Method for efficiently concentrating organic waste water of Maotai-flavor liquor

Abstract

This application discloses a method for efficiently concentrating organic wastewater from Maotai-flavor liquor in the field of liquor wastewater treatment technology. Addressing the problems of high energy consumption and easy component loss in traditional treatment technologies, this invention achieves wastewater resource utilization through a synergistic process of pretreatment, multi-stage molecular distillation, and ultrafiltration. First, suspended solids and heavy metals are removed through mechanical filtration and chemical precipitation. Then, the wastewater is sequentially passed through falling film, scraped film, and centrifugal molecular distillation devices to separate low-boiling-point substances under vacuum and low temperature, achieving a concentration factor of 5-10 times. Finally, a 10-50 nm ultrafiltration membrane is used to further enrich high-molecular-weight organic matter. The concentrated liquid can be directly used as fermentation raw material or for extracting flavor substances, providing an efficient solution for the high-value utilization of liquor wastewater.

Description

Technical Field

[0001] This invention relates to the field of liquor wastewater treatment technology, specifically to a method for efficiently concentrating organic wastewater from soy sauce-flavored liquor. Background Technology

[0002] Maotai-flavor liquor is one of the representatives of traditional Chinese brewing techniques, widely loved for its unique flavor and aroma. However, the production process of Maotai-flavor liquor generates a large amount of organic wastewater, which contains abundant organic matter, sugars, proteins, esters, and various trace elements. Although these organic components have certain resource utilization value, their low concentration and complex composition make direct treatment or utilization difficult.

[0003] Currently, the main methods for treating organic wastewater from liquor production include biodegradation, physicochemical methods (such as evaporation concentration and membrane separation), and combined processes. However, existing technologies still have some problems in practical applications: for example, traditional evaporation concentration technology has high energy consumption and is prone to the loss of low-boiling-point substances; while membrane separation technology can achieve a certain degree of concentration, its treatment efficiency for high-concentration wastewater is low, and it is easily affected by organic pollution, resulting in high operating costs. In addition, existing methods often fail to effectively preserve the activity and integrity of organic components during the treatment process, which poses a significant challenge to subsequent resource utilization. Summary of the Invention

[0004] The present invention aims to provide a method for efficiently concentrating organic wastewater from Maotai-flavor liquor, in order to solve the problems of high energy consumption, low treatment efficiency, and difficulty in preserving the activity of organic components in the existing technologies for treating organic wastewater from liquor.

[0005] To solve the above-mentioned technical problems, the present invention provides the following technical solution: a method for efficiently concentrating organic wastewater from Maotai-flavor liquor, comprising the following steps:

[0006] S1. Pretreatment stage: Remove suspended solids, impurities and heavy metal ions from wastewater through mechanical filtration and chemical precipitation;

[0007] S2, Molecular distillation concentration stage: The pretreated wastewater is sequentially passed through falling film, scraped film and centrifugal molecular distillation devices to separate low-boiling-point substances under vacuum conditions, thereby achieving high-efficiency concentration;

[0008] S3, Ultrafiltration Concentration Stage: The wastewater after molecular distillation is passed through an ultrafiltration system, using an ultrafiltration membrane with a pore size of 10-50nm to further concentrate high molecular weight organic matter.

[0009] S4. Collection and application of concentrate: Collect the concentrate for resource utilization and recover the separated low-boiling-point substances.

[0010] Furthermore, the mechanical filtration employs a multi-layer filter screen with a pore size of 0.5-1mm and a filtration speed of 1-2m / s. 3 / h.

[0011] Furthermore, the precipitant used in the chemical precipitation is ferrous sulfate, with an addition amount of 100-200 mg / L and a reaction time of 30-60 minutes.

[0012] Furthermore, the operating temperature of the falling film molecular distillation is 60-80℃, the vacuum degree is 1-10Pa, and the liquid film thickness is 0.1-3mm.

[0013] Furthermore, the operating temperature of the scraped-film molecular distillation is 50-70℃, the vacuum degree is 0.1-1Pa, the scraper rotation speed is 300-500rpm, and the liquid film thickness is 0.1-0.25mm.

[0014] Furthermore, the centrifugal molecular distillation is performed at an operating temperature of 40-60℃, a vacuum degree of 0.01-0.1 Pa, a turntable speed of 1000-2000 rpm, and a liquid film thickness of 5×10⁻⁶. -2 mm.

[0015] Furthermore, the operating pressure of the ultrafiltration stage is 0.2-0.6 MPa.

[0016] Furthermore, the concentration factor of the concentrate is 5-10 times.

[0017] Furthermore, according to any of the methods described above, the concentrate is used for the extraction of fermentation raw materials or functional components in the production of Maotai-flavor liquor.

[0018] The beneficial effects of this invention are as follows: 1. By combining multi-stage molecular distillation (falling film, scraped film, and centrifugal) with ultrafiltration technology, the useful components in wastewater are concentrated in stages, achieving a concentration factor of 5-10 times. 2. Molecular distillation operates under vacuum and low-temperature conditions, avoiding energy loss and component damage caused by high temperatures, reducing overall energy consumption by more than 30% compared to traditional evaporation methods. 3. The synergistic effect of low-temperature molecular distillation and ultrafiltration technologies preserves the activity and integrity of macromolecules such as sugars and proteins, providing high-quality raw materials for subsequent fermentation or extraction. 4. The separated low-boiling-point substances (such as alcohol and esters) can be recycled and reused, and the concentrate can be directly used in production, reducing processing costs and creating added value. 5. It reduces wastewater discharge, improves resource utilization, and meets the requirements of green production. Detailed Implementation

[0019] The following detailed description illustrates the specific implementation method:

[0020] Example 1:

[0021] A method for efficiently concentrating organic wastewater from Maotai-flavor liquor includes the following steps:

[0022] 1. Preprocessing stage

[0023] Mechanical filtration:

[0024] It employs a 3-layer filter system in series (pore sizes of 1mm, 0.8mm, and 0.5mm respectively), with a filtration speed of 1.5m / s. 3 / h, suspended solids removal rate reaches 92%, filtrate turbidity <5NTU.

[0025] Chemical precipitation:

[0026] Add 150 mg / L ferrous sulfate to the filtrate, stir for 45 minutes, allow to stand and precipitate, then take the supernatant. Heavy metals (such as Pb) will be present. 2 +、Cd 2 +) Removal rate > 95%, COD decreased from 8000 mg / L to 6500 mg / L.

[0027] 2. Molecular distillation concentration stage

[0028] Falling film molecular distillation:

[0029] Operating temperature 70℃, vacuum degree 5Pa, liquid film thickness 1mm, low boiling point substances (alcohol, esters) recovery rate 88%, wastewater volume reduced by 40%, COD increased to 10500mg / L.

[0030] Scraped membrane molecular distillation:

[0031] At a temperature of 60℃, a vacuum of 0.5Pa, a scraper speed of 400rpm, and a liquid film thickness of 0.2mm, low-boiling-point substances were further recovered (total recovery rate reached 95%), the volume was reduced by another 30%, and the COD reached 18000mg / L.

[0032] Centrifugal molecular distillation:

[0033] Temperature 50℃, vacuum degree 0.05Pa, turntable speed 1500rpm, liquid film thickness 0.04mm, final concentrated liquid volume is 10% of the original wastewater, COD reaches 55000mg / L (concentration factor 5.5 times).

[0034] 3. Ultrafiltration Concentration Stage

[0035] Membrane parameters: A polyethersulfone membrane with a molecular weight cutoff of 5000 Da was selected, and the operating pressure was 0.4 MPa.

[0036] Concentration effect: The retention rate of high molecular weight organic matter (protein, polysaccharide) is >90%, the volume of concentrated liquid is further reduced by 50%, the COD reaches 110000mg / L (total concentration multiple of 11 times), and 98% of small molecule salts are removed at the same time.

[0037] 4. Resource utilization

[0038] Application of concentrated liquid: Adding the concentrated liquid to the new mash at a ratio of 1:3 shortens the fermentation cycle by 12% and increases the alcohol yield by 3.2%.

[0039] Low-boiling-point substance recovery: The separated alcohol (92% purity) can be reused in production, and the ester extracts (aroma components) can be added to the finished wine as flavoring liquid.

[0040] Example 2: Parameter Optimization Experiment

[0041] Key parameters of molecular distillation were optimized through orthogonal experiments, and the results are as follows:

[0042] Centrifugation temperature (°C) 40 50 60 50 Vacuum level (Pa) 0.01 0.05 0.1 0.05 Rotational speed (rpm) 1000 1500 2000 1500 index COD Concentration Factor Alcohol recovery rate Protein retention rate optimal value 12.3 times 97.2％ 93.5％ L9(34)

[0043] Comparison of implementation results:

[0044] Processing cost (RMB / ton) 6.8 11.5 9.2 COD Concentration Factor 11 times 6 times 8 times Alcohol recovery rate 95％ 60％ 80％ Protein retention rate 92％ 45％ 75％ Operation cycle (days / time) 7 5 6

[0045] Precautions

[0046] Equipment selection: Select the molecular distillation unit specifications based on the wastewater treatment capacity (e.g., a treatment capacity of 5m³). 3 For a flow rate of [number] h, a centrifugal distiller diameter of 1.2 m is recommended.

[0047] Membrane fouling control: Before ultrafiltration, the membrane module needs to be filtered through a precision filter (0.2μm filter cartridge) to prevent large molecules from clogging the membrane pores. The membrane module should be cleaned regularly with NaOH solution (pH=12).

[0048] Vacuum system maintenance: Molecular distillation vacuum pumps need to be equipped with cold traps (-50℃) to capture volatiles and avoid oil contamination. Vacuum pump oil needs to be changed every 100 hours of operation.

[0049] Through the above implementation methods, the present invention can achieve efficient concentration and resource utilization of soy sauce-flavored liquor wastewater, providing a reliable technical solution for clean production in the liquor industry.

[0050] The above descriptions are merely embodiments of the present invention, and common knowledge regarding specific structures and characteristics is not elaborated upon here. It should be noted that those skilled in the art can make various modifications and improvements without departing from the structure of the present invention, and these should also be considered within the scope of protection of the present invention. These modifications and improvements will not affect the effectiveness of the present invention or the practicality of the patent. The scope of protection claimed in this application should be determined by the content of its claims, and the specific embodiments described in the specification can be used to interpret the content of the claims.

Claims

1. A method for efficiently concentrating organic wastewater from Maotai-flavor liquor, characterized in that, Includes the following steps: S1. Pretreatment stage: Remove suspended solids, impurities and heavy metal ions from wastewater through mechanical filtration and chemical precipitation; S2, Molecular distillation concentration stage: The pretreated wastewater is sequentially passed through falling film, scraped film and centrifugal molecular distillation devices to separate low-boiling-point substances under vacuum conditions, thereby achieving high-efficiency concentration; The operating temperature of falling film molecular distillation is 60-80℃ and the vacuum degree is 1-10 Pa; the operating temperature of scraped film molecular distillation is 50-70℃ and the vacuum degree is 0.1-1 Pa; and the operating temperature of centrifugal molecular distillation is 40-60℃ and the vacuum degree is 0.01-0.1 Pa. S3, Ultrafiltration Concentration Stage: The wastewater after molecular distillation is passed through an ultrafiltration system, using an ultrafiltration membrane with a pore size of 10-50 nm to further concentrate high molecular weight organic matter. S4. Collection and application of concentrated liquid: Collect the concentrated liquid obtained in step S3 for resource utilization and recover the separated low-boiling-point substances.

2. The method for efficiently concentrating organic wastewater from soy sauce-flavored liquor according to claim 1, characterized in that: The mechanical filtration employs a multi-layer filter screen with a pore size of 0.5-1 mm and a filtration velocity of 1-2 m / s. 3 / h.

3. The method for efficiently concentrating organic wastewater from soy sauce-flavored liquor according to claim 2, characterized in that: The precipitant used in the chemical precipitation is ferrous sulfate, with an addition amount of 100-200 mg / L and a reaction time of 30-60 minutes.

4. A method for efficiently concentrating organic wastewater from soy sauce-flavored liquor according to claim 3, characterized in that: The liquid film thickness of the falling film molecular distillation is 0.1-3 mm.

5. A method for efficiently concentrating organic wastewater from soy sauce-flavored liquor according to claim 4, characterized in that: The scraper rotation speed of the scraper in the scraped film molecular distillation is 300-500 rpm, and the liquid film thickness is 0.1-0.25 mm.

6. A method for efficiently concentrating organic wastewater from soy sauce-flavored liquor according to claim 5, characterized in that: The centrifugal molecular distillation process uses a rotating disk with a rotation speed of 1000-2000 rpm and a liquid film thickness of 5×10⁻⁶. -2 mm.

7. A method for efficiently concentrating organic wastewater from soy sauce-flavored liquor according to claim 6, characterized in that: The operating pressure of the ultrafiltration concentration stage is 0.2-0.6 MPa.

8. The method for efficiently concentrating organic wastewater from soy sauce-flavored liquor according to claim 7, characterized in that: The concentration factor of the concentrate is 5-10 times.

9. The application of the method according to any one of claims 1-8, characterized in that: The concentrate is used for the extraction of fermentation raw materials or functional components in the production of Maotai-flavor liquor.