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

Abstract

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

Description

Technical Field

[0001] This invention relates to the field of wastewater treatment and resource utilization technology, and in particular to a method for treating brewing yellow water and extracting effective components using a combination of micro-nano bubble microwave microfluidic extraction. Background Technology

[0002] Yellow wastewater from brewing is a high-concentration organic wastewater generated during the brewing industry. It contains a large amount of organic matter, such as proteins, polysaccharides, and amino acids. Among them, amino acids are important bioactive substances with high economic value.

[0003] However, the direct discharge of yellow wastewater from brewing will cause serious environmental pollution, and traditional treatment methods are difficult to achieve both the standard discharge of wastewater and the recovery and utilization of useful components at the same time.

[0004] Existing wastewater treatment technologies, such as physical, chemical, and biological methods, typically remove only a portion of organic pollutants and are costly and inefficient. Furthermore, traditional extraction techniques have low recovery rates of useful components in brewing wastewater, making them unsuitable for industrial applications.

[0005] Therefore, developing an efficient, economical, and environmentally friendly method for treating and utilizing brewing wastewater is of great practical significance and has promising application prospects. Summary of the Invention

[0006] In view of this, the present invention provides a method for treating brewing yellow water using a combination of micro-nano bubble microwave microfluidic extraction and extracting effective components.

[0007] To solve the above-mentioned technical problems, the present invention adopts the following technical solution:

[0008] A method for treating brewing yellow water using a combination of micro / nano bubble microwave / microfluidic extraction and extracting effective components includes the following steps:

[0009] (1) Pretreatment of yellow liquor from brewing:

[0010] The collected yellow brewing water is filtered to remove suspended solids and large particulate impurities, resulting in clear yellow water.

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

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

[0013] (3) Microwave treatment:

[0014] The yellow water that has undergone the first micro-nano bubble treatment is placed in a microwave reactor and microwave-treated under set microwave power and temperature conditions to break down large organic molecules into smaller molecules and increase the amino acid content.

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

[0016] The microwave-treated yellow water is then re-entered into a micro-nano bubble generator, where air or oxygen is introduced for 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 to contact the extractant for extraction, thereby enriching and extracting the effective components.

[0019] (6) Product recycling:

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

[0021] (7) Waste liquid treatment:

[0022] The raffinate and waste liquid generated during the treatment process are discharged after meeting the standards, or are utilized as resources.

[0023] Preferably, in step (1), the filter 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 generator is 50-500 nm, and the gas residence time is 5-15 minutes.

[0025] Preferably, in step (2), the gas introduced for the micro-nano bubble treatment is air or pure oxygen, the gas flow rate is 0.5-1.5L / 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℃, and the treatment time is 10-40 minutes; the power and temperature are controlled in a related manner during the microwave treatment, and the temperature increases by 10-15℃ for every 100W increase in power.

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

[0028] Hydrophobic organic solvents include n-hexane and isopropanol; ionic liquids include tetrabutylammonium bromide and triethyl phosphate; amine compounds include triethylamine and diethylamine.

[0029] Preferably, in step (5), the extraction process is carried out in a microfluidic extraction device, the volume ratio of 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 order and number of times of the micro-nano bubble treatment and microwave treatment can be flexibly adjusted according to the characteristics of the wastewater and the 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 is discharged in compliance with standards or is utilized as a resource.

[0033] The present invention achieves the following technical effects compared to the prior art:

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

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

[0036] (3) Green and environmentally friendly process: The treatment process produces no harmful byproducts, which is in line with 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 turns waste into treasure and has good economic value.

[0038] (5) High scalability: The process is simple, the equipment is easy to obtain, and it is easy to promote and apply in brewing and other related industries. It is suitable for industrial application and has broad application prospects and promotion value. Attached Figure Description

[0039] Figure 1 This is a flowchart of the present invention;

[0040] Figure 2 This is a diagram of the micro / nano bubble generator of the present invention. Detailed Implementation

[0041] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0042] like Figure 1 As shown, this invention discloses a method for treating brewing yellow water using a combination of micro / nano bubble microwave / microfluidic extraction and extracting effective components, comprising the following steps:

[0043] (1) Pretreatment of yellow liquor from brewing:

[0044] The collected yellow brewing water is filtered to remove suspended solids and large particulate impurities, resulting in clear yellow water.

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

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

[0047] (3) Microwave treatment:

[0048] The yellow water that has undergone the first micro-nano bubble treatment is placed in a microwave reactor and microwave-treated under set microwave power and temperature conditions to break down large organic molecules into smaller molecules and increase the amino acid content.

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

[0050] The microwave-treated yellow water is then re-entered into a micro-nano bubble generator, where air or oxygen is introduced for 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 to contact the extractant for extraction, thereby enriching and extracting the effective components.

[0053] (6) Product recycling:

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

[0055] (7) Waste liquid treatment:

[0056] The raffinate and waste liquid generated during the treatment process are discharged after meeting the standards, or are utilized as resources.

[0057] In step (1), the filter screen 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 generator is 50-500 nm, and the gas residence time is 5-15 minutes.

[0059] In step (2), the gas introduced for micro-nano bubble treatment is air or pure oxygen, the gas flow rate is 0.5-1.5L / 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℃, and the treatment time is 10-40 minutes; the power and temperature are controlled in a related manner during the microwave treatment, and the temperature increases by 10-15℃ for every 100W increase in power.

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

[0062] Hydrophobic organic solvents include n-hexane and isopropanol; ionic liquids include tetrabutylammonium bromide and triethyl phosphate; amine compounds include triethylamine and diethylamine.

[0063] In step (5), the extraction process is carried out in a microfluidic extraction device, the volume ratio of 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 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%.

[0065] The sequence and number of treatments for micro- and nano-bubble treatments can be flexibly adjusted according to the characteristics of the wastewater and the treatment requirements.

[0066] In step (7), waste liquid treatment includes biochemical treatment, membrane filtration, and evaporation concentration processes to ensure that the waste liquid is discharged in compliance with standards or is utilized as a resource.

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

[0068] Example 1: Treatment of yellow liquor from brewing and extraction of glutamic acid

[0069] 1. Raw materials: Yellow liquor from brewing, containing approximately 500 mg / L of suspended solids (SS), approximately 20,000 mg / L of COD, and approximately 2% of total amino acids, of which approximately 0.5% is glutamic acid.

[0070] 2. Operating steps:

[0071] (1) Pretreatment of yellow liquor from brewing:

[0072] The yellow water is filtered through a filter screen to remove suspended solids and large particulate impurities, resulting in clear yellow water.

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

[0074] The pretreated yellow water was introduced into a micro-nano bubble generator, and air was introduced to perform the first micro-nano bubble treatment. The gas flow rate was 1L / 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] Yellow water that has undergone 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 ℃, and a treatment time of 20 minutes. This process broke down large organic molecules into smaller molecules, increased the amino acid concentration, and raised the total amino acid content from 2% to 3%.

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

[0078] The microwave-treated yellow water was then reintroduced into a micro-nano bubble generator, where pure oxygen was introduced for a second micro-nano bubble treatment. The gas flow rate was 1 L / min, and the treatment time was 60 minutes. This further reduced the COD, with a total COD reduction of up to 30%, and improved the purity of the liquid.

[0079] (5) Microfluidic extraction:

[0080] The treated yellow water was introduced into a microfluidic extraction device and subjected to contact extraction with the ionic liquid tetrabutylammonium bromide. The volume ratio of the ionic liquid tetrabutylammonium bromide to the 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 was concentrated and purified to obtain an enriched glutamic acid product;

[0083] (7) Waste liquid treatment:

[0084] The raffinate is treated biochemically and discharged in compliance with standards or recycled.

[0085] 3. Results Analysis:

[0086] In this embodiment, through combined processing, the glutamic acid content in brewing yellow water was successfully increased from 0.5% to 5%, and the extraction efficiency was greatly improved. Micro-nano bubble treatment and microwave treatment effectively reduced COD and improved liquid purity, providing good conditions for subsequent extraction. Microfluidic extraction technology achieved efficient and selective enrichment of glutamic acid.

[0087] Example 2: Treatment of yellow liquor from brewing and extraction of glycine

[0088] 1. Raw materials: Yellow liquor from brewing, with a COD of approximately 15000 mg / L and a total amino acid content of approximately 1%, of which glycine content is approximately 0.2%.

[0089] 2. Operating steps:

[0090] (1) Pretreatment of yellow liquor from brewing:

[0091] The collected yellow brewing water is filtered to remove suspended solids and large particulate impurities, resulting in clear yellow water.

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

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

[0094] (3) Microwave treatment:

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

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

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

[0098] (5) Microfluidic extraction:

[0099] The treated yellow water was introduced into a microfluidic extraction device and contacted with isopropanol for extraction. The volume ratio of isopropanol to yellow water was 1:1, and glycine was enriched from 0.2% to 2%, with an extraction rate of 75%.

[0100] (6) Product recycling:

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

[0102] (7) Waste liquid treatment:

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

[0104] 3. Results Analysis:

[0105] The glycine content was successfully increased from 0.2% to 2%;

[0106] Optimized microwave processing conditions increased the amount of amino acids produced;

[0107] Using isopropanol as the extractant offers good selectivity and is easy to operate.

[0108] Example 3: Optimization of micro / nano bubble processing parameters and analysis of synergistic effects

[0109] 1. Types of Gases (one)

[0111] (1) Pretreatment of yellow liquor from brewing:

[0112] The collected yellow brewing water is filtered to remove suspended solids and large particulate impurities, resulting in clear yellow water.

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

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

[0115] (3) Microwave treatment:

[0116] The yellow water that has undergone the first micro-nano bubble treatment is placed in a microwave reactor and microwaved at a power of 700W, a temperature of 80℃ and a time of 30 minutes to break down large organic molecules into smaller molecules and increase the amino acid content.

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

[0118] The microwave-treated yellow water is then reintroduced into a micro-nano bubble generator, where air is introduced for 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 subjected to contact extraction with the ionic liquid tetrabutylammonium bromide. The volume ratio of the ionic liquid tetrabutylammonium bromide to the 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 product of active ingredients;

[0123] (7) Waste liquid treatment:

[0124] The raffinate and waste liquid generated during the treatment process are discharged after meeting the standards, or are utilized as resources. (two)

[0126] (1) Pretreatment of yellow liquor from brewing:

[0127] The collected yellow brewing water is filtered to remove suspended solids and large particulate impurities, resulting in clear yellow water.

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

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

[0130] (3) Microwave treatment:

[0131] The yellow water that has undergone the first micro-nano bubble treatment is placed in a microwave reactor and microwaved at a microwave power of 700W, a temperature of 80℃ and a time of 30 minutes to break down large organic molecules into smaller molecules and increase the amino acid content.

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

[0133] The microwave-treated yellow water is then reintroduced into a micro-nano bubble generator, where oxygen is introduced for a second micro-nano bubble treatment to further reduce the organic matter content.

[0134] (5) Microfluidic extraction:

[0135] The treated yellow water was introduced into a microfluidic extraction device and subjected to contact extraction with the ionic liquid tetrabutylammonium bromide. The volume ratio of the ionic liquid tetrabutylammonium bromide to the 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 product of active ingredients;

[0138] (7) Waste liquid treatment:

[0139] The raffinate and waste liquid generated during the treatment process are discharged after meeting the standards, or are utilized as resources.

[0140] Results: Introducing oxygen was more effective than air, increasing COD removal rate by approximately 5%.

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

[0143] (1) Pretreatment of yellow liquor from brewing:

[0144] The collected yellow brewing water is filtered to remove suspended solids and large particulate impurities, resulting in clear yellow water.

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

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

[0147] (3) Microwave treatment:

[0148] The yellow water that has undergone the first micro-nano bubble treatment is placed in a microwave reactor and microwaved at a power of 700W, a temperature of 80℃ and a time of 30 minutes to break down large organic molecules into smaller molecules and increase the amino acid content.

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

[0150] The microwave-treated yellow water is then reintroduced into a micro-nano bubble generator, where oxygen is introduced for a second micro-nano bubble treatment to further reduce the organic matter content.

[0151] (5) Microfluidic extraction:

[0152] The treated yellow water was introduced into a microfluidic extraction device and subjected to contact extraction with the ionic liquid tetrabutylammonium bromide. The volume ratio of the ionic liquid tetrabutylammonium bromide to the 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 product of active ingredients;

[0155] (7) Waste liquid treatment:

[0156] The raffinate and waste liquid generated during the treatment process are discharged after meeting the standards, or are utilized as resources. (two)

[0158] (1) Pretreatment of yellow liquor from brewing:

[0159] The collected yellow brewing water is filtered to remove suspended solids and large particulate impurities, resulting in clear yellow water.

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

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

[0162] (3) Microwave treatment:

[0163] The yellow water that has undergone the first micro-nano bubble treatment is placed in a microwave reactor and microwaved at a power of 700W, a temperature of 80℃ and a time of 30 minutes to break down large organic molecules into smaller molecules and increase the amino acid content.

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

[0165] The microwave-treated yellow water is then reintroduced into a micro-nano bubble generator, where oxygen is introduced for a second micro-nano bubble treatment to further reduce the organic matter content.

[0166] (5) Microfluidic extraction:

[0167] The treated yellow water was introduced into a microfluidic extraction device and subjected to contact extraction with the ionic liquid tetrabutylammonium bromide. The volume ratio of the ionic liquid tetrabutylammonium bromide to the 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 product of active ingredients;

[0170] (7) Waste liquid treatment:

[0171] The raffinate and waste liquid generated during the treatment process are discharged after meeting the standards, or are utilized as resources. (three)

[0173] (1) Pretreatment of yellow liquor from brewing:

[0174] The collected yellow brewing water is filtered to remove suspended solids and large particulate impurities, resulting in clear yellow water.

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

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

[0177] (3) Microwave treatment:

[0178] The yellow water that has undergone the first micro-nano bubble treatment is placed in a microwave reactor and microwaved at a power of 700W, a temperature of 80℃ and a time of 30 minutes to break down large organic molecules into smaller molecules and increase the amino acid content.

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

[0180] The microwave-treated yellow water is then reintroduced into a micro-nano bubble generator, where oxygen is introduced for a second micro-nano bubble treatment to further reduce the organic matter content.

[0181] (5) Microfluidic extraction:

[0182] The treated yellow water was introduced into a microfluidic extraction device and subjected to contact extraction with the ionic liquid tetrabutylammonium bromide. The volume ratio of the ionic liquid tetrabutylammonium bromide to the 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 product of active ingredients;

[0185] (7) Waste liquid treatment:

[0186] The raffinate and waste liquid generated during the treatment process are discharged after meeting the standards, or are utilized as resources.

[0187] Results: Appropriately increasing the gas flow rate and treatment time improves the COD removal effect, but excessive increases have no significant effect.

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

[0190] (1) Pretreatment of yellow liquor from brewing:

[0191] The collected yellow brewing water is filtered to remove suspended solids and large particulate impurities, resulting in clear yellow water.

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

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

[0194] (3) Microwave treatment:

[0195] The yellow water that had undergone the first micro-nano bubble treatment was placed in a microwave reactor and microwave-treated at a power of 400W, a temperature of 60℃, and a time of 10 minutes to break down large organic molecules into smaller molecules and increase the amino acid content.

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

[0197] The microwave-treated yellow water is then reintroduced into a micro-nano bubble generator, where oxygen is introduced for a second micro-nano bubble treatment to further reduce the organic matter content.

[0198] (5) Microfluidic extraction:

[0199] The treated yellow water was introduced into a microfluidic extraction device and subjected to contact extraction with the ionic liquid tetrabutylammonium bromide. The volume ratio of the ionic liquid tetrabutylammonium bromide to the 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 product of active ingredients;

[0202] (7) Waste liquid treatment:

[0203] The raffinate and waste liquid generated during the treatment process are discharged after meeting the standards, or are utilized as resources. (two)

[0205] (1) Pretreatment of yellow liquor from brewing:

[0206] The collected yellow brewing water is filtered to remove suspended solids and large particulate impurities, resulting in clear yellow water.

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

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

[0209] (3) Microwave treatment:

[0210] The yellow water that has undergone the first micro-nano bubble treatment is placed in a microwave reactor and microwaved at a power of 700W, a temperature of 80℃ and a time of 30 minutes to break down large organic molecules into smaller molecules and increase the amino acid content.

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

[0212] The microwave-treated yellow water is then reintroduced into a micro-nano bubble generator, where oxygen is introduced for a second micro-nano bubble treatment to further reduce the organic matter content.

[0213] (5) Microfluidic extraction:

[0214] The treated yellow water was introduced into a microfluidic extraction device and subjected to contact extraction with the ionic liquid tetrabutylammonium bromide. The volume ratio of the ionic liquid tetrabutylammonium bromide to the 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 product of active ingredients;

[0217] (7) Waste liquid treatment:

[0218] The raffinate and waste liquid generated during the treatment process are discharged after meeting the standards, or are utilized as resources. (three)

[0220] (1) Pretreatment of yellow liquor from brewing:

[0221] The collected yellow brewing water is filtered to remove suspended solids and large particulate impurities, resulting in clear yellow water.

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

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

[0224] (3) Microwave treatment:

[0225] The yellow water that had undergone the first micro-nano bubble treatment was placed in a microwave reactor and microwave-treated at a microwave power of 1000W, a temperature of 10℃, and a time of 40 minutes to break down large organic molecules into smaller molecules and increase the amino acid content.

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

[0227] The microwave-treated yellow water is then reintroduced into a micro-nano bubble generator, where oxygen is introduced for a second micro-nano bubble treatment to further reduce the organic matter content.

[0228] (5) Microfluidic extraction:

[0229] The treated yellow water was introduced into a microfluidic extraction device and subjected to contact extraction with the ionic liquid tetrabutylammonium bromide. The volume ratio of the ionic liquid tetrabutylammonium bromide to the 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 product of active ingredients;

[0232] (7) Waste liquid treatment:

[0233] The raffinate and waste liquid generated during the treatment process are discharged after meeting the standards, or are utilized as resources.

[0234] Results: Increased microwave power and temperature are beneficial for macromolecular cleavage, but excessively high temperatures may lead to amino acid degradation; the optimal temperature is 80-90℃ and the time is 20-30 minutes.

[0235] 4. Types of extractants (one)

[0237] (1) Pretreatment of yellow liquor from brewing:

[0238] The collected yellow brewing water is filtered to remove suspended solids and large particulate impurities, resulting in clear yellow water.

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

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

[0241] (3) Microwave treatment:

[0242] The yellow water that has undergone the first micro-nano bubble treatment is placed in a microwave reactor and microwaved at a power of 700W, a temperature of 60℃ and a time of 30 minutes to break down large organic molecules into smaller molecules and increase the amino acid content.

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

[0244] The microwave-treated yellow water is then reintroduced into a micro-nano bubble generator, where oxygen is introduced for a second micro-nano bubble treatment to further reduce the organic matter content.

[0245] (5) Microfluidic extraction:

[0246] The treated yellow water was introduced into a microfluidic extraction device and subjected to contact extraction with the ionic liquid tetrabutylammonium bromide. The volume ratio of the ionic liquid tetrabutylammonium bromide to the 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 product of active ingredients;

[0249] (7) Waste liquid treatment:

[0250] The raffinate and waste liquid generated during the treatment process are discharged after meeting the standards, or are utilized as resources. (two)

[0252] (1) Pretreatment of yellow liquor from brewing:

[0253] The collected yellow brewing water is filtered to remove suspended solids and large particulate impurities, resulting in clear yellow water.

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

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

[0256] (3) Microwave treatment:

[0257] The yellow water that has undergone the first micro-nano bubble treatment is placed in a microwave reactor and microwaved at a power of 700W, a temperature of 60℃ and a time of 30 minutes to break down large organic molecules into smaller molecules and increase the amino acid content.

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

[0259] The microwave-treated yellow water is then reintroduced into a micro-nano bubble generator, where oxygen is introduced for a second micro-nano bubble treatment to further reduce the organic matter content.

[0260] (5) Microfluidic extraction:

[0261] The treated yellow water was introduced into a microfluidic extraction device and subjected to contact extraction with the amine compound triethylamine. The volume ratio of the ionic liquid tetrabutylammonium bromide to the 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 product of active ingredients;

[0264] (7) Waste liquid treatment:

[0265] The raffinate and waste liquid generated during the treatment process are discharged after meeting the standards, or are utilized as resources. (three)

[0267] (1) Pretreatment of yellow liquor from brewing:

[0268] The collected yellow brewing water is filtered to remove suspended solids and large particulate impurities, resulting in clear yellow water.

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

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

[0271] (3) Microwave treatment:

[0272] The yellow water that has undergone the first micro-nano bubble treatment is placed in a microwave reactor and microwaved at a power of 700W, a temperature of 60℃ and a time of 30 minutes to break down large organic molecules into smaller molecules and increase the amino acid content.

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

[0274] The microwave-treated yellow water is then reintroduced into a micro-nano bubble generator, where oxygen is introduced for a second micro-nano bubble treatment to further reduce the organic matter content.

[0275] (5) Microfluidic extraction:

[0276] The treated yellow water was introduced into a microfluidic extraction device and subjected to contact extraction with the organic solvent n-hexane. The volume ratio of the ionic liquid tetrabutylammonium bromide to the 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 product of active ingredients;

[0279] (7) Waste liquid treatment:

[0280] The raffinate and waste liquid generated during the treatment process are discharged after meeting the standards, or are utilized as resources.

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

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

[0284] (1) Pretreatment of yellow liquor from brewing:

[0285] The collected yellow brewing water is filtered to remove suspended solids and large particulate impurities, resulting in clear yellow water.

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

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

[0288] (3) Microwave treatment:

[0289] The yellow water that has undergone the first micro-nano bubble treatment is placed in a microwave reactor and microwaved at a power of 700W, a temperature of 60℃ and a time of 30 minutes to break down large organic molecules into smaller molecules and increase the amino acid content.

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

[0291] The microwave-treated yellow water is then reintroduced into a micro-nano bubble generator, where oxygen is introduced for a second micro-nano bubble treatment to further reduce the organic matter content.

[0292] (5) Microfluidic extraction:

[0293] The treated yellow water was introduced into a microfluidic extraction device and subjected to contact extraction with the ionic liquid tetrabutylammonium bromide. The volume ratio of the ionic liquid tetrabutylammonium bromide to the 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 product of active ingredients;

[0296] (7) Waste liquid treatment:

[0297] The raffinate and waste liquid generated during the treatment process are discharged after meeting the standards, or are utilized as resources. (two)

[0299] (1) Pretreatment of yellow liquor from brewing:

[0300] The collected yellow brewing water is filtered to remove suspended solids and large particulate impurities, resulting in clear yellow water.

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

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

[0303] (3) Microwave treatment:

[0304] The yellow water that has undergone the first micro-nano bubble treatment is placed in a microwave reactor and microwaved at a power of 700W, a temperature of 60℃ and a time of 30 minutes to break down large organic molecules into smaller molecules and increase the amino acid content.

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

[0306] The microwave-treated yellow water is then reintroduced into a micro-nano bubble generator, where oxygen is introduced for a second micro-nano bubble treatment to further reduce the organic matter content.

[0307] (5) Microfluidic extraction:

[0308] The treated yellow water was introduced into a microfluidic extraction device and subjected to contact extraction with the ionic liquid tetrabutylammonium bromide. The volume ratio of the ionic liquid tetrabutylammonium bromide to the 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 product of active ingredients;

[0311] (7) Waste liquid treatment:

[0312] The raffinate and waste liquid generated during the treatment process are discharged after meeting the standards, or are utilized as resources. (three)

[0314] (1) Pretreatment of yellow liquor from brewing:

[0315] The collected yellow brewing water is filtered to remove suspended solids and large particulate impurities, resulting in clear yellow water.

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

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

[0318] (3) Microwave treatment:

[0319] The yellow water that has undergone the first micro-nano bubble treatment is placed in a microwave reactor and microwaved at a power of 700W, a temperature of 60℃ and a time of 30 minutes to break down large organic molecules into smaller molecules and increase the amino acid content.

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

[0321] The microwave-treated yellow water is then reintroduced into a micro-nano bubble generator, where oxygen is introduced for a second micro-nano bubble treatment to further reduce the organic matter content.

[0322] (5) Microfluidic extraction:

[0323] The treated yellow water was introduced into a microfluidic extraction device and subjected to contact extraction with the ionic liquid tetrabutylammonium bromide. The volume ratio of the ionic liquid tetrabutylammonium bromide to the 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 product of active ingredients;

[0326] (7) Waste liquid treatment:

[0327] The raffinate and waste liquid generated during the treatment process are discharged after meeting the standards, or are utilized as resources.

[0328] Results: Increasing the amount of extractant and the extraction time improved the extraction rate, but cost and efficiency need to be considered.

[0329] Synergistic effect:

[0330] Micro- and nano-bubble treatment creates favorable conditions for microwave processing, reducing the viscosity and COD of the liquid; the small molecules generated by microwave treatment are beneficial for microfluidic extraction, increasing the mass transfer driving force; the close cooperation and synergistic effect of each step maximizes the processing effect.

[0331] The effects of gas type, flow rate, and processing time are shown in Table 1.

[0332] Table 1:

[0333] Air 1.0 60 20000 10％ pure oxygen 1.0 60 20000 15％

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

[0335] Table 2:

[0336] 600 80 25 50％ 800 90 20 60％ 1000 100 30 70％

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

[0338] The effects of microfluidic extraction parameters on glutamic acid extraction rate are shown in Table 3.

[0339] Table 3:

[0340]

[0341] Example 4: The Influence of Filter Mesh Count 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] 100 mesh 20 100 83.3％ 150 mesh 20 50 91.7％ 200 mesh 20 30 95％

[0347] The removal rate of suspended solids (SS) after filtration can reach 80%-95%.

[0348] The results are shown in Table 5:

[0349] Table 5:

[0350] 500 150 mesh 20 50 90％ 300 200 mesh 15 30 90％

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

[0352] Microwave temperature = 90℃, processing time = 20 minutes.

[0353] The results are shown in Table 6;

[0354] Table 6:

[0355] 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 rate. Raw material: glutamic acid = 0.5%.

[0357] Extractant: Tetrabutylammonium bromide, extraction time = 30 minutes.

[0358] The results are shown in Table 7;

[0359] Table 7:

[0360] 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 constitute any limitation on the technical scope of the present invention. Therefore, any minor modifications, equivalent changes, and alterations made to the above embodiments based on the technical essence of the present invention shall still fall within the scope of the technical solution of the present invention.

Claims

1. A method for treating brewing yellow water using a combination of micro / nano bubble microwave / microfluidic extraction and other methods to extract effective components, characterized in that... Includes the following steps: (1) Pretreatment of yellow liquor from brewing: The collected yellow brewing water is filtered to remove suspended solids and large particulate impurities, resulting in clear yellow water. (2) Micro-nano bubble treatment: The pretreated yellow water is introduced into a micro-nano bubble generator, and air or oxygen is introduced to perform the first micro-nano bubble treatment, which removes some organic matter and reduces COD. (3) Microwave treatment: The yellow water that has undergone the first micro-nano bubble treatment is placed in a microwave reactor and microwave-treated under set microwave power and temperature conditions to break down large organic molecules into smaller molecules and increase the amino acid content. (4) Secondary treatment of micro- and nano-bubbles: The microwave-treated yellow water is then re-entered into a micro-nano bubble generator, where air or oxygen is introduced for 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 to contact the extractant for extraction, thereby enriching and extracting the effective components. (6) Product recycling: The extract phase is concentrated and purified to obtain an enriched product of active ingredients; (7) Waste liquid treatment: The raffinate and waste liquid generated during the treatment process are discharged after meeting the standards, or are utilized as resources.

2. The method for combined micro / nano bubble microwave microfluidic extraction and treatment of brewing yellow water to extract effective components according to claim 1, characterized in that, In step (1), the filter mesh size is 100-200 mesh, and the filtration time is 10-30 minutes.

3. The method for combined micro / nano bubble microwave microfluidic extraction and treatment of brewing yellow water to extract effective components according to claim 1, characterized in that, In step (2), the diameter of the bubbles generated by the micro-nano bubble generator is 50-500 nm, and the gas residence time is 5-15 minutes.

4. The method for combined micro / nano bubble microwave microfluidic extraction and treatment of brewing yellow water to extract effective components according to claim 1, characterized in that, In step (2), the gas introduced for 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 for combined micro / nano bubble microwave microfluidic extraction and treatment of brewing yellow water to extract effective components according to claim 1, characterized in that, In step (3), the microwave power of the microwave treatment is 400-1000 W, the temperature is 60-100℃, and the treatment time is 10-40 minutes; the power and temperature are controlled in a related manner during the microwave treatment, and the temperature increases by 10-15℃ for every 100 W increase in power.

6. The method for combined micro / nano bubble microwave microfluidic extraction and treatment of brewing yellow water to extract effective components according to claim 1, characterized in that, In step (5), the extractant is a hydrophobic organic solvent, an ionic liquid, or an amine compound; wherein, Hydrophobic organic solvents include n-hexane and isopropanol; ionic liquids include tetrabutylammonium bromide and triethyl phosphate; amine compounds include triethylamine and diethylamine.

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

8. The method for combined micro / nano bubble microwave microfluidic extraction and treatment of brewing yellow water to extract effective components according to claim 1, characterized in that, In step (6), the extracted active ingredients include glutamic acid and glycine, and the extraction purity can be increased from the original content of 0.1%-2% to 1%-10%.

9. The method for combined micro / nano bubble microwave microfluidic extraction and treatment of brewing yellow water to extract effective components according to claim 1, characterized in that, In step (7), the waste liquid treatment includes biochemical treatment, membrane filtration, and evaporation concentration processes to ensure that the waste liquid is discharged in compliance with standards or is utilized as a resource.

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