Method for treating waste liquid in production process of momordica grosvenori extract

Abstract

The invention provides a method for treating waste liquid generated in the production process of a momordica grosvenori extract. The method comprises the following steps: collecting the waste liquid generated in the production process of the momordica grosvenori extract; filtering to remove insoluble impurities in the waste liquid; the filtered waste liquid is subjected to electrodialysis separation treatment, and recycled waste liquid with the concentration reaching the standard is obtained; and carrying out post-treatment on the recovered waste liquid with the concentration reaching the standard to obtain recovered liquid. The invention provides a new path for acid and alkali recovery and cyclic utilization of siraitia grosvenorii deep processing enterprises; the consumption of acid and alkali in the production process of the siraitia grosvenorii extract is greatly reduced, and the cost of a siraitia grosvenorii deep processing auxiliary agent is greatly reduced.

Description

Technical Field

[0001] The present application belongs to the field of Momordica grosvenori, and specifically relates to a method for treating waste liquid in the production process of Momordica grosvenori extract, specifically waste acid liquid and / or waste alkali liquid. Background Art

[0002] In the large-scale application of the monk fruit industry, while a small amount of mature monk fruit is dried into dried fruit for use in the pharmaceutical and primary food processing industries, the majority of the fruit is used for deep processing into monk fruit extract. The main products can be divided into three categories: mogroside, monk fruit concentrate, and monk fruit powder. The production of monk fruit extract generally involves raw material crushing, extraction, clarification and filtration, adsorption separation, decolorization, concentration, and drying. The macroporous resin in the adsorption separation process and the anionic resin in the decolorization process both require large amounts of strong alkaline sodium hydroxide solution for regeneration. A portion of this sodium hydroxide directly participates in ion exchange and acid-base neutralization, while the remaining 70%-85% remains in the regeneration waste caustic soda. The ceramic membranes or spiral membranes used for extract clarification, filtration, and concentration are also mostly regenerated using strong alkaline cleaning. The resulting waste caustic soda is ultimately discharged into the sewage system, resulting in a significant waste of resources and a significant burden on alkaline wastewater treatment, significantly increasing the acid consumption required for neutralization. In addition, a certain amount of waste acid containing sulfuric acid will be produced during the regeneration process of cationic resin. Therefore, in the cost structure of processing aids for monk fruit extract, the cost of acid and alkali is usually higher, second only to alcohol.

[0003] Charged membranes (also known as ion exchange membranes) are polymer membranes with fixed charged groups on their surface or in their bulk. They achieve separation through the attraction or repulsion of ions in the separation medium, utilizing sieving and the Donnan effect. Charged membrane separation technology offers unique advantages, including low energy consumption, high efficiency, simple and easy operation, and the absence of chemicals. It has become an effective means of addressing current major energy and environmental challenges and is considered the technological foundation for achieving sustainable development strategies. Charged membrane technology is now widely used in the treatment of acidic, alkaline, and saline wastewater in the food, pharmaceutical, biological, environmental protection, chemical, metallurgical, energy, petroleum, and water treatment industries, generating significant economic and social benefits. Charged membranes have the ability to selectively permeate ions in solution. They consist of three components: a polymer backbone, fixed groups, and mobile ions. Charged membranes are primarily categorized by charge type into anion exchange membranes (anion exchange membranes) and cation exchange membranes (cation exchange membranes). The fixed groups in the polymer backbone of anion exchange membranes carry a positive charge, selectively permeating anions while blocking cations. The fixed groups in the polymer backbone of cation exchange membranes carry a negative charge, selectively permeating cations while blocking anions. According to the application field and membrane material, it can also be divided into standard membranes suitable for general desalination and concentration processes, dense membranes suitable for high-concentration brine systems, and alkali-resistant membranes suitable for strong acid or strong alkaline systems.

[0004] At present, there has been no successful report on the application of alkali-resistant charged membrane technology in the recovery and recycling of waste alkali generated during the deep processing of Momordica grosvenori. Summary of the Invention

[0005] To solve the above problems, this application provides the following solutions:

[0006] 1. A method for treating waste liquid in the production process of Momordica grosvenori extract, comprising:

[0007] Collect waste liquid generated during the production of monk fruit extract;

[0008] Filtration to remove insoluble impurities from wastewater;

[0009] The filtered waste liquid is subjected to electrodialysis separation treatment to obtain a recovered waste liquid with a concentration meeting the standard;

[0010] Post-processing the recovered waste liquid with concentration meeting the standards to obtain a recovered liquid;

[0011] The waste liquid is waste acid liquid and / or waste alkali liquid, and the recovered liquid is recovered acid liquid and / or recovered alkali liquid.

[0012] 2. The method according to claim 1, wherein

[0013] The post-treatment is adsorption treatment or clarification treatment.

[0014] 3. The method according to claim 2, wherein:

[0015] The adsorption treatment is selected from any one of bentonite adsorption treatment, diatomaceous earth adsorption treatment, activated carbon adsorption treatment, silica gel adsorption treatment, and alumina adsorption treatment; or,

[0016] The clarification treatment is any one of diatomaceous earth clarification treatment, bentonite clarification treatment, perlite clarification treatment, cellulose clarification treatment, and clay clarification treatment.

[0017] 4. The method according to claim 1, wherein

[0018] The electrodialysis separation treatment uses an acid-resistant homogeneous ion exchange membrane or an alkali-resistant homogeneous ion exchange membrane;

[0019] Preferably,

[0020] The membrane pore diameter of the acid-resistant homogeneous ion exchange membrane or the alkali-resistant homogeneous ion exchange membrane is 0.1 nm to 0.5 nm, preferably 0.1 nm to 0.3 nm.

[0021] 5. The method according to claim 1, wherein

[0022] The light transmittance of the recovered acid solution at an acid concentration of 40 g / L and a wavelength of 625 nm is ≥90%; and / or,

[0023] The light transmittance of the recovered alkali solution is greater than or equal to 95% when the alkali concentration is 40 g / L and the wavelength is 625 nm.

[0024] 6. The method according to claim 1, wherein

[0025] The acid concentration in the recovered waste acid solution that meets the concentration standard is 40g / L to 80g / L, preferably 50g / L; or

[0026] The concentration of alkali in the recovered waste alkali solution that meets the concentration standard is 40g / L to 80g / L, preferably 50g / L.

[0027] 7. The method according to claim 6, wherein

[0028] The acid recovery rate in the electrodialysis separation treatment is ≥60%, or the alkali recovery rate is ≥70%.

[0029] 8. The method according to claim 1, wherein

[0030] The waste acid liquid refers to the waste liquid generated during the regeneration process of cationic resin acid in the production process of Momordica grosvenori extract, and the acid concentration range is 5g / L to 50g / L; and / or,

[0031] The waste alkali liquor comprises any one of the waste alkali liquors generated in the macroporous adsorption resin regeneration process, the decolorization anion resin alkali regeneration process and the ceramic membrane cleaning process during the production of the monk fruit extract, and the alkali concentration range is 5g / L to 50g / L;

[0032] Preferably,

[0033] The acid in the waste acid liquid is sulfuric acid; and / or,

[0034] The alkali in the waste alkali liquor is sodium hydroxide.

[0035] 9. The method according to claim 1, wherein

[0036] The filtration is one or more of sand rod filtration, plate and frame filtration, stainless steel folded filter element filtration, disc filtration, activated carbon filtration, high-efficiency fiber filtration, PP cotton filter element filtration, and microporous membrane cross-flow filtration.

[0037] 10. Use of the recovered liquid obtained by the method according to any one of items 1 to 9 in resin regeneration;

[0038] Preferably, the resin regeneration is macroporous adsorption resin regeneration or ion exchange resin regeneration.

[0039] 11. Use of the recovered liquid obtained by the method described in any one of items 1 to 9 in the cleaning and regeneration of ceramic membranes, wherein the recovered liquid is a recovered alkali solution.

[0040] Through the above technical solution, this application can produce the following beneficial effects:

[0041] 1. It provides a new path for the acid and alkali recovery and recycling of monk fruit deep processing enterprises.

[0042] 2. It greatly saves the consumption of acid and alkali in the production process of monk fruit extract, and significantly reduces the cost of monk fruit deep processing additives.

[0043] 3. Greatly reduces the emission of acid and alkali in the production process of monk fruit extract and the acid consumption used to neutralize alkaline wastewater, reduces the pressure on sewage treatment and saves costs.

[0044] 4. The process scheme of the present application provides a good technical reference for recovering and purifying the functional and flavor substances lost in the waste alkali solution during the production process of monk fruit extract, so as to achieve low-cost development of products with higher added value, turn waste into treasure, save resources, and promote the development of monk fruit deep processing enterprises in the direction of resource conservation and environmental friendliness.

[0045] 5. The process of this application has high efficiency in recovering waste acid and alkali generated in the production of monk fruit extract, and has the advantages of good quality of recovered auxiliary agents, high food safety, good process continuity, stable operation of core equipment, and easy cleaning and recovery. In terms of solid recovery rate, glycoside recovery rate and sensory indicators, the effect of regenerating resin by using a combination of recycled acid and alkali in whole or in part with new acid and alkali is no different from that of regeneration using new acid and alkali alone. The effect of regenerated alkali for cleaning ceramic membranes is also the same as that of cleaning with new alkali. DETAILED DESCRIPTION

[0046] The present application is further described below with reference to examples. It should be understood that the examples are only used to further illustrate and explain the present application and are not intended to limit the present application.

[0047] Unless otherwise defined, technical and scientific terms used in this specification have the same meaning as those commonly understood by those skilled in the art. Although methods and materials similar or identical to those described herein may be used in experiments or practical applications, the materials and methods are described herein below. In the event of a conflict, the present specification, including definitions, will prevail. In addition, the materials, methods, and examples are provided for illustrative purposes only and are not intended to be limiting. The present application is further described below with reference to specific examples, which are not intended to limit the scope of this application.

[0048] It should be noted that the endpoints and any values ​​of the various index ranges disclosed in the examples herein are not limited to the precise ranges or values ​​of the indexes, and these data ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of each range, the endpoint values ​​of each range and individual point values, and the individual point values ​​can be combined with each other to obtain one or more new numerical ranges, and these numerical ranges should be considered to be specifically disclosed herein.

[0049] Furthermore, it should be understood that the one or more method steps mentioned in the present invention do not exclude the presence of other method steps before or after the combination step, or the insertion of other method steps between these explicitly mentioned steps, unless otherwise specified. It should also be understood that the combination connection relationship between one or more devices / apparatuses mentioned in the present invention does not exclude the presence of other devices / apparatuses before or after the combination device / apparatus, or the insertion of other devices / apparatuses between two explicitly mentioned devices / apparatuses, unless otherwise specified. Furthermore, unless otherwise specified, the numbering of each method step is merely a convenient tool for identifying each method step, and is not intended to limit the order of arrangement of each method step or to define the scope of the present invention. Changes or adjustments to their relative relationships, without substantially changing the technical content, should also be considered within the scope of the present invention.

[0050] In addition, those skilled in the art can easily understand the advantages of the present invention and the various branch technical points that are not fully mentioned in the limited specific embodiments from the technical solutions and ideas disclosed in this specification, such as the selection of waste alkali liquid clarification equipment, optimization of the ratio of recovered acid and alkali, selection of resin regeneration conditions, etc. Therefore, any process invention in the art that uses alkali-resistant charged membranes to recover waste acid and alkali liquid in the production process of monk fruit extract, or attempts to use acid-resistant and alkali-resistant microfiltration, nanofiltration, etc. in combination with alkali-resistant charged membranes to implement alkali recovery, should be regarded as the scope of implementation of the present invention, and are applicable to the routes and methods provided by the present invention.

[0051] The present application provides a method for treating waste liquid in the production process of Monk Fruit Extract, which comprises: collecting waste liquid generated in the production process of Monk Fruit Extract; filtering to remove insoluble impurities in the waste liquid; performing electrodialysis separation treatment on the filtered waste liquid to obtain recycled waste liquid with a concentration that meets the standard; performing post-treatment on the recycled waste liquid with a concentration that meets the standard to obtain a recycled liquid; the waste liquid is waste acid liquid and / or waste alkali liquid, and the recovered liquid is recovered acid liquid and / or recovered alkali liquid.

[0052] The applicant has discovered that the production of monk fruit extract places high demands on the quality of additives such as acids, alkalis, and alcohol. The waste acid and alkaline water produced during the processing not only contain organic impurities such as insoluble particles, plant fibers, pigments, polysaccharides, deformed proteins, and organic acid salts, but also contain a large amount of inorganic salt components, usually accompanied by odors caused by microbial fermentation of the liquid components. Recycling and reuse are relatively difficult. However, if efficient recycling and reuse can be achieved, the consumption of acid and alkaline additives in the production of monk fruit extract will be greatly reduced, reducing production costs. Factors such as acid and alkali recovery efficiency, membrane cleaning and recovery performance, recovered acid and alkali quality, recycled acid and alkali recycling effect, and food safety of recycled acid and alkali recycling are all key factors that determine whether charged membrane electrodialysis acid and alkali recovery technology can be successfully applied to the recovery and recycling of waste acid and alkaline water in the monk fruit deep processing industry. In order to solve this problem, the applicant found through experiments that introducing electrodialysis separation treatment into the waste acid and alkali recovery process in the production process of monk fruit extract can well solve the above series of problems; it not only evaluated the recovered acid and alkali that can be used in the production process of monk fruit, but also ensured the flavor of monk fruit.

[0053] In some embodiments of the present application, the post-treatment is adsorption treatment or clarification treatment.

[0054] In some embodiments of the present application, the adsorption treatment is selected from any one of bentonite adsorption treatment, diatomaceous earth adsorption treatment, activated carbon adsorption treatment, silica gel adsorption treatment, and alumina adsorption treatment, preferably activated carbon adsorption treatment.

[0055] The applicant found that after the recycled waste liquid was treated with electrodialysis separation, trace components would migrate, but after adsorption treatment, impurities could be well removed.

[0056] In some embodiments of the present application, the clarification treatment is any one of diatomaceous earth clarification treatment, bentonite clarification treatment, perlite clarification treatment, cellulose clarification treatment, and clay clarification treatment, preferably diatomaceous earth clarification treatment.

[0057] In some embodiments of the present application, the electrodialysis separation treatment uses an acid-resistant homogeneous ion exchange membrane or an alkali-resistant homogeneous ion exchange membrane.

[0058] This application does not impose any restrictions on the electrodialysis equipment, as long as it meets the purpose of this application.

[0059] In some embodiments of the present application, the membrane pore size of the acid-resistant homogeneous ion exchange membrane or the alkali-resistant homogeneous ion exchange membrane is between 0.1 nm and 0.5 nm, preferably between 0.1 nm and 0.3 nm. For example, the membrane pore size can be 0.1 nm, 0.11 nm, 0.12 nm, 0.13 nm, 0.14 nm, 0.15 nm, 0.16 nm, 0.17 nm, 0.18 nm, 0.19 nm, 0.2 nm, 0.21 nm, 0.22 nm, 0.23 nm, 0.24 nm, 0.25 nm, 0.26 nm, 0.27 nm, 0.28 nm, 0.29 nm, 0. 3 nm, 0.31 nm, 0.32 nm, 0.33 nm, 0.34 nm, 0.35 nm, 0.36 nm, 0.37 nm, 0.38 nm, 0.39 nm, 0.4 nm, 0.41 nm, 0.42 nm, 0.43 nm, 0.44 nm, 0.45 nm, 0.46 nm, 0.47 nm, 0.48 nm, 0.49 nm, 0.5 nm, or any range therebetween.

[0060] In some embodiments of the present application, the operating temperature of the electrodialysis separation treatment is 15 to 45°C; for example, the operating temperature of the electrodialysis separation treatment can be 15°C, 20°C, 25°C, 30°C, 35°C, 40°C, 45°C or any range therebetween.

[0061] In some embodiments of the present application, the circulating pump pressure of the electrodialysis separation treatment is 0.03 to 0.1 MPa; for example, the circulating pump pressure of the electrodialysis separation treatment can be 0.03 MPa, 0.04 MPa, 0.05 MPa, 0.06 MPa, 0.07 MPa, 0.08 MPa, 0.09 MPa, 0.1 MPa or any range therebetween.

[0062] The applicant discovered that under specific conditions, the transmittance of recycled acid solution or recycled alkali solution meets certain conditions.

[0063] In some embodiments of the present application, the light transmittance of the recovered acid solution is ≥90% when the acid concentration is 40 g / L and the wavelength is 625 nm.

[0064] In some embodiments of the present application, the light transmittance of the recovered alkali solution is ≥95% when the alkali concentration is 40 g / L and the wavelength is 625 nm.

[0065] In some embodiments of the present application, the concentration of the acid in the recycled waste acid solution that meets the concentration standard is 40 g / L to 80 g / L, preferably 50 g / L; for example, the concentration of the acid in the recycled waste acid solution that meets the concentration standard can be 40 g / L, 45 g / L, 50 g / L, 55 g / L, 60 g / L, 65 g / L, 70 g / L, 75 g / L, 80 g / L or any range therebetween.

[0066] In some embodiments of the present application, the concentration of alkali in the recycled waste alkali liquid that meets the concentration standard is 40g / L to 80g / L, preferably 50g / L; for example, the concentration of alkali in the recycled waste alkali liquid that meets the concentration standard can be 40g / L, 45g / L, 50g / L, 55g / L, 60g / L, 65g / L, 70g / L, 75g / L, 80g / L or any range therebetween.

[0067] In some embodiments of the present application, the acid recovery rate of the recovered acid solution in the electrodialysis separation treatment is ≥60%.

[0068] In some embodiments of the present application, the alkali recovery rate of the recovered alkali solution in the electrodialysis separation treatment is ≥70%.

[0069] In this article, the recovery rate in the electrodialysis separation treatment refers to the recovery rate of the electrodialysis separation treatment step, wherein the acid recovery rate and the alkali recovery rate are calculated as follows: acid recovery rate (%) = total amount of inorganic acid in the recovered acid solution ÷ total amount of inorganic acid in the waste acid solution × 100%; alkali recovery rate (%) = total amount of alkali in the recovered alkali solution ÷ total amount of alkali in the waste alkali solution × 100%.

[0070] In some embodiments of the present application, the waste acid liquid refers to the waste liquid generated in the regeneration process of cationic resin acid during the production of Momordica grosvenori extract, and the acid concentration range is 5g / L to 50g / L; for example, the acid concentration range can be 5g / L, 10g / L, 15g / L, 20g / L, 25g / L, 30g / L, 35g / L, 40g / L, 45g / L, 50g / L or any range therebetween.

[0071] In some embodiments of the present application, the acid in the waste acid solution is sulfuric acid.

[0072] In some embodiments of the present application, the waste alkali liquor includes any one of the waste alkali liquors generated in the macroporous adsorption resin regeneration process, the decolorization anion resin alkali regeneration process and the ceramic membrane cleaning process during the production of the monk fruit extract, and the alkali concentration range is 5g / L to 50g / L; for example, the alkali concentration can be 5g / L, 10g / L, 15g / L, 20g / L, 25g / L, 30g / L, 35g / L, 40g / L, 45g / L, 50g / L or any range therebetween.

[0073] In some embodiments of the present application, the alkali in the waste alkali solution is sodium hydroxide.

[0074] In some embodiments of the present application, the filtration is one or more of sand rod filtration, plate and frame filtration, stainless steel pleated filter element filtration, disc filtration, activated carbon filtration, high-efficiency fiber filtration, PP cotton filter element filtration, and microporous membrane cross-flow filtration, preferably PP cotton filter element filtration.

[0075] The present application provides the use of the above-mentioned recovery liquid in resin regeneration.

[0076] In some embodiments of the present application, the resin regeneration is macroporous adsorption resin regeneration or ion exchange resin regeneration.

[0077] The present application provides the use of the above-mentioned recovered alkali solution in the cleaning and regeneration of ceramic membranes.

[0078] In some embodiments of the present application, the method for treating waste alkali liquor during the production of Monk Fruit Extract comprises:

[0079] (1) collecting waste alkali liquor generated in the production process of the monk fruit extract, wherein the waste alkali liquor includes any one of the waste alkali liquors generated in the regeneration process of the macroporous adsorption resin, the alkali regeneration process of the decolorization anion resin, and the ceramic membrane cleaning process in the production process of the monk fruit extract, and the alkali concentration range is 5 g / L to 50 g / L;

[0080] (2) PP cotton filter to remove insoluble impurities in the waste alkali solution;

[0081] (3) performing electrodialysis separation on the filtered waste alkali liquor to obtain a recovered waste alkali liquor having a concentration meeting the standard, wherein the electrodialysis separation uses an acid-resistant homogeneous ion exchange membrane or an alkali-resistant homogeneous ion exchange membrane, the operating temperature of the electrodialysis separation is 15 to 45° C., and the circulating pump pressure of the electrodialysis separation is 0.03 to 0.1 MPa; the concentration of alkali in the recovered alkali liquor having a concentration meeting the standard is 40 g / L to 80 g / L, preferably 50 g / L; and the alkali recovery rate of the recovered alkali liquor in the electrodialysis separation is ≥70%;

[0082] (4) performing activated carbon adsorption treatment on the recovered waste alkali liquor having a concentration meeting the standard to obtain a recovered alkali liquor, wherein the recovered alkali liquor has a transmittance of ≥95% at an alkali concentration of 40 g / L and a wavelength of 625 nm;

[0083] (5) Using the recovered alkali solution to match the concentration in the production process or combining it with new alkali for regeneration of macroporous adsorption resin, specifically:

[0084] The macroporous adsorption resins used in the adsorption production process of the mogroside extract were respectively taken and loaded into the chromatography columns, wherein each column was respectively used with a recovered alkali solution, and the flow rate was 1BV / h. After the recovered alkali solution was introduced into the experimental column, the newly configured alkali solution was continuously introduced and passed through the column in a forward direction, and then the purified water was used to wash the column in a forward direction until the pH of the effluent was ≤10, and then 0.2BV-0.5BV4% citric acid solution was used to treat the column in a forward direction, and then the purified water was used to wash the column in a forward direction until the pH of the effluent was neutral;

[0085] The above-mentioned resin columns are respectively fed with water extracts of Momordica grosvenori containing mogroside V, washed with water after feeding, eluted with alcohol, and the eluates are collected, concentrated, and tested for mogroside V and taste;

[0086] (6) Collect the waste acid and alkali solution after use and recycle it for reuse.

[0087] In some embodiments of the present application, the method for treating waste alkali liquor during the production of Monk Fruit Extract comprises:

[0088] (1) collecting waste alkali liquor generated in the production process of the monk fruit extract, wherein the waste alkali liquor includes any one of the waste alkali liquors generated in the regeneration process of the macroporous adsorption resin, the alkali regeneration process of the decolorization anion resin, and the ceramic membrane cleaning process in the production process of the monk fruit extract, and the alkali concentration range is 5 g / L to 50 g / L;

[0089] (2) PP cotton filter to remove insoluble impurities in the waste alkali solution;

[0090] (3) performing electrodialysis separation on the filtered waste alkali solution to obtain a recovered waste alkali solution having a concentration meeting the standard; the electrodialysis separation treatment uses an acid-resistant homogeneous ion exchange membrane or an alkali-resistant homogeneous ion exchange membrane, the operating temperature of the electrodialysis separation treatment is 15 to 45° C., and the circulating pump pressure of the electrodialysis separation treatment is 0.03 to 0.1 MPa; the concentration of alkali in the recovered alkali solution having a concentration meeting the standard is 40 g / L to 80 g / L, preferably 50 g / L; and the alkali recovery rate of the recovered alkali solution in the electrodialysis separation treatment is ≥70%;

[0091] (4) performing diatomaceous earth clarification treatment on the recovered waste alkali liquor having a concentration meeting the standard to obtain a recovered alkali liquor, wherein the recovered alkali liquor has a light transmittance of ≥95% at an alkali concentration of 40 g / L and a wavelength of 625 nm;

[0092] (5) The recovered alkali liquor is used in the production process to match the concentration or is combined with new alkali for the clarification and regeneration production of ceramic membranes, specifically:

[0093] The water extract of Luo Han Guo (Sheng Guo) was obtained from the production line of Guilin Jifusi Luo Han Guo Biotechnology Co., Ltd. after centrifugation in a horizontal screw centrifuge. Part of the water extract was clarified using an experimental ceramic membrane. The used experimental ceramic membrane was circulated and cleaned with a new alkali solution prepared with a solid base, and then circulated and cleaned several times with purified water until the pH of the circulating water was neutral. This was set as the control group. Part of the water extract was further clarified using an experimental ceramic membrane; the experimental ceramic membrane was circulated and cleaned with recycled alkali solution, and the subsequent steps were consistent with the regeneration process of the control group. This was set as the experimental group, and the remaining water extract was clarified using an experimental ceramic membrane.

[0094] After each regeneration and cleaning is completed, purified water is added to the ultrafiltration machine, and the flux of the clear liquid is monitored at a membrane inlet pressure of 0.1 MPa. Samples are taken to monitor the taste of each clarified liquid.

[0095] (6) Collect the used waste alkali again for recycling and reuse.

[0096] In some embodiments of the present application, the method for treating waste liquid during the production of Monk Fruit Extract includes:

[0097] (1) collecting waste acid liquid generated during the production of Momordica grosvenori extract, wherein the waste acid liquid refers to the waste liquid generated during the regeneration process of cationic resin acid during the production of Momordica grosvenori extract, and the acid concentration range is 5 g / L to 50 g / L;

[0098] (2) PP cotton filter element removes insoluble impurities in the waste acid solution;

[0099] (3) performing electrodialysis separation on the filtered waste acid solution to obtain a recovered waste acid solution having a concentration meeting the standard; the electrodialysis separation treatment uses an acid-resistant homogeneous ion exchange membrane or an alkali-resistant homogeneous ion exchange membrane, the operating temperature of the electrodialysis separation treatment is 15 to 45° C., and the circulating pump pressure of the electrodialysis separation treatment is 0.03 to 0.1 MPa; the acid concentration in the recovered acid solution having a concentration meeting the standard is 40 g / L to 80 g / L, preferably 50 g / L, and the acid recovery rate of the recovered acid solution in the electrodialysis separation treatment is ≥60%;

[0100] (4) performing activated carbon adsorption treatment on the recovered waste acid solution having a concentration meeting the standard to obtain a recovered acid solution, wherein the recovered acid solution has a light transmittance of ≥90% at an acid concentration of 40 g / L and a wavelength of 625 nm;

[0101] (5) The recovered acid solution is adjusted to a concentration matching the production process or mixed with new acid for regeneration of the cation resin;

[0102] (6) Collect the waste acid after use again for recycling and reuse.

[0103] Example

[0104] The sample indicators in the examples of this application were measured by the following methods.

[0105] 1. Detection method of mogroside V content

[0106] The test is carried out in accordance with the national standard "GB1886.77-2016" test method.

[0107] 2. Sulfuric acid and sodium hydroxide concentration

[0108] The test is carried out in accordance with the national standards "GB 29205-2012" and "GB1886.20-2016" test methods.

[0109] 3. Light transmittance

[0110] The recovered alkali solution was prepared to a concentration of 40 g / L and detected using an ultraviolet spectrophotometer at a wavelength of 625 nm with purified water as a blank control.

[0111] 4. The taste sensory evaluation of this application was carried out in the following manner:

[0112] Based on GB / T 1629.1-2012, "General Guidelines for the Selection, Training, and Management of Sensory Analysis Evaluators - Part 1: Selection of Evaluators," basic sensory testing and training were conducted. Fifteen sensory assessors were selected for their high sensory acuity, strong logical thinking, and excellent descriptive and communication skills. Appropriate amounts of samples were mixed with purified water to a relative sucrose sweetness of 5%. The samples were evaluated for two representative characteristics: sweetness and off-flavor.

[0113] The electrodialysis equipment used in the electrodialysis separation treatment in this application meets the following requirements: the membrane component of the electrodialysis equipment is an acid-resistant and alkali-resistant homogeneous ion exchange membrane, the operating temperature is 15-45°C, and the circulating pump pressure is 0.03-0.1 MPa; the fresh water chamber of the electrodialysis equipment contains the waste acid and alkali solution to be recovered, the concentrated water chamber contains the recovered acid, alkali solution or pure water with a concentration of ≤80g / L, and the extreme water chamber contains a solution prepared with new acid and alkali with a concentration of 5g / L-10 / L.

[0114] Preliminary experiment

[0115] Preliminary Experiment 1

[0116] (1) Collection: 60 L of waste liquid from macroporous adsorption resin alkali regeneration during the production of Monk Fruit Extract by Guilin Jifusi Biotechnology Co., Ltd. was collected. The sodium hydroxide concentration was 34.5 g / L. The waste alkali liquid was filtered using a sand rod.

[0117] (2) Electrodialysis separation: Electrodialysis recovery is performed using a small acid-resistant and alkali-resistant charged membrane. The ion exchange membrane is an alkali-resistant homogeneous ion exchange membrane of model TWED-8-20. The operating temperature is 30°C and the circulating pump pressure is 0.05 MPa. The membrane pore size is between 0.1 nm and 0.3 nm.

[0118] After separation, a total of 31.5L of qualified recovered alkali solution was obtained in the concentrated chamber, with a sodium hydroxide concentration of 64.1g / L; 35L of waste liquid was obtained in the dilute chamber, containing 1.4g / L of sodium hydroxide; it took 2h;

[0119] (3) Activated carbon treatment: 2% activated carbon was added to the recovered alkali solution based on solid sodium hydroxide, and the solution was stirred at 50°C for 40 min. 292 g of diatomaceous earth was added and filtered through a stainless steel folded filter to clarify the recovered alkali solution. 39.2 L of alkali solution was obtained, and the concentration of sodium hydroxide was 51.3 g / L. The concentration of sodium hydroxide at a wavelength of 625 nm was 40.0 g / L. The transmittance of the recovered alkali solution was 100.00%, and the alkali recovery rate was 97.1%.

[0120] The total recovery rate of sodium hydroxide is calculated as follows: the total recovery rate of sodium hydroxide, i.e., the alkali recovery rate = the weight of sodium hydroxide in the recovered alkali solution ÷ the weight of sodium hydroxide in the regenerated waste alkali solution; the weight of sodium hydroxide in the alkali solution = the volume of the alkali solution × the concentration of sodium hydroxide in the alkali solution.

[0121] The difference between Preliminary Experiment 2 and Preliminary Experiment 1 is only the membrane pore size. The membrane pore size is 0.3-0.5 nm. At this time, the transmittance of the recovered alkali solution is 96.8%, and the alkali recovery rate is 96.6%.

[0122] In addition to acids and bases, there are many other substances in this system. In order to prevent other substances from migrating into the recovered alkali, the applicant found that when the pore size of the electrodialysis membrane is between 0.1nm and 0.3nm, the transmittance of the recovered alkali solution is high, meeting the use requirements.

[0123] Example 1-1

[0124] (1) Collection: 60 L of macroporous adsorption resin alkali regeneration liquid from the production process of Monk Fruit Extract by Guilin Jifusi Biotechnology Co., Ltd. was collected, with a sodium hydroxide concentration of 34.5 g / L, and the waste alkali liquid was filtered using a sand rod;

[0125] (2) Electrodialysis separation: Electrodialysis recovery is performed using a small acid-resistant and alkali-resistant charged membrane. The ion exchange membrane is an alkali-resistant homogeneous ion exchange membrane of model TWED-8-20. The operating temperature is 30°C and the circulating pump pressure is 0.05 MPa. The membrane pore size is between 0.1 nm and 0.3 nm. After separation, a total of 31.5 L of qualified recovered alkali solution is obtained in the concentrated chamber, with a sodium hydroxide concentration of 64.1 g / L. The waste liquid in the dilute chamber is 35 L, containing 1.4 g / L of sodium hydroxide. The separation process takes 2 hours.

[0126] (3) Activated carbon treatment: 2% activated carbon was added to the recovered alkali solution based on solid sodium hydroxide, and the solution was stirred at 50°C for 40 min. 292 g of diatomaceous earth was added and filtered through a stainless steel folded filter to clarify the recovered alkali solution. 39.2 L of alkali solution was recovered, and the sodium hydroxide concentration was 51.3 g / L. The sodium hydroxide concentration at a wavelength of 625 nm was 40.0 g / L. The light transmittance of the recovered alkali solution was 100.00%, and the total recovery rate of sodium hydroxide was 97.1%.

[0127] The recovered alkali was diluted with purified water to a sodium hydroxide concentration of 50.0 g / L, and set aside as the recovered alkali solution; the solid sodium hydroxide was dissolved with purified water to a sodium hydroxide concentration of 50.0 g / L, and set aside as the newly configured alkali solution;

[0128] (4) Macroporous adsorption resin treatment: 500 mL of macroporous adsorption resin used in the adsorption production process of mogroside extract was taken respectively and loaded into 5 chromatography columns (diameter 30 mm*column height 400 mm), 100 mL per column, one of which was set as the control column, and 300 mL of freshly prepared alkali solution was used to pass through the column in a forward direction. The other four columns were set as experimental columns 1 to 4, and 210 mL, 240 mL, 270 mL, and 300 mL of recovered alkali solution were used, respectively, and passed through the column in a forward direction, with a flow rate of 1 BV / h. After the recovered alkali solution was passed into the experimental column, 90 mL, 60 mL, 30 mL, and 0 mL of freshly prepared alkali solution were continued to be passed through the column in a forward direction, and then the column was washed with purified water in a forward direction until the pH of the effluent was ≤10, and then 0.2 BV to 0.5 BV of 4% citric acid solution was used to pass through the column in a forward direction, and then the column was washed with purified water in a forward direction until the pH of the effluent was neutral;

[0129] (5) Feeding of water extract of Momordica grosvenori: The five groups of resin columns were fed with water extract of Momordica grosvenori containing 3.6 g of mogroside V, respectively. After feeding, the resin columns were washed with water and eluted with alcohol. The eluate was collected and concentrated, and the mogroside V and taste were tested. The results are shown in Table 1.

[0130] Table 1

[0131]

[0132] In Table 1, the proportion of recovered alkali regeneration refers to the proportion of recovered alkali in the total regenerated alkali, which is calculated as follows: the weight of sodium hydroxide as recovered alkali in the total regenerated alkali ÷ the weight of sodium hydroxide in the total regenerated alkali × 100%.

[0133] The comparative difference value of mogroside V content refers to the difference between the content of mogroside V in the eluate of the experimental macroporous adsorption resin column and the content of mogroside V in the eluate of the control macroporous adsorption resin column. The calculation method is: the content of mogroside V in the eluate of the experimental macroporous adsorption resin column minus the content of mogroside V in the eluate of the control macroporous adsorption resin column, or the content of mogroside V in the eluate of the control macroporous adsorption resin column minus the content of mogroside V in the eluate of the experimental macroporous adsorption resin column.

[0134] The recovery rate of mogroside V refers to the ratio of the weight of mogroside V in the macroporous resin eluate to the weight of the total feed mogroside V, and is calculated as follows: the weight of mogroside V in the macroporous resin eluate ÷ the weight of the total feed mogroside V × 100%.

[0135] The comparative difference value of mogroside V recovery rate refers to the difference between the recovery rate of mogroside V in the eluate of the experimental macroporous adsorption resin column and the recovery rate of mogroside V in the eluate of the control macroporous adsorption resin column. The calculation method is: the recovery rate of mogroside V in the eluate of the experimental macroporous adsorption resin column - the recovery rate of mogroside V in the eluate of the control macroporous adsorption resin column, or the recovery rate of mogroside V in the eluate of the control macroporous adsorption resin column - the recovery rate of mogroside V in the eluate of the experimental macroporous adsorption resin column.

[0136] The only difference between Example 1-1 and Comparative Examples 1-1 to 1-3 is the presence or absence of electrodialysis separation and activated carbon treatment. The differences and results are shown in Table 2. The remaining conditions are the same as those of Example 1-1. The membrane filtration conditions in Comparative Example 1-2 are as follows: the waste alkali liquor, after removal of insoluble impurities through a PP cotton filter element, is clarified using an alkali-resistant nanofiltration membrane with a pore size of 150D to 300D, at a filtration pressure of 0.6 MPa. The clarified filtrate is treated with activated carbon and then concentrated under vacuum to a sodium hydroxide concentration of 50.0 g / L before being used to regenerate the adsorption resin.

[0137] The vacuum concentration conditions in Comparative Examples 1-3 are as follows: the waste alkali liquor after filtering the PP cotton filter element to remove insoluble impurities is not subjected to any treatment, is directly concentrated under vacuum pressure, and then treated with activated carbon to adjust the sodium hydroxide concentration to 50.0 g / L, and then used for adsorption resin regeneration.

[0138] The transmittance of the recovered alkali solutions in Comparative Examples 1-1 to 1-3 at a concentration of 40 g / L and a wavelength of 625 nm was less than 95%.

[0139] Table 2

[0140]

[0141] In Table 2, the concepts and calculation methods of the comparative difference values ​​of the glycoside V content and the comparative difference values ​​of the recovery rates are the same as those in Example 1-1.

[0142] Example 2-1

[0143] (1) Collecting acid solution: 50 L of cationic resin acid regeneration solution from the production process of Monk Fruit Extract by Guilin Jifusi Biotechnology Co., Ltd. was collected, with a sulfuric acid concentration of 34.5 g / L, and filtered and clarified using a PP cotton filter element;

[0144] (2) Electrodialysis separation of acid solution: The electrodialysis equipment is the same as that in Example 1-1, wherein the ion exchange membrane is an acid-resistant homogeneous ion exchange membrane of type TWED-8-20, the operating temperature is 30°C, the circulating pump pressure is 0.05 MPa; and the membrane pore size is between 0.1 nm and 0.3 nm;

[0145] After separation, the qualified recovered acid solution was removed and the acid solution to be recovered was added to the concentrated chamber for recovery. A total of 30.2 L of qualified recovered acid solution was obtained in the concentrated chamber, with a sulfuric acid concentration of 53.7 g / L; about 30 L of waste liquid was obtained in the dilute chamber, containing about 3.5 g / L of sulfuric acid. This took 2.2 hours.

[0146] (3) Activated carbon treatment of acid solution: 2% activated carbon was added to the acid solution recovered in the concentration chamber based on sulfuric acid, and the mixture was stirred at 45°C for 60 min. 120 g of diatomaceous earth was added and filtered through a stainless steel folded filter to clarify the recovered acid solution. 32.2 L of acid solution was recovered, and the sulfuric acid concentration was 50.0 g / L. The sulfuric acid concentration at a wavelength of 625 nm was 40.0 g / L. The light transmittance of the recovered acid solution was 94.95%, and the total sulfuric acid recovery rate was 92.0%.

[0147] The recovered acid with a concentration of 50.0 g / L is set aside as the recovered acid solution, and then purified water and 98% concentrated sulfuric acid are used to prepare a 50.0 g / L acid solution for use, which is recorded as the newly prepared acid solution;

[0148] (4) Collecting alkali solution: 50 L of anion resin alkali regeneration solution from the production process of Momordica grosvenori extract was collected, with a sodium hydroxide concentration of 35.8 g / L, and filtered and clarified using a PP cotton filter element;

[0149] (5) Electrodialysis separation of alkali liquor: The electrodialysis equipment for alkali recovery refers to Example 1-1. The ion exchange membrane adopts an acid-resistant homogeneous ion exchange membrane of model TWED-8-20, the operating temperature is 30°C, the circulating pump pressure is 0.05 MPa; the membrane pore size is between 0.1 nm and 0.3 nm;

[0150] After separation and recovery, the concentrated chamber recovered about 27.8L of qualified alkali solution, containing 62.4g / L of sodium hydroxide; the dilute chamber recovered 27L of waste alkali solution, containing 2.0g / L of sodium hydroxide; it took 1.5h;

[0151] (6) Activated carbon treatment of alkali liquor: 4% activated carbon was added to the alkali liquor recovered from the concentration chamber based on solid sodium hydroxide, and the mixture was stirred at 45°C for 60 min. 140 g of bentonite was added and filtered through a stainless steel folded filter to clarify the recovered alkali liquor. 34.2 L of alkali liquor was recovered, and the sodium hydroxide concentration was 50.3 g / L. The sodium hydroxide concentration at a wavelength of 625 nm was 40.0 g / L. The light transmittance of the recovered alkali liquor was 99.95%, and the total recovery rate of sodium hydroxide was 96.1%.

[0152] The recovered alkali was diluted with purified water to a sodium hydroxide concentration of 50.0 g / L, and the solution was set aside as the recovered alkali solution; the solid sodium hydroxide was dissolved with purified water to a sodium hydroxide concentration of 50.0 g / L, and the solution was set aside as the newly configured alkali solution;

[0153] (7) Ion exchange resin treatment: 500 mL of anion and cation resins used in the production process of Monk Fruit Extract were loaded into 10 chromatography columns (30 mm diameter * 400 mm column height), 5 anion columns and 5 cation columns, each with 100 mL. The experimental column was a series of one anion and one cation resin after regeneration.

[0154] Regeneration of positive resin: one column was set as the control column, and 300 mL of freshly prepared 5% sulfuric acid solution was used to pass through the column in the forward direction. The other four columns were set as experimental columns 1 to 4, and 210 mL, 240 mL, 270 mL, and 300 mL of 5% sulfuric acid recovery acid were used to pass through the columns in the forward direction, respectively. After the recovery acid was added, 90 mL, 60 mL, 30 mL, and 0 mL of freshly prepared acid solution were added in the forward direction, with a flow rate of 1 BV / h. The columns were then washed with purified water in the forward direction until the pH of the effluent was ≥4.

[0155] Anion resin regeneration: One column was set as the control column, and 300 mL of freshly prepared alkali solution was used to flow through the column in the forward direction. The other four columns were set as experimental columns 1 to 4, and 210 mL, 240 mL, 270 mL, and 300 mL of recovered alkali solution were used to flow through the columns in the forward direction, respectively. After the alkali solution A was added, 90 mL, 60 mL, 30 mL, and 0 mL of fresh alkali solution prepared with solid alkali were added, respectively, at a flow rate of 1 BV / h. The water washing step was referred to Example 1;

[0156] Feeding of the water extract of Momordica grosvenori: One column of the anion and cation resin after the above regeneration was connected in series, and 50 g of solid water extract of Momordica grosvenori was fed to each set of anion and cation resin columns in series. After feeding, the resin was washed with water, and the column liquid was collected and concentrated. The mogroside V and taste were tested. The results are shown in Table 3.

[0157] Table 3

[0158]

[0159] In Table 3, the percentage of acid and alkali recovered by the regeneration agent is the ratio of the recovered acid and alkali to the total regenerated acid and alkali, calculated as follows: percentage of acid recovered by the regeneration agent = weight of sulfuric acid recovered in the total regenerated acid / weight of sulfuric acid recovered in the total regenerated acid × 100%; percentage of alkali recovered by the regeneration agent = weight of sodium hydroxide recovered in the total regenerated alkali / weight of sodium hydroxide recovered in the total regenerated alkali × 100%. The concepts and testing methods for the comparative difference values ​​of glycoside V content and glycoside V recovery rates are the same as those in Example 1-1.

[0160] The only difference between Example 2-1 and Comparative Examples 2-1 to 2-4 is whether there is electrodialysis separation, whether there is activated carbon treatment in the acid recovery stage, whether there is macroporous adsorption resin treatment in the acid recovery stage, whether there is activated carbon treatment in the alkali recovery stage, and whether there is macroporous adsorption resin treatment in the alkali recovery stage. The differences and results are shown in Table 4. The rest are the same as Example 2-1.

[0161] The light transmittance of the acid solution recovered in Comparative Examples 2-1 to 2-4 at a concentration of 40 g / L and a wavelength of 625 nm was less than 90%. The light transmittance of the alkali solution recovered in Comparative Examples 2-1 to 2-4 at a concentration of 40 g / L and a wavelength of 625 nm was less than 95%.

[0162] Table 4

[0163]

[0164] In Table 4, the concepts and calculation methods of the comparative difference values ​​of the glycoside V content and the glycoside V recovery rate are the same as those in Example 1-1.

[0165] Example 3-1

[0166] (1) Collecting alkali solution: 100 L of ceramic membrane alkali cleaning solution used for clarifying Momordica grosvenori water extract from Guilin Jifusi Luo Han Guo Biotechnology Co., Ltd. was collected, with a sodium hydroxide concentration of 19.1 g / L, and filtered using PP cotton;

[0167] (2) Electrodialysis separation: The electrodialysis equipment is as described in Example 1-1, wherein the ion exchange membrane is an alkali-resistant homogeneous ion exchange membrane of type TWED-8-20, the operating temperature is 30°C, the circulating pump pressure is 0.05 MPa; and the membrane pore size is between 0.1 nm and 0.3 nm.

[0168] After separation and recovery, about 35.4L of alkali solution was recovered in the concentration chamber, and the concentration of sodium hydroxide was 51.8g / L;

[0169] (3) Diatomaceous earth clarification: The alkali liquor recovered from the concentration chamber was treated with diatomaceous earth clarification. 150 g of diatomaceous earth was added and filtered through a stainless steel folded filter at room temperature to obtain a recovered alkali liquor. The sodium hydroxide concentration at 625 nm was 40.0 g / L and the transmittance of the recovered alkali liquor was 98.76%. The waste alkali liquor was approximately 54 L, containing 1.4 g / L of sodium hydroxide, and the treatment took 1.95 h.

[0170] The recovered alkali was diluted with purified water to a sodium hydroxide concentration of 20 g / L, and the solution was set aside as the recovered alkali solution; the solid sodium hydroxide was dissolved with purified water to a sodium hydroxide concentration of 20 g / L, and the solution was set aside as the newly prepared alkali solution;

[0171] (5) Comparison of cleaning effects of ceramic membranes: 300L of water extract of Luo Han Guo (Lotus) was obtained from the production line of Guilin Jifusi Luo Han Guo Biotechnology Co., Ltd. after centrifugation in a horizontal screw centrifuge. 100L of the water extract was clarified using an experimental ceramic membrane. The experimental ceramic membrane was then cleaned with 8L of fresh alkali solution prepared with solid alkali for 1 hour, and then cleaned several times with purified water until the pH of the circulating water was neutral. This was set as the control group. Another 100L of water extract was clarified using an experimental ceramic membrane. The experimental ceramic membrane was then cleaned with 8L of recycled alkali solution for 1 hour. The subsequent steps were consistent with the regeneration process of the control group. This was set as the experimental group, and the last 100L of water extract was clarified using an experimental ceramic membrane.

[0172] After each regeneration and cleaning, purified water was added to the ultrafiltration machine, and the flux of the clear liquid was monitored at a membrane inlet pressure of 0.1 MPa. Samples were taken to monitor the taste of each clarified liquid. The results are shown in Table 5.

[0173] Table 5

[0174] type Water flux (L / h) Flux difference (L / h) Filtrate flavor control group 30.0 - Sweet, no odor Experimental group 29.8 0.2 Sweet, no odor

[0175] In Table 5, water flux refers to the filtration flow rate of clean water by the ceramic membrane at a membrane inlet pressure of 0.1 MPa, and the collection method is to read the reading directly on the flow meter.

[0176] The flux difference refers to the difference between the water flux of the ceramic membrane after recycling alkali cleaning in the experimental group and the water flux of the ceramic membrane after new alkali cleaning in the control group. The calculation method is: water flux of the ceramic membrane after recycling alkali cleaning - water flux of the ceramic membrane after new alkali cleaning, or water flux of the ceramic membrane after new alkali cleaning - water flux of the ceramic membrane after recycling alkali cleaning.

[0177] The only difference between Example 3-1 and Comparative Examples 3-1 to 3-3 is whether or not there is electrodialysis separation and whether or not there is diatomaceous earth clarification treatment. The differences are shown in Table 6. The rest are the same as Example 3-1.

[0178] The membrane filtration conditions of Comparative Example 3-2 are as follows: the waste alkali liquid after filtering the PP cotton filter element to remove insoluble impurities is clarified with an alkali-resistant nanofiltration membrane with a pore size of 150D to 300D, the filtration pressure is 0.6Mpa, and the clarified filtrate is clarified with diatomaceous earth and then concentrated by vacuum decompression and adjusted to a sodium hydroxide concentration of 20.0g / L before being used for ceramic membrane cleaning.

[0179] The vacuum concentration conditions in Comparative Example 3-3 are as follows: the waste alkali liquor after filtering the insoluble impurities with the PP cotton filter element is not subjected to any treatment, and is directly concentrated under vacuum pressure and then clarified with diatomaceous earth and adjusted to a sodium hydroxide concentration of 20.0 g / L.

[0180] The transmittance of the recovered alkali solutions in Comparative Examples 3-1 to 3-3 at a concentration of 40 g / L and a wavelength of 625 nm was less than 95%.

[0181] Table 6

[0182]

[0183] In Table 6, the concepts and calculation methods of water flux and flux difference are the same as those in Example 3-1.

[0184] Example 4

[0185] 20 L of macroporous adsorption resin used in the production of mogroside extract at Guilin Jifusi Luo Han Guo Biotechnology Co., Ltd. was loaded into a chromatography column. The alkali liquor collection, electrodialysis separation, activated carbon treatment, and macroporous adsorption resin treatment steps were the same as in Example 1-1. The indicators of the regenerated waste alkali liquor are shown in Table 7. The waste alkali liquor treated in this application is referred to as the recovered alkali liquor, and the relevant indicators are shown in Table 7.

[0186] Feed of water extract of Momordica grosvenori: The regenerated resin feed contains 360g water extract of Momordica grosvenori containing mogroside V. After feeding, the feed is washed with water and eluted with alcohol. The eluate is collected and concentrated as a control to detect mogroside V and taste.

[0187] The resin to be regenerated was regenerated with a recycled alkali as described in Example 1-1. The recycled alkali was diluted with purified water to a sodium hydroxide concentration of 50.0 g / L and set aside, referred to as the recycled alkali solution. The solid sodium hydroxide was dissolved with purified water to a sodium hydroxide concentration of 50.0 g / L and set aside, referred to as the freshly prepared alkali solution. The recycled alkali solution and the freshly prepared alkali solution accounted for 80% and 20% of the alkali used for regeneration, respectively. This method was used for a total of seven times of continuous feeding and adsorption resin regeneration, as well as seven times of alkali solution recovery. The alkali recovery conditions and the test results of the sweet glycoside concentrate indicators are shown in Tables 7 and 8, respectively.

[0188] Table 7

[0189]

[0190] Regeneration waste alkali liquor refers to the waste alkali liquor discharged after resin regeneration or membrane cleaning, which is collected for regeneration.

[0191] Recovered alkali liquor refers to the alkali liquor regenerated by the method of the present application.

[0192] In Table 7, volume refers to the volume of the waste or recovered alkali liquor, measured in L, and is obtained by direct measurement using a solution volume measuring container (e.g., a glass graduated cylinder). Alkali content refers to the mass concentration (%) of sodium hydroxide in the waste or recovered alkali liquor, as determined by the method previously described. Total alkali content refers to the weight of sodium hydroxide in the waste or recovered alkali liquor, calculated as: Total alkali content = Alkali content × Alkali volume.

[0193] Table 8

[0194]

[0195]

[0196] In Table 8, the concepts and calculation methods of the difference values ​​of the recovery alkali regeneration ratio and the recovery rate are the same as those in Example 1-1.

[0197] Example 5

[0198] The experimental ceramic membrane ultrafiltration equipment after clarifying the water extract of Momordica grosvenori was washed with 8L of alkali solution with a concentration of 20g / L of sodium hydroxide dissolved in purified water using food-grade sodium hydroxide solid alkali for 1 hour, and then washed with purified water for several times until the pH of the circulating water was neutral;

[0199] The cleaned ceramic membrane was set as the control group and injected into the purified water and ultrafiltration unit. The clear liquid flux was monitored under the membrane inlet pressure of 0.1 MPa. The cleaned ultrafiltration membrane was used to filter and clarify the monk fruit extract, and the taste of the clarified liquid was monitored.

[0200] The ceramic membrane cleaning solution was collected and recorded as the cleaning waste alkali solution, which was about 17-18 L and had a sodium hydroxide concentration of 8-9 g / L. For details, see Table 9. The cleaning waste alkali solution was recovered according to the recovery method described in Example 3-1, and the alkali solution obtained by treating the alkali solution recovered in the concentrate chamber was recorded as the concentrate chamber alkali solution. For details, see Table 9.

[0201] The recovered alkali was diluted with purified water to a sodium hydroxide concentration of 20 g / L, and the solution was set aside as the recovered alkali solution; the solid sodium hydroxide was dissolved with purified water to a sodium hydroxide concentration of 20 g / L, and the solution was set aside as the newly prepared alkali solution;

[0202] The cleaning liquid first uses recycled alkali solution, and the insufficient part is supplemented by new alkali solution prepared with solid alkali. In this alkali recovery and recycling mode, the ceramic membrane is used and cleaned four times, and the alkali solution is recovered four times. After the last material clarification is completed, it is cleaned with new alkali solution prepared with solid alkali for comparison.

[0203] The alkali recovery and extract clarified liquid detection results are shown in Tables 9 and 10, respectively. The ceramic membrane regeneration flux decays at a normal rate, and there is no significant difference in the regeneration effect between the regenerated alkali and the new alkali.

[0204] Table 9

[0205]

[0206] In Table 9, the concepts and calculation methods of volume, alkali content, and total alkali amount are the same as those in Example 4.

[0207] Table 10

[0208]

[0209] In Table 10, the proportion of alkali recovered in the cleaning liquid (%) refers to the proportion of recovered alkali in the total cleaning alkali of the ceramic membrane, and the calculation method is: the weight of sodium hydroxide recovered in the total cleaning alkali ÷ the weight of sodium hydroxide in the total cleaning alkali × 100%.

[0210] Water wash flux refers to water flux. Water flux refers to the filtration flow rate of clean water by the ceramic membrane at a membrane inlet pressure of 0.1 MPa. The collection method is to read the reading directly on the flow meter.

[0211] The flux decline value refers to the decline in the water flux of the ceramic membrane after the 2nd to 5th cleaning of the experimental group compared with the water flux of the first fresh alkali cleaning of the control group. The calculation method is: cleaning water flux of the experimental group - cleaning water flux of the control group.

[0212] It can be seen from Tables 9 and 10 that the recovered alkali solution can still maintain stable quality and meet the process requirements after being recycled and reused for multiple times.

[0213] Although the present invention has been disclosed above with reference to the embodiments, they are not intended to limit the present invention. Anyone with ordinary knowledge in the art may make slight changes and modifications without departing from the spirit and scope of the present invention. Therefore, the scope of protection of the present invention shall be determined by the scope of the patent application attached hereto.

Claims

1. A method for treating waste liquid in the production process of Momordica grosvenori extract, comprising: Collect waste liquid generated during the production of monk fruit extract; Filtration to remove insoluble impurities from wastewater; The filtered waste liquid is subjected to electrodialysis separation treatment to obtain a recovered waste liquid with a concentration meeting the standard; Post-processing the recovered waste liquid with concentration meeting the standards to obtain a recovered liquid; The waste liquid is waste acid liquid and / or waste alkali liquid, and the recovered liquid is recovered acid liquid and / or recovered alkali liquid.

2. The method according to claim 1, wherein The post-treatment is adsorption treatment or clarification treatment.

3. The method according to claim 2, wherein: The adsorption treatment is selected from any one of bentonite adsorption treatment, diatomaceous earth adsorption treatment, activated carbon adsorption treatment, silica gel adsorption treatment, and alumina adsorption treatment; or, The clarification treatment is any one of diatomaceous earth clarification treatment, bentonite clarification treatment, perlite clarification treatment, cellulose clarification treatment, and clay clarification treatment.

4. The method according to claim 1, wherein The electrodialysis separation treatment uses an acid-resistant homogeneous ion exchange membrane or an alkali-resistant homogeneous ion exchange membrane; Preferably, The membrane pore diameter of the acid-resistant homogeneous ion exchange membrane or the alkali-resistant homogeneous ion exchange membrane is 0.1 nm to 0.5 nm, preferably 0.1 nm to 0.3 nm.

5. The method according to claim 1, wherein The light transmittance of the recovered acid solution at an acid concentration of 40 g / L and a wavelength of 625 nm is ≥90%; and / or, The light transmittance of the recovered alkali solution is greater than or equal to 95% when the alkali concentration is 40 g / L and the wavelength is 625 nm.

6. The method according to claim 1, wherein The acid concentration in the recovered waste acid solution that meets the concentration standard is 40g / L to 80g / L, preferably 50g / L; or The concentration of alkali in the recovered waste alkali solution that meets the concentration standard is 40g / L to 80g / L, preferably 50g / L.

7. The method according to claim 6, wherein: The acid recovery rate in the electrodialysis separation treatment is ≥60%, or the alkali recovery rate is ≥70%.

8. The method according to claim 1, wherein The waste acid liquid refers to the waste liquid generated during the regeneration process of cationic resin acid in the production process of Momordica grosvenori extract, and the acid concentration range is 5g / L to 50g / L; and / or, The waste alkali liquor comprises any one of the waste alkali liquors generated in the macroporous adsorption resin regeneration process, the decolorization anion resin alkali regeneration process and the ceramic membrane cleaning process during the production of the monk fruit extract, and the alkali concentration range is 5g / L to 50g / L; Preferably, The acid in the waste acid liquid is sulfuric acid; and / or, The alkali in the waste alkali liquor is sodium hydroxide.

9. The method according to claim 1, wherein The filtration is one or more of sand rod filtration, plate and frame filtration, stainless steel folded filter element filtration, disc filtration, activated carbon filtration, high-efficiency fiber filtration, PP cotton filter element filtration, and microporous membrane cross-flow filtration.

10. Use of the recovered liquid obtained by the method according to any one of claims 1 to 9 in resin regeneration; Preferably, the resin regeneration is macroporous adsorption resin regeneration or ion exchange resin regeneration.

11. Use of the recovered liquid obtained by the method according to any one of claims 1 to 9 in cleaning and regenerating ceramic membranes, wherein the recovered liquid is recovered alkali solution.

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