Method for treating wine brewing yellow water and extracting effective components by combining micro-nano bubble microwave microfluid extraction

Abstract

The invention discloses a method for treating wine-brewing yellow water and extracting effective components by combining micro-nano bubble microwave microfluid extraction. The method comprises the following steps: (1) pretreating the wine-brewing yellow water; (2) micro-nano bubble treatment; (3) microwave treatment; (4) secondary treatment of the micro-nano bubbles; (5) microfluid extraction; (6) product recovery; and (7) waste liquid treatment. The method provided by the invention fully combines the advantages of micro-nano bubbles, microwave treatment and microfluid extraction technologies, realizes efficient treatment of the wine-brewing yellow water and recycling of useful components, has the characteristics of high treatment efficiency, good economic benefit and strong environmental protection property, and is suitable for industrial application.

Description

Technical Field

[0001] The present invention relates to the technical field of wastewater treatment and resource utilization, and in particular to a method for treating winemaking yellow water and extracting effective components through combined micro-nano bubble microwave-microfluid extraction. Background Art

[0002] Winery yellow water is a high-concentration organic wastewater generated during the winemaking process. It contains a large amount of organic matter, such as proteins, polysaccharides, amino acids, etc. Among them, amino acids are important bioactive substances with high economic value.

[0003] However, the direct discharge of winemaking yellow water will cause serious pollution to the environment, and traditional treatment methods are difficult to achieve both the discharge of wastewater in compliance with standards and the recycling of useful components.

[0004] Existing wastewater treatment technologies, such as physical, chemical, and biological treatment methods, typically only partially remove organic pollutants and are costly and inefficient. Furthermore, traditional extraction techniques have a low recovery rate of useful components from brewing yellow water, making it difficult to meet industrial requirements.

[0005] Therefore, developing an efficient, economical and environmentally friendly method for treating and utilizing brewing yellow water has important practical significance and application prospects. Summary of the Invention

[0006] In view of this, the present invention provides a method for treating yellow wine water by combining micro-nano bubble microwave and microfluid extraction and extracting effective ingredients.

[0007] In order to solve the above technical problems, the present invention adopts the following technical solutions:

[0008] A method for treating yellow wine water and extracting effective ingredients by combining micro-nano bubble microwave and microfluid extraction comprises the following steps:

[0009] (1) Pretreatment of winemaking yellow water:

[0010] The collected yellow wine water is filtered to remove suspended matter and large particles of impurities to obtain clear yellow water;

[0011] (2) Micro-nano bubble treatment:

[0012] The pretreated yellow water is introduced into the micro-nano bubble generator and air or oxygen is introduced to perform the first micro-nano bubble treatment to remove some organic matter and reduce COD.

[0013] (3) Microwave treatment:

[0014] The yellow water treated with the first micro-nano bubble is placed in a microwave reactor and microwave-treated under set microwave power and temperature conditions to crack macromolecular organic matter into small molecules and increase the amino acid content;

[0015] (4) Secondary treatment of micro-nano bubbles:

[0016] The yellow water after microwave treatment enters the micro-nano bubble generating device again, and air or oxygen is introduced to perform a second micro-nano bubble treatment to further reduce the organic matter content;

[0017] (5) Microfluidic extraction:

[0018] The treated yellow water is introduced into a microfluidic extraction device for contact extraction with an extractant to enrich and extract the effective components;

[0019] (6) Product Recycling:

[0020] The extract phase is concentrated and purified to obtain an enriched active ingredient product;

[0021] (7) Wastewater treatment:

[0022] The raffinate and waste liquid generated during the treatment process are treated to meet the standards and then discharged or recycled as resources.

[0023] Preferably, in step (1), the filtration mesh is 100-200 mesh, and the filtration time is 10-30 minutes.

[0024] Preferably, in step (2), the diameter of the bubbles generated by the micro-nano bubble generating device is 50-500 nm, and the gas residence time is 5-15 minutes.

[0025] Preferably, in step (2), the gas introduced into the micro-nano bubble treatment is air or pure oxygen, the gas flow rate is 0.5-1.5 L / min, and the treatment time is 30-90 minutes.

[0026] Preferably, in step (3), the microwave power of the microwave treatment is 400-1000W, the temperature is 60-100°C, and the treatment time is 10-40 minutes; the power and temperature are controlled in a correlated manner during the microwave treatment, and each increase of 100W in power corresponds to a 10-15°C increase in temperature.

[0027] Preferably, in step (5), the extractant is a hydrophobic organic solvent, an ionic liquid or an amine compound; wherein,

[0028] The hydrophobic organic solvent includes n-hexane and isopropyl alcohol; the ionic liquid includes tetrabutylammonium bromide and triethyl phosphate; and the amine compound includes triethylamine and diethylamine.

[0029] Preferably, in step (5), the extraction process is carried out in a microfluidic extraction device, the volume ratio of the extractant to yellow water is 1:1 to 1:3, the extraction time is 20-60 minutes, and the flow rate is 0.2-1.0 mL / min.

[0030] Preferably, in step (6), the extracted active ingredients include amino acids such as glutamic acid and glycine, and the extraction purity can be increased from 0.1%-2% of the original content to 1%-10%.

[0031] Preferably, the sequence and frequency of the micro-nano bubble treatment and microwave treatment can be flexibly adjusted according to the wastewater characteristics and treatment requirements.

[0032] Preferably, in step (7), the waste liquid treatment includes biochemical treatment, membrane filtration, and evaporation concentration processes to ensure that the waste liquid meets the discharge standards or is recycled as a resource.

[0033] Compared with the prior art, the present invention has achieved the following technical effects:

[0034] (1) Technological innovation: For the first time, micro-nano bubbles, microwave treatment and microfluidic extraction technologies are combined to give full play to their respective advantages to form a complete and efficient process for the treatment and resource utilization of yellow wine water;

[0035] (2) High treatment efficiency: By optimizing process parameters and the synergistic effect of various technical links, efficient removal of organic pollutants and efficient extraction of effective components are achieved;

[0036] (3) Green and environmentally friendly process: The treatment process has no harmful by-products, conforms to the concept of green chemistry and sustainable development, and reduces the risk of environmental pollution;

[0037] (4) Significant economic benefits: The extraction and recovery of useful components in wastewater has turned waste into treasure and has good economic value.

[0038] (5) Strong scalability: The process is simple, the equipment is easily available, and it is easy to promote and apply in related industries such as brewing. It is suitable for industrial application and has broad application prospects and promotion value. BRIEF DESCRIPTION OF THE DRAWINGS

[0039] Figure 1 is a flow chart of the present invention;

[0040] Figure 2 This is a diagram of the micro-nano bubble generating device of the present invention. DETAILED DESCRIPTION

[0041] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0042] like Figure 1 As shown, the present invention discloses a method for treating yellow wine water with micro-nano bubble microwave-microfluid extraction and extracting effective ingredients, comprising the following steps:

[0043] (1) Pretreatment of winemaking yellow water:

[0044] The collected yellow wine water is filtered to remove suspended matter and large particles of impurities to obtain clear yellow water;

[0045] (2) Micro-nano bubble treatment:

[0046] The pretreated yellow water is introduced into the micro-nano bubble generator and air or oxygen is introduced to perform the first micro-nano bubble treatment to remove some organic matter and reduce COD.

[0047] (3) Microwave treatment:

[0048] The yellow water treated with the first micro-nano bubble is placed in a microwave reactor and microwave-treated under set microwave power and temperature conditions to crack macromolecular organic matter into small molecules and increase the amino acid content;

[0049] (4) Secondary treatment of micro-nano bubbles:

[0050] The yellow water after microwave treatment enters the micro-nano bubble generating device again, and air or oxygen is introduced to perform a second micro-nano bubble treatment to further reduce the organic matter content;

[0051] (5) Microfluidic extraction:

[0052] The treated yellow water is introduced into a microfluidic extraction device for contact extraction with an extractant to enrich and extract the effective components;

[0053] (6) Product Recycling:

[0054] The extract phase is concentrated and purified to obtain an enriched active ingredient product;

[0055] (7) Wastewater treatment:

[0056] The raffinate and waste liquid generated during the treatment process are treated to meet the standards and then discharged or recycled as resources.

[0057] In step (1), the filtration mesh is 100-200 mesh, and the filtration time is 10-30 minutes.

[0058] In step (2), the diameter of the bubbles generated by the micro-nano bubble generating device is 50-500 nm, and the gas residence time is 5-15 minutes.

[0059] In step (2), the gas introduced into the micro-nano bubble treatment is air or pure oxygen, the gas flow rate is 0.5-1.5 L / min, and the treatment time is 30-90 minutes.

[0060] In step (3), the microwave power of the microwave treatment is 400-1000W, the temperature is 60-100°C, and the treatment time is 10-40 minutes; the power and temperature are controlled in a correlated manner during the microwave treatment, and each increase of 100W in power corresponds to a 10-15°C increase in temperature.

[0061] In step (5), the extractant is a hydrophobic organic solvent, an ionic liquid or an amine compound; wherein,

[0062] The hydrophobic organic solvent includes n-hexane and isopropyl alcohol; the ionic liquid includes tetrabutylammonium bromide and triethyl phosphate; and the amine compound includes triethylamine and diethylamine.

[0063] In step (5), the extraction process is carried out in a microfluidic extraction device, the volume ratio of the extractant to yellow water is 1:1 to 1:3, the extraction time is 20-60 minutes, and the flow rate is 0.2-1.0 mL / min.

[0064] In step (6), the extracted effective components include amino acids such as glutamic acid and glycine, and the extraction purity can be increased from 0.1%-2% of the original content to 1%-10%.

[0065] The order and frequency of micro-nano bubble treatment and microwave treatment can be flexibly adjusted according to the wastewater characteristics and treatment requirements.

[0066] In step (7), waste liquid treatment includes biochemical treatment, membrane filtration, and evaporation concentration processes to ensure that the waste liquid meets discharge standards or is recycled as a resource.

[0067] Among them, micro-nano ozone bubble generating device such as Figure 2 shown.

[0068] Example 1: Treatment of winemaking yellow water and extraction of glutamic acid

[0069] 1. Raw materials: Yellow wine water, containing suspended solids (SS) of about 500 mg / L, COD of about 20,000 mg / L, total amino acid content of about 2%, of which glutamic acid content is about 0.5%.

[0070] 2. Operation steps:

[0071] (1) Pretreatment of winemaking yellow water:

[0072] Filter the yellow water through a filter to remove suspended matter and large particles of impurities to obtain clear yellow water;

[0073] (2) Micro-nano bubble treatment:

[0074] The pretreated yellow water was introduced into the micro-nano bubble generator and air was introduced for the first micro-nano bubble treatment. The gas flow rate was 1 L / min and the treatment time was 60 minutes. The COD was reduced by about 10%, and some organic matter was oxidized and degraded.

[0075] (3) Microwave treatment:

[0076] The yellow water treated with the first micro-nano bubble treatment was placed in a microwave reactor at a frequency of 2.45 GHz, a microwave power of 800 W, a temperature of 90°C, and a treatment time of 20 minutes. The yellow water was microwave-treated to break down the macromolecular organic matter into small molecules, thereby increasing the amino acid concentration and the total amino acid content from 2% to 3%.

[0077] (4) Secondary treatment of micro-nano bubbles:

[0078] The yellow water after microwave treatment was put into the micro-nano bubble generator again and pure oxygen was introduced for the second micro-nano bubble treatment. The gas flow rate was 1L / min and the treatment time was 60 minutes. The COD was further reduced, with the total COD reduction reaching 30%, and the liquid purity was improved.

[0079] (5) Microfluidic extraction:

[0080] The treated yellow water was introduced into a microfluidic extraction device and contacted with ionic liquid tetrabutylammonium bromide for extraction. The volume ratio of ionic liquid tetrabutylammonium bromide to yellow water was 1:1, the flow rate was 0.5 mL / min, the temperature was room temperature, and the extraction time was 30 minutes. Glutamic acid was enriched from 0.5% to 5%, and the extraction rate reached 80%.

[0081] (6) Product Recycling:

[0082] The extract phase is concentrated and purified to obtain an enriched glutamic acid product;

[0083] (7) Wastewater treatment:

[0084] The raffinate is biochemically treated and discharged to meet standards or recycled.

[0085] 3. Result analysis:

[0086] Through combined treatment, this example successfully increased the glutamate content in brewing yellow water from 0.5% to 5%, significantly improving the extraction efficiency; micro-nano bubble treatment and microwave treatment effectively reduced COD, improved liquid purity, and provided good conditions for subsequent extraction; microfluidic extraction technology achieved efficient and selective enrichment of glutamate.

[0087] Example 2: Treatment of winemaking yellow water and extraction of glycine

[0088] 1. Raw materials: brewing yellow water, COD about 15000mg / L, total amino acid content about 1%, of which glycine content about 0.2%.

[0089] 2. Operation steps:

[0090] (1) Pretreatment of winemaking yellow water:

[0091] The collected yellow wine water is filtered to remove suspended matter and large particles of impurities to obtain clear yellow water;

[0092] (2) Micro-nano bubble treatment:

[0093] The pretreated yellow water was introduced into the micro-nano bubble generator and air was introduced for the first micro-nano bubble treatment. The gas flow rate was 0.8 L / min and the treatment time was 50 minutes. Part of the organic matter was removed and the COD was reduced by about 8%.

[0094] (3) Microwave treatment:

[0095] The yellow water treated with the first micro-nano bubble was placed in a microwave reactor and microwave-treated at a microwave power of 600 W, a temperature of 80° C., and a treatment time of 25 minutes to cleave macromolecules and increase the amino acid content, with the total amino acid content increasing from 1% to 1.5%.

[0096] (4) Secondary treatment of micro-nano bubbles:

[0097] The yellow water after microwave treatment was put into the micro-nano bubble generator again and air was introduced for the second micro-nano bubble treatment. The gas flow rate was 0.8 L / min and the treatment time was 50 minutes. The COD was further reduced, with a total reduction of 25%.

[0098] (5) Microfluidic extraction:

[0099] The treated yellow water was introduced into a microfluidic extraction device and extracted with isopropyl alcohol. The volume ratio of isopropyl alcohol to yellow water was 1:1. Glycine was enriched from 0.2% to 2%, and the extraction rate reached 75%.

[0100] (6) Product Recycling:

[0101] The extract phase is concentrated and purified to obtain enriched glycine;

[0102] (7) Wastewater treatment:

[0103] The raffinate is subsequently treated and discharged in compliance with discharge standards.

[0104] 3. Result analysis:

[0105] Successfully increased the glycine content from 0.2% to 2%;

[0106] Optimization of microwave treatment conditions increased the production of amino acids;

[0107] Isopropyl alcohol is used as the extraction agent, which has good selectivity and is easy to operate.

[0108] Example 3: Micro-nano bubble treatment parameter optimization and synergistic effect analysis

[0109] 1. Gas type (one)

[0111] (1) Pretreatment of winemaking yellow water:

[0112] The collected yellow wine water is filtered to remove suspended matter and large particles of impurities to obtain clear yellow water;

[0113] (2) Micro-nano bubble treatment:

[0114] The pretreated yellow water was introduced into the micro-nano bubble generator and air was introduced at a gas flow rate of 1.0 L / min for 60 minutes to perform the first micro-nano bubble treatment to remove some organic matter and reduce COD.

[0115] (3) Microwave treatment:

[0116] The yellow water treated with the first micro-nano bubble treatment was placed in a microwave reactor and subjected to microwave treatment at a microwave power of 700 W, a temperature of 80° C., and a time of 30 minutes to crack large organic molecules into small molecules and increase the amino acid content.

[0117] (4) Secondary treatment of micro-nano bubbles:

[0118] The yellow water after microwave treatment is put into the micro-nano bubble generating device again, and air is introduced to perform a second micro-nano bubble treatment to further reduce the organic matter content;

[0119] (5) Microfluidic extraction:

[0120] The treated yellow water was introduced into a microfluidic extraction device and contacted with ionic liquid tetrabutylammonium bromide for extraction. The volume ratio of ionic liquid tetrabutylammonium bromide to yellow water was 1:2, the flow rate was 0.6 mL / min, the temperature was room temperature, and the extraction time was 40 minutes to enrich and extract the effective components.

[0121] (6) Product Recycling:

[0122] The extract phase is concentrated and purified to obtain an enriched active ingredient product;

[0123] (7) Wastewater treatment:

[0124] The raffinate and waste liquid generated during the treatment process are treated to meet the standards and then discharged or recycled as resources. (two)

[0126] (1) Pretreatment of winemaking yellow water:

[0127] The collected yellow wine water is filtered to remove suspended matter and large particles of impurities to obtain clear yellow water;

[0128] (2) Micro-nano bubble treatment:

[0129] The pretreated yellow water was introduced into the micro-nano bubble generator and oxygen was introduced at a gas flow rate of 1.0 L / min for 60 minutes to perform the first micro-nano bubble treatment to remove some organic matter and reduce COD.

[0130] (3) Microwave treatment:

[0131] The yellow water treated with the first micro-nano bubble treatment was placed in a microwave reactor and subjected to microwave treatment at a microwave power of 700W, a temperature of 80°C, and a time of 30 minutes to crack large organic molecules into small molecules and increase the amino acid content.

[0132] (4) Secondary treatment of micro-nano bubbles:

[0133] The yellow water after microwave treatment is put into the micro-nano bubble generator again, oxygen is introduced, and a second micro-nano bubble treatment is performed to further reduce the organic matter content;

[0134] (5) Microfluidic extraction:

[0135] The treated yellow water was introduced into a microfluidic extraction device and contacted with ionic liquid tetrabutylammonium bromide for extraction. The volume ratio of ionic liquid tetrabutylammonium bromide to yellow water was 1:2, the flow rate was 0.6 mL / min, the temperature was room temperature, and the extraction time was 40 minutes to enrich and extract the effective components.

[0136] (6) Product Recycling:

[0137] The extract phase is concentrated and purified to obtain an enriched active ingredient product;

[0138] (7) Wastewater treatment:

[0139] The raffinate and waste liquid generated during the treatment process are treated to meet the standards and then discharged or recycled as resources.

[0140] Results: The effect of introducing oxygen was better than that of air, and the COD removal rate increased by about 5%.

[0141] 2. Gas flow and processing time (one)

[0143] (1) Pretreatment of winemaking yellow water:

[0144] The collected yellow wine water is filtered to remove suspended matter and large particles of impurities to obtain clear yellow water;

[0145] (2) Micro-nano bubble treatment:

[0146] The pretreated yellow water was introduced into the micro-nano bubble generator and oxygen was introduced at a gas flow rate of 0.5 L / min for 30 minutes to perform the first micro-nano bubble treatment to remove some organic matter and reduce COD.

[0147] (3) Microwave treatment:

[0148] The yellow water treated with the first micro-nano bubble treatment was placed in a microwave reactor and subjected to microwave treatment at a microwave power of 700 W, a temperature of 80° C., and a time of 30 minutes to crack large organic molecules into small molecules and increase the amino acid content.

[0149] (4) Secondary treatment of micro-nano bubbles:

[0150] The yellow water after microwave treatment is put into the micro-nano bubble generator again, oxygen is introduced, and a second micro-nano bubble treatment is performed to further reduce the organic matter content;

[0151] (5) Microfluidic extraction:

[0152] The treated yellow water was introduced into a microfluidic extraction device and contacted with ionic liquid tetrabutylammonium bromide for extraction. The volume ratio of ionic liquid tetrabutylammonium bromide to yellow water was 1:2, the flow rate was 0.6 mL / min, the temperature was room temperature, and the extraction time was 40 minutes to enrich and extract the effective components.

[0153] (6) Product Recycling:

[0154] The extract phase is concentrated and purified to obtain an enriched active ingredient product;

[0155] (7) Wastewater treatment:

[0156] The raffinate and waste liquid generated during the treatment process are treated to meet the standards and then discharged or recycled as resources. (two)

[0158] (1) Pretreatment of winemaking yellow water:

[0159] The collected yellow wine water is filtered to remove suspended matter and large particles of impurities to obtain clear yellow water;

[0160] (2) Micro-nano bubble treatment:

[0161] The pretreated yellow water was introduced into the micro-nano bubble generator and oxygen was introduced at a gas flow rate of 1.0 L / min for 60 minutes to perform the first micro-nano bubble treatment to remove some organic matter and reduce COD.

[0162] (3) Microwave treatment:

[0163] The yellow water treated with the first micro-nano bubble treatment was placed in a microwave reactor and subjected to microwave treatment at a microwave power of 700 W, a temperature of 80° C., and a time of 30 minutes to crack large organic molecules into small molecules and increase the amino acid content.

[0164] (4) Secondary treatment of micro-nano bubbles:

[0165] The yellow water after microwave treatment is put into the micro-nano bubble generator again, oxygen is introduced, and a second micro-nano bubble treatment is performed to further reduce the organic matter content;

[0166] (5) Microfluidic extraction:

[0167] The treated yellow water was introduced into a microfluidic extraction device and contacted with ionic liquid tetrabutylammonium bromide for extraction. The volume ratio of ionic liquid tetrabutylammonium bromide to yellow water was 1:2, the flow rate was 0.6 mL / min, the temperature was room temperature, and the extraction time was 40 minutes to enrich and extract the effective components.

[0168] (6) Product Recycling:

[0169] The extract phase is concentrated and purified to obtain an enriched active ingredient product;

[0170] (7) Wastewater treatment:

[0171] The raffinate and waste liquid generated during the treatment process are treated to meet the standards and then discharged or recycled as resources. (three)

[0173] (1) Pretreatment of winemaking yellow water:

[0174] The collected yellow wine water is filtered to remove suspended matter and large particles of impurities to obtain clear yellow water;

[0175] (2) Micro-nano bubble treatment:

[0176] The pretreated yellow water was introduced into the micro-nano bubble generator and oxygen was introduced at a gas flow rate of 1.5 L / min for 90 minutes to perform the first micro-nano bubble treatment to remove some organic matter and reduce COD.

[0177] (3) Microwave treatment:

[0178] The yellow water treated with the first micro-nano bubble treatment was placed in a microwave reactor and subjected to microwave treatment at a microwave power of 700 W, a temperature of 80° C., and a time of 30 minutes to crack large organic molecules into small molecules and increase the amino acid content.

[0179] (4) Secondary treatment of micro-nano bubbles:

[0180] The yellow water after microwave treatment is put into the micro-nano bubble generator again, oxygen is introduced, and a second micro-nano bubble treatment is performed to further reduce the organic matter content;

[0181] (5) Microfluidic extraction:

[0182] The treated yellow water was introduced into a microfluidic extraction device and contacted with ionic liquid tetrabutylammonium bromide for extraction. The volume ratio of ionic liquid tetrabutylammonium bromide to yellow water was 1:2, the flow rate was 0.6 mL / min, the temperature was room temperature, and the extraction time was 40 minutes to enrich and extract the effective components.

[0183] (6) Product Recycling:

[0184] The extract phase is concentrated and purified to obtain an enriched active ingredient product;

[0185] (7) Wastewater treatment:

[0186] The raffinate and waste liquid generated during the treatment process are treated to meet the standards and then discharged or recycled as resources.

[0187] Results: The COD removal effect was improved with appropriate increase of gas flow rate and treatment time, but the effect was not obvious with excessive increase.

[0188] 3. Microwave power, microwave temperature and processing time (one)

[0190] (1) Pretreatment of winemaking yellow water:

[0191] The collected yellow wine water is filtered to remove suspended matter and large particles of impurities to obtain clear yellow water;

[0192] (2) Micro-nano bubble treatment:

[0193] The pretreated yellow water was introduced into the micro-nano bubble generator and oxygen was introduced at a gas flow rate of 1.0 L / min for 60 minutes to perform the first micro-nano bubble treatment to remove some organic matter and reduce COD.

[0194] (3) Microwave treatment:

[0195] The yellow water treated with the first micro-nano bubble treatment was placed in a microwave reactor and subjected to microwave treatment at a microwave power of 400 W, a temperature of 60° C., and a time of 10 minutes to crack large organic molecules into small molecules and increase the amino acid content.

[0196] (4) Secondary treatment of micro-nano bubbles:

[0197] The yellow water after microwave treatment is put into the micro-nano bubble generator again, oxygen is introduced, and a second micro-nano bubble treatment is performed to further reduce the organic matter content;

[0198] (5) Microfluidic extraction:

[0199] The treated yellow water was introduced into a microfluidic extraction device and contacted with ionic liquid tetrabutylammonium bromide for extraction. The volume ratio of ionic liquid tetrabutylammonium bromide to yellow water was 1:2, the flow rate was 0.6 mL / min, the temperature was room temperature, and the extraction time was 40 minutes to enrich and extract the effective components.

[0200] (6) Product Recycling:

[0201] The extract phase is concentrated and purified to obtain an enriched active ingredient product;

[0202] (7) Wastewater treatment:

[0203] The raffinate and waste liquid generated during the treatment process are treated to meet the standards and then discharged or recycled as resources. (two)

[0205] (1) Pretreatment of winemaking yellow water:

[0206] The collected yellow wine water is filtered to remove suspended matter and large particles of impurities to obtain clear yellow water;

[0207] (2) Micro-nano bubble treatment:

[0208] The pretreated yellow water was introduced into the micro-nano bubble generator and oxygen was introduced at a gas flow rate of 1.0 L / min for 60 minutes to perform the first micro-nano bubble treatment to remove some organic matter and reduce COD.

[0209] (3) Microwave treatment:

[0210] The yellow water treated with the first micro-nano bubble treatment was placed in a microwave reactor and subjected to microwave treatment at a microwave power of 700 W, a temperature of 80° C., and a time of 30 minutes to crack large organic molecules into small molecules and increase the amino acid content.

[0211] (4) Secondary treatment of micro-nano bubbles:

[0212] The yellow water after microwave treatment is put into the micro-nano bubble generator again, oxygen is introduced, and a second micro-nano bubble treatment is performed to further reduce the organic matter content;

[0213] (5) Microfluidic extraction:

[0214] The treated yellow water was introduced into a microfluidic extraction device and contacted with ionic liquid tetrabutylammonium bromide for extraction. The volume ratio of ionic liquid tetrabutylammonium bromide to yellow water was 1:2, the flow rate was 0.6 mL / min, the temperature was room temperature, and the extraction time was 40 minutes to enrich and extract the effective components.

[0215] (6) Product Recycling:

[0216] The extract phase is concentrated and purified to obtain an enriched active ingredient product;

[0217] (7) Wastewater treatment:

[0218] The raffinate and waste liquid generated during the treatment process are treated to meet the standards and then discharged or recycled as resources. (three)

[0220] (1) Pretreatment of winemaking yellow water:

[0221] The collected yellow wine water is filtered to remove suspended matter and large particles of impurities to obtain clear yellow water;

[0222] (2) Micro-nano bubble treatment:

[0223] The pretreated yellow water was introduced into the micro-nano bubble generator and oxygen was introduced at a gas flow rate of 1.0 L / min for 60 minutes to perform the first micro-nano bubble treatment to remove some organic matter and reduce COD.

[0224] (3) Microwave treatment:

[0225] The yellow water treated with the first micro-nano bubble treatment was placed in a microwave reactor and subjected to microwave treatment at a microwave power of 1000W, a temperature of 10°C, and a time of 40 minutes to crack large organic molecules into small molecules and increase the amino acid content.

[0226] (4) Secondary treatment of micro-nano bubbles:

[0227] The yellow water after microwave treatment is put into the micro-nano bubble generator again, oxygen is introduced, and a second micro-nano bubble treatment is performed to further reduce the organic matter content;

[0228] (5) Microfluidic extraction:

[0229] The treated yellow water was introduced into a microfluidic extraction device and contacted with ionic liquid tetrabutylammonium bromide for extraction. The volume ratio of ionic liquid tetrabutylammonium bromide to yellow water was 1:2, the flow rate was 0.6 mL / min, the temperature was room temperature, and the extraction time was 40 minutes to enrich and extract the effective components.

[0230] (6) Product Recycling:

[0231] The extract phase is concentrated and purified to obtain an enriched active ingredient product;

[0232] (7) Wastewater treatment:

[0233] The raffinate and waste liquid generated during the treatment process are treated to meet the standards and then discharged or recycled as resources.

[0234] Results: The increase of microwave power and temperature was beneficial to the cleavage of macromolecules, but too high a temperature might lead to the degradation of amino acids. The optimal temperature was 80-90℃ and the time was 20-30 minutes.

[0235] 4. Type of extraction agent (one)

[0237] (1) Pretreatment of winemaking yellow water:

[0238] The collected yellow wine water is filtered to remove suspended matter and large particles of impurities to obtain clear yellow water;

[0239] (2) Micro-nano bubble treatment:

[0240] The pretreated yellow water was introduced into the micro-nano bubble generator and oxygen was introduced at a gas flow rate of 1.0 L / min for 60 minutes to perform the first micro-nano bubble treatment to remove some organic matter and reduce COD.

[0241] (3) Microwave treatment:

[0242] The yellow water treated with the first micro-nano bubble treatment was placed in a microwave reactor and microwave-treated at a microwave power of 700 W, a temperature of 60° C., and a time of 30 minutes to crack large organic molecules into small molecules and increase the amino acid content.

[0243] (4) Secondary treatment of micro-nano bubbles:

[0244] The yellow water after microwave treatment is put into the micro-nano bubble generator again, oxygen is introduced, and a second micro-nano bubble treatment is performed to further reduce the organic matter content;

[0245] (5) Microfluidic extraction:

[0246] The treated yellow water was introduced into a microfluidic extraction device and contacted with ionic liquid tetrabutylammonium bromide for extraction. The volume ratio of ionic liquid tetrabutylammonium bromide to yellow water was 1:2, the flow rate was 0.6 mL / min, the temperature was room temperature, and the extraction time was 40 minutes to enrich and extract the effective components.

[0247] (6) Product Recycling:

[0248] The extract phase is concentrated and purified to obtain an enriched active ingredient product;

[0249] (7) Wastewater treatment:

[0250] The raffinate and waste liquid generated during the treatment process are treated to meet the standards and then discharged or recycled as resources. (two)

[0252] (1) Pretreatment of winemaking yellow water:

[0253] The collected yellow wine water is filtered to remove suspended matter and large particles of impurities to obtain clear yellow water;

[0254] (2) Micro-nano bubble treatment:

[0255] The pretreated yellow water was introduced into the micro-nano bubble generator and oxygen was introduced at a gas flow rate of 1.0 L / min for 60 minutes to perform the first micro-nano bubble treatment to remove some organic matter and reduce COD.

[0256] (3) Microwave treatment:

[0257] The yellow water treated with the first micro-nano bubble treatment was placed in a microwave reactor and microwave-treated at a microwave power of 700 W, a temperature of 60° C., and a time of 30 minutes to crack large organic molecules into small molecules and increase the amino acid content.

[0258] (4) Secondary treatment of micro-nano bubbles:

[0259] The yellow water after microwave treatment is put into the micro-nano bubble generator again, oxygen is introduced, and a second micro-nano bubble treatment is performed to further reduce the organic matter content;

[0260] (5) Microfluidic extraction:

[0261] The treated yellow water was introduced into a microfluidic extraction device and contacted with the amine compound triethylamine for extraction. The volume ratio of ionic liquid tetrabutylammonium bromide to yellow water was 1:2, the flow rate was 0.6 mL / min, the temperature was room temperature, and the extraction time was 40 minutes to enrich and extract the effective components.

[0262] (6) Product Recycling:

[0263] The extract phase is concentrated and purified to obtain an enriched active ingredient product;

[0264] (7) Wastewater treatment:

[0265] The raffinate and waste liquid generated during the treatment process are treated to meet the standards and then discharged or recycled as resources. (three)

[0267] (1) Pretreatment of winemaking yellow water:

[0268] The collected yellow wine water is filtered to remove suspended matter and large particles of impurities to obtain clear yellow water;

[0269] (2) Micro-nano bubble treatment:

[0270] The pretreated yellow water was introduced into the micro-nano bubble generator and oxygen was introduced at a gas flow rate of 1.0 L / min for 60 minutes to perform the first micro-nano bubble treatment to remove some organic matter and reduce COD.

[0271] (3) Microwave treatment:

[0272] The yellow water treated with the first micro-nano bubble treatment was placed in a microwave reactor and microwave-treated at a microwave power of 700 W, a temperature of 60° C., and a time of 30 minutes to crack large organic molecules into small molecules and increase the amino acid content.

[0273] (4) Secondary treatment of micro-nano bubbles:

[0274] The yellow water after microwave treatment is put into the micro-nano bubble generator again, oxygen is introduced, and a second micro-nano bubble treatment is performed to further reduce the organic matter content;

[0275] (5) Microfluidic extraction:

[0276] The treated yellow water was introduced into a microfluidic extraction device and contacted with an organic solvent, n-hexane, for extraction. The volume ratio of ionic liquid tetrabutylammonium bromide to yellow water was 1:2, the flow rate was 0.6 mL / min, the temperature was room temperature, and the extraction time was 40 minutes to enrich and extract the effective components.

[0277] (6) Product Recycling:

[0278] The extract phase is concentrated and purified to obtain an enriched active ingredient product;

[0279] (7) Wastewater treatment:

[0280] The raffinate and waste liquid generated during the treatment process are treated to meet the standards and then discharged or recycled as resources.

[0281] Results: The type of extractant had a significant effect on the extraction effect: ionic liquids > amine compounds > organic solvents.

[0282] 5. Extractant dosage, extraction flow rate and extraction time (one)

[0284] (1) Pretreatment of winemaking yellow water:

[0285] The collected yellow wine water is filtered to remove suspended matter and large particles of impurities to obtain clear yellow water;

[0286] (2) Micro-nano bubble treatment:

[0287] The pretreated yellow water was introduced into the micro-nano bubble generator and oxygen was introduced at a gas flow rate of 1.0 L / min for 60 minutes to perform the first micro-nano bubble treatment to remove some organic matter and reduce COD.

[0288] (3) Microwave treatment:

[0289] The yellow water treated with the first micro-nano bubble treatment was placed in a microwave reactor and microwave-treated at a microwave power of 700 W, a temperature of 60° C., and a time of 30 minutes to crack large organic molecules into small molecules and increase the amino acid content.

[0290] (4) Secondary treatment of micro-nano bubbles:

[0291] The yellow water after microwave treatment is put into the micro-nano bubble generator again, oxygen is introduced, and a second micro-nano bubble treatment is performed to further reduce the organic matter content;

[0292] (5) Microfluidic extraction:

[0293] The treated yellow water was introduced into a microfluidic extraction device and contacted with ionic liquid tetrabutylammonium bromide for extraction. The volume ratio of ionic liquid tetrabutylammonium bromide to yellow water was 1:1, the flow rate was 0.2 mL / min, the temperature was room temperature, and the extraction time was 20 minutes to enrich and extract the effective components.

[0294] (6) Product Recycling:

[0295] The extract phase is concentrated and purified to obtain an enriched active ingredient product;

[0296] (7) Wastewater treatment:

[0297] The raffinate and waste liquid generated during the treatment process are treated to meet the standards and then discharged or recycled as resources. (two)

[0299] (1) Pretreatment of winemaking yellow water:

[0300] The collected yellow wine water is filtered to remove suspended matter and large particles of impurities to obtain clear yellow water;

[0301] (2) Micro-nano bubble treatment:

[0302] The pretreated yellow water was introduced into the micro-nano bubble generator and oxygen was introduced at a gas flow rate of 1.0 L / min for 60 minutes to perform the first micro-nano bubble treatment to remove some organic matter and reduce COD.

[0303] (3) Microwave treatment:

[0304] The yellow water treated with the first micro-nano bubble treatment was placed in a microwave reactor and microwave-treated at a microwave power of 700 W, a temperature of 60° C., and a time of 30 minutes to crack large organic molecules into small molecules and increase the amino acid content.

[0305] (4) Secondary treatment of micro-nano bubbles:

[0306] The yellow water after microwave treatment is put into the micro-nano bubble generator again, oxygen is introduced, and a second micro-nano bubble treatment is performed to further reduce the organic matter content;

[0307] (5) Microfluidic extraction:

[0308] The treated yellow water was introduced into a microfluidic extraction device and contacted with ionic liquid tetrabutylammonium bromide for extraction. The volume ratio of ionic liquid tetrabutylammonium bromide to yellow water was 1:2, the flow rate was 0.6 mL / min, the temperature was room temperature, and the extraction time was 40 minutes to enrich and extract the effective components.

[0309] (6) Product Recycling:

[0310] The extract phase is concentrated and purified to obtain an enriched active ingredient product;

[0311] (7) Wastewater treatment:

[0312] The raffinate and waste liquid generated during the treatment process are treated to meet the standards and then discharged or recycled as resources. (three)

[0314] (1) Pretreatment of winemaking yellow water:

[0315] The collected yellow wine water is filtered to remove suspended matter and large particles of impurities to obtain clear yellow water;

[0316] (2) Micro-nano bubble treatment:

[0317] The pretreated yellow water was introduced into the micro-nano bubble generator and oxygen was introduced at a gas flow rate of 1.0 L / min for 60 minutes to perform the first micro-nano bubble treatment to remove some organic matter and reduce COD.

[0318] (3) Microwave treatment:

[0319] The yellow water treated with the first micro-nano bubble treatment was placed in a microwave reactor and microwave-treated at a microwave power of 700 W, a temperature of 60° C., and a time of 30 minutes to crack large organic molecules into small molecules and increase the amino acid content.

[0320] (4) Secondary treatment of micro-nano bubbles:

[0321] The yellow water after microwave treatment is put into the micro-nano bubble generator again, oxygen is introduced, and a second micro-nano bubble treatment is performed to further reduce the organic matter content;

[0322] (5) Microfluidic extraction:

[0323] The treated yellow water was introduced into a microfluidic extraction device and contacted with ionic liquid tetrabutylammonium bromide for extraction. The volume ratio of ionic liquid tetrabutylammonium bromide to yellow water was 1:3, the flow rate was 1.0 mL / min, the temperature was room temperature, and the extraction time was 60 minutes to enrich and extract the effective components.

[0324] (6) Product Recycling:

[0325] The extract phase is concentrated and purified to obtain an enriched active ingredient product;

[0326] (7) Wastewater treatment:

[0327] The raffinate and waste liquid generated during the treatment process are treated to meet the standards and then discharged or recycled as resources.

[0328] Results: The extraction rate increased with the increase of the amount of extractant and extraction time, but the cost and efficiency should be considered.

[0329] Synergy:

[0330] Micro-nano bubble treatment creates favorable conditions for microwave treatment, reducing the viscosity and COD of the liquid; the small molecules produced by microwave treatment are beneficial to microfluidic extraction and increase the driving force of mass transfer; each step works closely together and synergistically to maximize the treatment effect.

[0331] Among them, the results of the effects of gas type, flow rate, and processing time are shown in Table 1;

[0332] Table 1:

[0333] Gas type Flow rate (L / min) Processing time (min) Initial COD (mg / L) COD reduction rate Air 1.0 60 20000 10％ pure oxygen 1.0 60 20000 15％

[0334] The effects of microwave power, microwave temperature, and treatment time on total amino acid content are shown in Table 2 ;

[0335] Table 2:

[0336] Microwave power (W) Temperature (℃) Processing time (min) Amino acid enhancement rate 600 80 25 50％ 800 90 20 60％ 1000 100 30 70％

[0337] After microwave treatment, the total amino acid content increases by 50%-100%;

[0338] The effects of microfluidic extraction parameters on glutamate extraction yield are shown in Table 3 ;

[0339] Table 3:

[0340]

[0341] Example 4: Effect of filter mesh size on pretreatment effect

[0342] Raw material: SS = 600 mg / L.

[0343] Variable: filter mesh size (100 mesh, 150 mesh, 200 mesh).

[0344] The results are shown in Table 4;

[0345] Table 4:

[0346] Filter mesh number Filtration time (min) SS after treatment (mg / L) Removal rate 100 mesh 20 100 83.3％ 150 mesh 20 50 91.7％ 200 mesh 20 30 95％

[0347] After filtration, the removal rate of suspended solids (SS) can reach 80%-95%.

[0348] The results are shown in Table 5:

[0349] Table 5:

[0350] Raw material SS (mg / L) Filter mesh number Filtration time (min) SS after treatment (mg / L) Removal rate 500 150 mesh 20 50 90％ 300 200 mesh 15 30 90％

[0351] Example 5: Effect of microwave power on amino acid production Raw materials: total amino acids = 1.5%.

[0352] Microwave temperature = 90°C, treatment time = 20 minutes.

[0353] The results are shown in Table 6;

[0354] Table 6:

[0355] Microwave power (W) Increased total amino acid content 400 1.5％→2.0％(+33％) 600 1.5％→2.5％(+67％) 800 1.5％→3.0％(+100％)

[0356] Example 5: Effect of Extractant Volume Ratio on Extraction Yield Raw material: glutamic acid = 0.5%.

[0357] Extraction solvent: tetrabutylammonium bromide, extraction time = 30 minutes.

[0358] The results are shown in Table 7;

[0359] Table 7:

[0360] Volume ratio (extractant: yellow water) Glutamic acid extraction rate 1:1 80％ 1:2 65％ 1:3 50％

[0361] The above description is merely a preferred embodiment of the present invention and does not limit the technical scope of the present invention. Therefore, any minor modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention are still within the scope of the technical solution of the present invention.

Claims

1. A method for treating yellow wine water with micro-nano bubble microwave and microfluid extraction to extract effective ingredients, characterized in that: The steps include: (1) Pretreatment of winemaking yellow water: The collected yellow wine water is filtered to remove suspended matter and large particles of impurities to obtain clear yellow water; (2) Micro-nano bubble treatment: The pretreated yellow water is introduced into the micro-nano bubble generator and air or oxygen is introduced to perform the first micro-nano bubble treatment to remove some organic matter and reduce COD. (3) Microwave treatment: The yellow water treated with the first micro-nano bubble is placed in a microwave reactor and microwave-treated under set microwave power and temperature conditions to crack macromolecular organic matter into small molecules and increase the amino acid content; (4) Secondary treatment of micro-nano bubbles: The yellow water after microwave treatment enters the micro-nano bubble generating device again, and air or oxygen is introduced to perform a second micro-nano bubble treatment to further reduce the organic matter content; (5) Microfluidic extraction: The treated yellow water is introduced into a microfluidic extraction device for contact extraction with an extractant to enrich and extract the effective components; (6) Product Recycling: The extract phase is concentrated and purified to obtain an enriched active ingredient product; (7) Wastewater treatment: The raffinate and waste liquid generated during the treatment process are treated to meet the standards and then discharged or recycled as resources.

2. The method for treating yellow wine water with micro-nano bubble microwave-microfluid extraction and extracting effective ingredients according to claim 1, characterized in that: In the step (1), the filtration mesh is 100-200 mesh, and the filtration time is 10-30 minutes.

3. The method for treating yellow wine water with micro-nano bubble microwave-microfluid extraction and extracting effective ingredients according to claim 1, characterized in that: In the step (2), the diameter of the bubbles generated by the micro-nano bubble generating device is 50-500 nm, and the gas residence time is 5-15 minutes.

4. The method of claim 1, wherein the micro-nano bubble microwave-microfluid extraction is combined with the treatment of yellow wine water to extract effective ingredients. In the step (2), the gas introduced into the micro-nano bubble treatment is air or pure oxygen, the gas flow rate is 0.5-1.5 L / min, and the treatment time is 30-90 minutes.

5. The method of claim 1, wherein the micro-nano bubble microwave-microfluid extraction is combined with the treatment of yellow wine water to extract effective ingredients. In the step (3), the microwave power of the microwave treatment is 400-1000W, the temperature is 60-100°C, and the treatment time is 10-40 minutes; the power and temperature are controlled in a correlated manner during the microwave treatment, and each increase of 100W in power corresponds to a 10-15°C increase in temperature.

6. The method of claim 1, wherein the micro-nano bubble microwave-microfluid extraction is combined with the treatment of yellow wine water to extract effective ingredients. In the step (5), the extractant is a hydrophobic organic solvent, an ionic liquid or an amine compound; wherein, The hydrophobic organic solvent includes n-hexane and isopropyl alcohol; the ionic liquid includes tetrabutylammonium bromide and triethyl phosphate; and the amine compound includes triethylamine and diethylamine.

7. The method of claim 1, wherein the micro-nano bubble microwave-microfluid extraction is combined with the treatment of yellow wine water to extract effective ingredients. In the step (5), the extraction process is carried out in a microfluidic extraction device, the volume ratio of the extractant to yellow water is 1:1 to 1:3, the extraction time is 20-60 minutes, and the flow rate is 0.2-1.0 mL / min.

8. The method of claim 1, wherein the micro-nano bubble microwave-microfluid extraction is combined with the treatment of yellow wine water to extract effective ingredients. In the step (6), the extracted effective components include amino acids such as glutamic acid and glycine, and the extraction purity can be increased from 0.1%-2% of the original content to 1%-10%.

9. The method of claim 1, wherein the micro-nano bubble microwave-microfluid extraction is combined with the treatment of yellow wine water to extract effective ingredients. The sequence and frequency of the micro-nano bubble treatment and microwave treatment can be flexibly adjusted according to wastewater characteristics and treatment requirements.

10. The method of claim 1, wherein the micro-nano bubble microwave-microfluid extraction is combined with the treatment of yellow wine water to extract effective ingredients. In the step (7), the waste liquid treatment includes biochemical treatment, membrane filtration, and evaporation concentration processes to ensure that the waste liquid meets the discharge standards or is recycled as a resource.

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