2 O 5 +K 2 O) 62g/L, water insoluble matter 6.5g/L, amino acid content as shown in Table 5; COD of the evaporated condensate is 30000mg/L, ammonia nitrogen is 16mg/L, total nitrogen is 22mg/L, and total phosphorus is 2mg/L。
TABLE 5 example 2 amino acid content (unit: g/L) in a pit bottom water evaporative concentrate of Sichuan certain Maotai-flavor liquor manufacturing enterprises
Figure BDA0004188910310000081
Figure BDA0004188910310000091
Evaporating and concentrating the water at the bottom of the cellar for 3.8 times, and then concentrating the water until the total amount of amino acid in the concentrated solution is 83.95g/L; amino acid loss during evaporation concentration was 8.63%.
(4) The evaporating concentrated solution is used as the raw material for producing the organic water-soluble fertilizer, and the potassium fulvate, the polyethylene glycol and the EDTA are added to produce the special organic water-soluble fertilizer. The weight ratio is as follows: 994.65kg of evaporated concentrate, 1.80kg of potassium fulvate, 0.15kg of polyethylene glycol and 3.40kg of EDTA3.
(5) The evaporated condensate is cooled by a heat exchanger and then pumped into an internal circulation anaerobic reactor for anaerobic fermentation, the anaerobic fermentation time is 3.0d, the temperature is 35 ℃, and the anaerobic fermentation COD removal rate is 92%. Biogas generated by anaerobic fermentation enters a gas boiler to produce steam, the steam quantity of 0.8MPa is 9.12t/d, and the steam quantity is used as heat energy for a rectification and evaporation section, so that the heat energy is saved by 38% compared with the whole fresh steam. Anaerobic fermentation effluent is mixed with boiler bottom water and other low-concentration production wastewater discharged by enterprises, and the process treatment of pretreatment, anaerobism, aerobiotic and advanced treatment is adopted, wherein the effluent meets the direct discharge standard of the wastewater pollutants in the fermented alcohol and white spirit industry (GB 27631-2011) in table 3.
Example 3
The method for recycling pit bottom water in Maotai-flavor liquor production of this embodiment takes Guizhou liquor production enterprises as an example, and the enterprises daily produce pit bottom water of 100m 3 The water quality is as follows: 92g/L of total organic matters, 2.0g/L of ammonia nitrogen, 4.6g/L of total nitrogen, 2.1g/L of total phosphorus, pH4.3 and total nutrient (N+P) 2 O 5 +K 2 O) 13.80g/L, total amino acid amount 18.90g/L, ethanol content 3.2%, amino acid content in waterAs shown in table 6.
TABLE 6 example 3 Guizhou Maotai-flavor liquor manufacturing enterprises pit bottom water amino acid content (unit: g/L)
Asparagin acid Arginine (Arg) Proline (proline) Methionine Lysine Glutamic acid
1.62 0.18 1.86 0.12 0.78 6.35
Glycine (Gly) Alanine (Ala) Cystine (cystine) Phenylalanine (Phe) Tryptophan Serine (serine)
1.11 1.63 0.12 0.53 0.15 0.62
Threonine (Thr) Valine (valine) Isoleucine (Ile) Leucine (leucine) Histidine Tyrosine
0.63 0.87 0.68 1.02 0.37 0.26
The method for recycling the pit bottom water comprises the following steps:
(1) Separately collecting the pit bottom water to a storage pool for 2.5 days, pumping to a stirring tank, and adding ammonium bicarbonate 8kg/m 3 The reaction was stirred for 40min and ended.
(2) The feed liquid added with ammonium bicarbonate is pumped to a rectifying tower, and is primarily heated to 47 ℃ through a heat exchanger, the vacuum degree of the rectifying tower is minus 0.08MPa, the rectifying temperature is 70 ℃, the alcohol degree of distillate is 60 ℃, the methanol content is less than 0.2g/L, lead is not detected, the daily output of the distillate is 5.4t, and the feed liquid is used for distilling wine in a production workshop and improving the output of base wine.
(3) The bottom liquid of the rectifying still is pumped to an MVR evaporation device, the vacuum degree of the evaporation device is controlled to be-0.09 MPa, the evaporation temperature is 80 ℃, and the concentration multiple is 4.5 times. The organic matter content of the concentrated solution is 385g/L, and the total nutrient (N+P) 2 O 5 +K 2 O) 63g/L, 7.5g/L of water-insoluble matter; the COD of the evaporated condensate is 32000mg/L, the ammonia nitrogen is 14mg/L, the total nitrogen is 20mg/L, the total phosphorus is 3.0mg/L, and the amino acid content is shown in Table 7.
TABLE 7 example 3 amino acid content (Unit: g/L) in a pit bottom water evaporative concentrate of a Guizhou Maotai-flavor liquor manufacturing enterprise
Asparagin acid Arginine (Arg) Proline (proline) Methionine Lysine Glutamic acid
6.86 0.74 7.67 0.49 3.22 25.87
Glycine (Gly) Alanine (Ala) Cystine (cystine) Phenylalanine (Phe) Tryptophan Serine (serine)
4.52 6.53 0.51 2.19 0.61 2.51
Threonine (Thr) Valine (valine) Isoleucine (Ile) Leucine (leucine) Histidine Tyrosine
2.53 3.58 2.74 4.07 1.48 1.02
Evaporating and concentrating the pit bottom water for 4.5 times, and then concentrating the total amount of amino acid in the concentrated solution to 77.14g/L; amino acid loss during evaporation concentration was 9.30%.
(4) The evaporating concentrated solution is used as the raw material for producing the organic water-soluble fertilizer, and the potassium fulvate, the polyethylene glycol and the EDTA are added to produce the special organic water-soluble fertilizer. The weight ratio is as follows: 1000kg of evaporated concentrate, 1.85kg of potassium fulvate, 0.10kg of polyethylene glycol and 4.00kg of EDTA4.
(5) The evaporated condensate is cooled by a heat exchanger and then pumped into an internal circulation anaerobic reactor for anaerobic fermentation, the anaerobic fermentation time is 3.5d, the temperature is 37 ℃, and the anaerobic fermentation COD removal rate is 94%. The biogas generated by anaerobic fermentation is used for producing steam by a gas boiler, the steam yield is 7.92t/d, the steam yield is 0.8MPa, the steam is used as heat energy for a rectification and evaporation section, and the heat energy is saved by 40% compared with the whole fresh steam. Anaerobic fermentation effluent is mixed with boiler bottom water and other low-concentration production wastewater discharged by enterprises, and the process treatment of pretreatment, anaerobism, aerobiotic and advanced treatment is adopted, wherein the effluent meets the direct discharge standard of the wastewater pollutants in the fermented alcohol and white spirit industry (GB 27631-2011) in table 3.
Long-term operation data show that the method for treating the pit bottom water of the soy sauce flavor type white spirit enterprises has the advantages of high recycling utilization rate, stable and reliable process and considerable additional economic benefit.

Claims (10)

1. The method for recycling the pit bottom water in the production of the Maotai-flavor white spirit is characterized by comprising the following steps of:
(1) Reacting ammonium bicarbonate with organic acid in the pit bottom water to generate pit bottom water containing organic ammonium salt;
(2) Rectifying and separating the pit bottom water obtained in the step (1) to obtain ethanol fraction and rectifying residual liquid;
(3) Evaporating and separating the rectification residual liquid to obtain concentrated solution containing amino acid.
2. The method for recycling pit bottom water in the production of Maotai-flavor liquor according to claim 1, wherein in the step (1), the addition amount of ammonium bicarbonate is 5-30 kg/m 3 Stirring and reacting for 40-60 min.
3. The method for recycling pit bottom water in the production of Maotai-flavor liquor according to claim 2, wherein in the step (1), the storage time of the pit bottom water is not more than 3 days.
4. The method for recycling pit bottom water in the production of Maotai-flavor liquor according to claim 1, wherein in the step (2), the vacuum degree is-0.07 to-0.08 MPa during rectification and separation, and the rectification temperature is 65 ℃ to 75 ℃; and the alcohol content of the distillate at the top of the tower is received at 55-65 degrees, and the ethanol fraction is obtained and used for steaming wine in a production workshop, so that the yield of base wine is improved.
5. The method for recycling pit bottom water in the production of Maotai-flavor liquor according to claim 1, wherein in the step (3), the vacuum degree is-0.07 to-0.09 MPa, the evaporation temperature is 50 to 90 ℃, and the concentration multiple is 3.0 to 5.0 times during evaporation and separation.
6. The method for recycling pit bottom water in the production of Maotai-flavor liquor according to claim 1, wherein the pH of the pit bottom water is 3-5, the total organic matter is 80-180g/L, the total nitrogen is 3.5-6.0g/L, the ammonia nitrogen is 1.5-3.0g/L, the total amino acid amount is 15-30g/L, the total phosphorus is 0.8-3.0g/L, the total nutrient is greater than 10g/L, and the ethanol content is 2-5%.
7. The method for recycling pit bottom water in the production of Maotai-flavor liquor according to claim 6, wherein in the step (3), the concentrated solution and the condensate are obtained by evaporation and separation; in the concentrated solution, the organic matter content is more than 300g/L, the total nutrient is more than 60g/L, and the total amino acid content is more than 70g/L; in the condensate liquid, COD is 10000-40000 mg/L, ammonia nitrogen is less than 20mg/L, total nitrogen is less than 50mg/L, and total phosphorus is less than 10mg/L.
8. The method for recycling pit bottom water in the production of Maotai-flavor liquor according to any one of claims 1 to 6, wherein the concentrated solution containing amino acid is used for preparing an organic water-soluble fertilizer, and the organic water-soluble fertilizer comprises the following components in parts by weight: 994-1000 parts of concentrated solution, 1-2 parts of potassium fulvate, 0.1-0.3 part of polyethylene glycol and 2-4 parts of EDTA.
9. The method for recycling pit bottom water in the production of Maotai-flavor liquor according to claim 8, wherein in the step (3), the concentrated solution and the condensate are obtained by evaporation and separation, and the condensate is subjected to anaerobic fermentation to produce biogas.
10. The method for recycling pit bottom water in the production of Maotai-flavor liquor according to claim 9, wherein the produced biogas is used for producing steam by a gas boiler, and the produced steam is used as heat energy for the rectification section in step (2) and the evaporation section in step (3).
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