Process for the preparation of betaine

Abstract

The application provides a preparation method of betaine, and belongs to the technical field of food processing. The method can greatly improve the yield of betaine by sequentially performing pretreatment and two-stage impurity removal on a sample and then extracting betaine by using specific exchange resin. Compared with a conventional extraction method, the yield can be increased by 9-10 times, the problem of low yield when the beet molasses raw material is subjected to ion column separation is better solved, and the extraction of natural betaine can be mass-produced.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of food processing, and particularly relates to a preparation method of betaine. BACKGROUND

[0002] Betaine (trimethylglycine) has a molecular formula of C5H 11 NO2, belongs to alkaloids, has no strong hygroscopicity, is non-toxic, and is relatively stable in nature and can withstand a temperature close to 200 DEG C. Betaine has three non-stable methyl groups and is an effective methyl donor. In an animal body, betaine, choline and methionine can be converted into each other. Choline needs to be converted into betaine before playing a role of providing methyl groups in the body, so betaine can replace choline and directly participate in the methionine cycle without the oxidation process in the human body.

[0003] Betaine is widely used abroad and is used in large quantities in various aspects such as sports food and health food. In China, betaine is classified as a natural spice for food and is added to food as a food additive, and only natural extracted betaine is allowed.

[0004] Sugar beet molasses is a by-product of sugar beet sugar production. There are many sources of sugar molasses, and the amount is also large. Good development of sugar beet molasses can make resources not wasted, and there are few natural extracted betaine products on the market. When betaine is separated by resin, the resin adsorption rate is low due to many impurities and pigments, resulting in poor resin separation efficiency. Therefore, effectively improving the yield of betaine during extraction can make it better adapt to factory production, which is of great significance for good use of sugar beet molasses. SUMMARY

[0005] The application provides a preparation method of betaine. The method can greatly improve the yield of betaine by sequentially pretreating a sample, removing impurities in two stages and extracting betaine by using specific exchange resin. Compared with a conventional extraction method, the yield can be improved by 9-10 times, the problem of low yield of sugar beet molasses raw material when being loaded on an ion column is better solved, and the extraction of natural betaine can be mass-produced.

[0006] In order to achieve the above purpose, the application provides a preparation method of betaine, which comprises the following steps:

[0007] The sample preparation step: dilute and adjust the solid content of sugar beet molasses to be in the range of Brix 20 DEG -25 DEG ;

[0008] The sample pretreatment step: before loading, remove impurities from the sugar beet molasses, centrifuge the supernatant after removing impurities, and set the conductivity of the supernatant obtained by re-separation to be not higher than 10 ms / cm, and adjust the pH of the supernatant to be 6.8-7.2;

[0009] A first extraction and impurity removal step: sequentially performing a first impurity removal and a second impurity removal on the supernatant by using a macroporous strong basic type II styrene anion exchange resin D202 and a macroporous strong acid styrene cation exchange resin D001 to obtain effluent;

[0010] A separation step: sequentially adsorbing and eluting the obtained second impurity removal effluent by using a styrene gel type strong acid cation exchange resin SA-2 of H type and a styrene gel type strong base anion exchange resin HZ202 of OH type to obtain betaine.

[0011] In the above sample preparation step, preferably, 450-550 kg of sugar beet molasses is taken, the molasses solid is adjusted to Brix 20°-25° by adding 900-1100 kg of purified water, which can increase the flowability and prepare for impurity removal.

[0012] In the above scheme, the conductivity of the supernatant is specifically limited, because the greater the conductivity, the greater the ionic strength in the liquid, and in the present application, the main use is the cation and anion resin, and the greater the conductivity will have a great influence on the adsorption of the resin, so the conductivity is required to be controlled within the range of not higher than 10 ms / cm.

[0013] As preferred, before sample loading, the sugar beet molasses is subjected to impurity removal, specifically:

[0014] The diluted sugar beet molasses liquid is heated to 40-50°C, 450-550 g of ethylenediamine tetraethylene acid disodium salt, 110-130 g of dimercaptosuccinic acid disodium salt, and 230-270 g of polyacrylic acid sodium salt, 220-230 g of tannic acid, and 350-250 g of zinc sulfate are added, stirred for 15-25 minutes, heated to 75-85°C, 3%-6% V of ethanol is added, stirred for 15-25 minutes, and placed in a decanting tank, the material in the decanting tank is cooled to 2-4°C by using a jacket, and maintained for 12-15 hours.

[0015] In the above step, the sugar beet molasses is treated by using chelation and flocculation, the metal ions and the chelating agent generate chelates, and then the flocculating agent is used for flocculation, under the action of centrifugation, some chelate precipitates are separated out, and then the second impurity removal is performed, which can greatly reduce the metal ions in the raw material and improve the betaine adsorption rate.

[0016] As preferred, before the supernatant is subjected to impurity removal by using a macroporous strong basic type II styrene anion exchange resin D202 and a macroporous strong acid styrene cation exchange resin D001, a step of treating the above two resins is further included.

[0017] As preferred, the treatment of the macroporous strong basic type II styrene anion exchange resin D202 is specifically as follows:

[0018] The macroporous strong basic type II styrene anion exchange resin D202 is first soaked in 8%-12% sodium chloride solution for 3-5 hours, then soaked in 0.2% H2O2 for 3 minutes, quickly washed with water until no yellow liquid flows out, then soaked in 98%-95% ethanol for 3-5 hours, and washed with purified water until no obvious alcohol smell;

[0019] The resin is soaked in 2N-3N NaOH solution for 2-3 hours, then continuously washed with 2-3 BV of sodium hydroxide solution at a flow rate of 1 BV / h, and then washed with purified water until the effluent pH is 7.0-8.0;

[0020] The resin is soaked in 2N-3N HCl solution for 2-3 hours, then continuously washed with 2-3 BV of hydrochloric acid solution at a flow rate of 1 BV / h, and then washed with purified water until the effluent pH is 6.0-7.0;

[0021] The resin is soaked in 2N-3N NaOH solution for 2-3 hours, then continuously washed with 2-3 BV of sodium hydroxide solution at a flow rate of 1 BV / h, and then washed with purified water until the effluent pH is 7.0-8.0.

[0022] As preferred, the treatment of the macroporous strong basic type II styrene anion exchange resin D202 is specifically as follows:

[0023] The macroporous strong basic type II styrene anion exchange resin D202 is first soaked in 8%-12% sodium chloride solution for 3-5 hours, then soaked in 0.2% H2O2 for 3 minutes, quickly washed with water until no yellow liquid flows out, then soaked in 98%-95% ethanol for 3-5 hours, and washed with purified water until no obvious alcohol smell;

[0024] The resin is soaked in 2N-3N NaOH solution for 2-3 hours, then continuously washed with 2-3 BV of sodium hydroxide solution at a flow rate of 1 BV / h, and then washed with purified water until the effluent pH is 7.0-8.0;

[0025] The resin is soaked in 2N-3N HCl solution for 2-3 hours, then continuously washed with 2-3 BV of hydrochloric acid solution at a flow rate of 1 BV / h, and then washed with purified water until the effluent pH is 6.0-7.0.

[0026] As preferred, the treatment of the macroporous strong basic type II styrene anion exchange resin D202 is specifically as follows:

[0027] The prepared macroporous strong base type II styrene-based anion exchange resin D202 was placed in the chromatographic column, and a sand core filter plate was placed on top of it. A 400-mesh filter screen was placed above the sand core filter plate. Activated carbon particles were placed on top of the sand core filter plate at an amount of 20%-30% of the resin volume. The prepared sample was passed through the filter, and a section of the eluent was collected.

[0028] As a preferred method, the two-stage impurity removal of the first-stage effluent is performed using macroporous strong acid styrene-based cation exchange resin D001, specifically as follows:

[0029] Add 0.75%-0.85% ammonium chloride and 0.65%-0.75% ammonium acetate to the first effluent, then add 1%-1.2% arginine, stir thoroughly, then add 1.5%-2.5% ethanol, stir thoroughly, adjust the pH to 7.2-7.4, then load it onto a macroporous strong acid styrene-based cation exchange resin D001 column at a flow rate of 0.5 BV / h, and collect the second effluent.

[0030] In the above scheme, before the formal extraction, the supernatant is subjected to two-stage impurity removal using two different ion exchange resins. The purpose is to remove most of the pigments and metal ions that interfere with the cation exchange resin. In addition, during the two-stage impurity removal, some compounds and ions that would interfere with the resin during the adsorption of betaine can be adsorbed in advance.

[0031] As a preferred embodiment, the separation step specifically includes:

[0032] The effluent from the second stage was passed into the treated styrene-based gel-type strong acid cation exchange resin SA-2, which had been converted to the H-type, to adsorb betaine at a flow rate of 0.5 BV / h. After adsorption, the resin was rinsed with 2-3 BV of purified water at a flow rate of 0.9-1.1 BV / h.

[0033] Then, elute with a 0.7-0.8 mol / L ammonia solution, collect the eluent, and pass the eluent into a pre-treated styrene-based gel-type strong base anion exchange resin HZ202 (converted to OH form) to remove anions at a flow rate of 0.4-0.6 BV / h. Collect the effluent.

[0034] In the above scheme, the H-type styrene-based gel-type strong acid cation exchange resin SA-2 can be treated by conventional methods, such as soaking it in 2N-3N sodium hydroxide and then rinsing it with 2N-3N hydrochloric acid; similarly, the OH-type styrene-based gel-type strong base anion exchange resin can be treated by conventional methods, such as soaking it in 2N-3N hydrochloric acid and then rinsing it with 2N-3N sodium hydroxide.

[0035] As a preferred method, the effluent is concentrated under reduced pressure at 70℃-80℃ until there is no obvious ammonia odor, and then evaporated and crystallized at 60℃-65℃ to obtain crude crystals;

[0036] The crude crystals were dissolved in ethanol, separated, filtered, and then naturally crystallized.

[0037] The naturally crystallized crystals were dried at 110℃-120℃ to obtain betaine.

[0038] Preferably, the obtained betaine content is ≥95% and the yield is ≥75.75%.

[0039] Compared with the prior art, the advantages and positive effects of the present invention are as follows:

[0040] This invention significantly improves the yield of betaine by pretreating the sample sequentially, performing two-stage impurity removal, and then extracting betaine using a specific ion exchange resin. Compared with conventional extraction methods, the yield can be increased by 9-10 times, effectively solving the problem of low yield of beet molasses raw materials when using an ion exchange column, and enabling the mass production of natural betaine extraction. Attached Figure Description

[0041] Figure 1 A comparison chart of the adsorption rates of different resins provided for this invention. Detailed Implementation

[0042] The technical solutions in the embodiments of the present invention will be clearly and completely described below. 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.

[0043] Example 1

[0044] 1. Sample preparation: Take 450-550 kg of beet molasses, with the molasses solids at Brix 65°-72°, add 900-1100 kg of purified water, and adjust the solids at Brix 20°-25°.

[0045] 2. Impurity removal: Heat the diluted beet molasses solution to 40℃-50℃, add 450g of disodium ethylenediaminetetraadiate and 110g of disodium dimercaptosuccinate, stir for 15-25 minutes, then heat to 75-85℃, add 230g of sodium polyacrylate, 220g of tannic acid and 350g of zinc sulfate, and continue stirring for 25-35 minutes. Add 3%-6% ethanol, stir for 15-25 minutes, and place in a vortex settling tank. Use the jacket to cool the material in the vortex settling tank to 2℃-4℃ and maintain for 12-15 hours.

[0046] 3. Resin treatment:

[0047] 1) Soak the macroporous, strongly basic type II styrene-based anion exchange resin (D2O2-N+(CH3)2C2H4OH) in 8%-12% sodium chloride solution for 3-5 hours, then soak it in 0.2% H2O2 for 3 minutes, and quickly rinse it with water until no yellow liquid flows out. Then soak it in 98%-95% ethanol for 3-5 hours, and rinse it with purified water until there is no obvious alcohol odor. Then soak the resin in 2N-3N NaOH solution for 2-3 hours, and then continue to soak it in 2-3 BV (volume multiple) sodium hydroxide solution at 1 BV / Rinse the resin with a flow rate of 1 BV / h using purified water until the effluent pH reaches 7.0-8.0. Then soak the resin in 2N-3N HCl solution for 2-3 hours. Next, rinse the resin with 2-3 BV hydrochloric acid solution at a flow rate of 1 BV / h, then wash with purified water until the effluent pH reaches 6.0-7.0. Then soak the resin in 2N-3N NaOH solution for 2-3 hours. Next, rinse the resin with 2-3 BV sodium hydroxide solution at a flow rate of 1 BV / h, then wash with purified water until the effluent pH reaches 7.0-8.0.

[0048] 2) First, soak the styrene-based macroporous strong acid cation exchange resin (D001-CC-SO3H) in a solution containing 4-6% sodium chloride and 4-6% potassium chloride for 2-3 hours. Then, wash it with purified water until no yellow liquid flows out. Next, soak the resin in 2N-3N NaOH solution for 2-3 hours. Then, continue to rinse the resin with 2-3 BV sodium hydroxide solution at a flow rate of 1 BV / h. Then, wash it with purified water until the pH of the effluent is 7.0-8.0. Next, soak the resin in 2N-3N HCl solution for 2-3 hours. Then, continue to rinse the resin with 2-3 BV hydrochloric acid solution at a flow rate of 1 BV / h. Finally, wash it with purified water until the pH of the effluent is 6.0-7.0.

[0049] 4. Sample preparation before column loading: Slowly release the supernatant from the vortex sedimentation solution and place it in a separation disc centrifuge to separate the supernatant. Then, measure the conductivity and pH of the separated supernatant. The conductivity should not be higher than 10 ms / cm. If it exceeds the threshold, repeat the impurity removal process. For every 0.1 ms / cm exceeding the threshold, the feed amount should be 0.005% of the amount removed in the first impurity removal. Repeat the impurity removal process until the sample is qualified. Then, adjust the pH to 6.8-7.2.

[0050] 5. Extraction of impurities in the first two stages:

[0051] First stage of impurity removal: Place the treated macroporous strong base styrene-based anion exchange resin (D202) into the chromatographic column, then place a sand core filter plate, and place a 400-mesh filter screen on top of the sand core filter plate. Place activated carbon particles at a volume of 20%-30% of the resin on top of the filter paper plate, pass the treated material through it, and collect the effluent.

[0052] Second-stage impurity removal: Add 0.75%-0.85% ammonium chloride and 0.65%-0.75% ammonium acetate to the first-stage effluent, then add 1%-1.2% arginine, stir thoroughly, then add 1.5%-2.5% ethanol, stir thoroughly, adjust the pH to about 7.2-7.4, and load the adjusted solution onto a styrene-based macroporous strong acid cation exchange resin (D001-CC-SO3H) at a flow rate of 0.5 BV / h, and collect the effluent.

[0053] 6. Separation: The two sections of purified effluent are passed into a styrene-based gel-type strong acid cation exchange resin (SA-2) that has been converted to H-type to adsorb betaine at a flow rate of 0.5 BV / h. After adsorption, the resin is rinsed with 2-3 BV of purified water at a flow rate of 1 BV / h.

[0054] Then, elute with a 0.7-0.8 mol / L ammonia solution, collect the eluent, and pass the eluent through a styrene-based gel-type strong base anion exchange resin (HZ202) converted to OH form to remove anions at a flow rate of 0.5 BV / h. Collect the effluent.

[0055] 7. Concentration and Crystallization: The effluent is concentrated under reduced pressure and vacuum, and heated to 70℃-80℃ until there is no obvious ammonia odor. Then it is introduced into a crystallization tank and evaporated at 60℃-65℃ to obtain crude crystals. The crude crystals are dissolved in ethanol, separated using a separation disc centrifuge, and then filtered using a plate and frame filter press. The filtrate is allowed to naturally precipitate crystals.

[0056] 8. Finished product and testing: The self-precipitated crystals are placed in a vacuum belt dryer and dried at a temperature of 110℃-120℃ to obtain betaine with a content of ≥95%.

[0057] Example 2

[0058] The preparation method is the same as in Example 1, except that in step 2) the impurity removal step: the diluted beet molasses solution is heated to 40℃-50℃, 500g of disodium ethylenediaminetetraadiate and 120g of disodium dimercaptosuccinate are added, and stirred for 15-25 minutes. Then it is heated to 75-85℃, 250g of sodium polyacrylate, 225g of tannic acid and 300g of zinc sulfate are added, and stirred continuously for 25-35 minutes. Then 3%-6% V of ethanol is added, and stirred for 15-25 minutes. The mixture is then placed in a vortex tank, and the material in the vortex tank is cooled to 2℃-4℃ using the jacket wall and kept there for 12-15 hours.

[0059] Example 3

[0060] The preparation method is the same as in Example 1, except that in step 2) the impurity removal step: the diluted beet molasses solution is heated to 40℃-50℃, 550g of disodium ethylenediaminetetraadiate and 130g of disodium dimercaptosuccinate are added, and stirred for 15-25 minutes. Then it is heated to 75-85℃, 270g of sodium polyacrylate, 230g of tannic acid and 250g of zinc sulfate are added, and stirred continuously for 25-35 minutes. Then 3%-6% of ethanol is added, and stirred for 15-25 minutes. The mixture is then placed in a vortex tank, and the material in the vortex tank is cooled to 2℃-4℃ using the jacket wall and kept there for 12-15 hours.

[0061] Performance testing

[0062] Static adsorption yield detection method:

[0063] Equipment: High-performance liquid chromatography with UV detector or DAD detector

[0064] Column: Inertsil NH2 5um 4.6*250mm

[0065] Detection wavelength: 195nm

[0066] Standard: Betaine (China National Institutes for Food and Drug Control) CAS No.: 107-43-7

[0067] Mobile phase: Acetonitrile: Water: Isopropanol (70:25:5V / V / V)

[0068] Flow rate: 0.8 ml / min

[0069] Column temperature: 35℃

[0070] Standard preparation method: 0.25 mg / ml - 0.35 mg / ml betaine aqueous solution.

[0071] Sample preparation method: Dilute the sample into an aqueous solution of a certain concentration.

[0072] Table 1 shows the loading and yield of betaine prepared using the method of this application, as well as the loading and yield of betaine under different processing steps in the method of this application. Table 2 shows the loading and yield of betaine prepared using the method of this application, as well as the loading and yield of betaine under different processing steps in the method of this application, the difference being that styrene-based gel-type strong acid cation exchange resin 001*7 is used instead of SA-2 when adsorbing betaine. Table 3 shows the loading and yield of betaine prepared using the method of this application, as well as the loading and yield of betaine under different processing steps in the method of this application, the difference being that styrene-based gel-type strong acid cation exchange resin 001*12 is used instead of SA-2 when adsorbing betaine.

[0073] Table 1

[0074]

[0075]

[0076] Table 2

[0077]

[0078] Table 3

[0079]

[0080]

[0081] Combining the data in Tables 1-3 and the appendix Figure 1 It can be seen that although different cation exchange resins have similar loading rates for 95% betaine, the adsorption rates of betaine obtained by individual treatments at different stages of the processing method in this application are compared with those obtained by the complete processing method in this application. After conducting adsorption rate experiments on different cation exchange resins simultaneously, it was found that the resin with a higher initial selectivity rate will have a better loading rate after treating the molasses dilution solution, which is beneficial to production. That is, the adsorption rate of betaine obtained under the scheme of this application can reach 75.75%, which has a significant advantage compared with the adsorption rates of betaine at the same stage in Tables 2 and 3, and is 9-10 times better than the adsorption rate of betaine in the initial dilution solution in Table 1.

Claims

1. A method for preparing betaine, characterized in that, Includes the following steps: Sample preparation steps: Dilute and adjust the beet molasses solids to the Brix range of 20°-25°; Sample pretreatment steps: Before loading the sample, heat the diluted beet molasses solution to 40℃-50℃, add 450-550g of disodium ethylenediaminetetraadiate and 110-130g of disodium dimercaptosuccinate, stir for 15-25 minutes, then heat to 75-85℃, add 230-270g of sodium polyacrylate, 220-230g of tannic acid and 350-250g of zinc sulfate, and continue stirring for 25-35 minutes. Add 3%-6% ethanol, stir for 15-25 minutes, and place in a vortex tank. Use the jacket to cool the material in the vortex tank to 2℃-4℃ and maintain for 12-15 hours to remove impurities from the beet molasses. Centrifuge the supernatant after impurity removal and set the conductivity of the supernatant obtained after separation to a range not exceeding 10 mS / cm. At the same time, adjust the pH of the supernatant to 6.8-7.

2. The first two-stage impurity removal steps before extraction: The supernatant is subjected to first-stage and second-stage impurity removal sequentially using macroporous strong-basic type II styrene-based anion exchange resin D202 and macroporous strong-acidic styrene-based cation exchange resin D001 to obtain the effluent. Specifically, the first-stage impurity removal using macroporous strong-basic type II styrene-based anion exchange resin D202 involves placing the treated resin in a chromatographic column, placing a sand filter plate on top, and then placing a 400-mesh filter screen above the sand filter plate. Activated carbon particles are then placed in the sand filter at a volume of 20%-30% of the resin volume. Above the filter core, the treated sample is passed through it, and the first effluent is collected. The second stage of impurity removal of the first effluent is carried out using macroporous strong acid styrene-based cation exchange resin D001. Specifically, 0.75%-0.85% ammonium chloride and 0.65%-0.75% ammonium acetate are added to the first effluent, followed by 1%-1.2% arginine. The mixture is stirred thoroughly, and then 1.5%-2.5% ethanol is added. The mixture is stirred thoroughly, and the pH is adjusted to 7.2-7.

4. The mixture is then passed through a macroporous strong acid styrene-based cation exchange resin D001 column at a flow rate of 0.5 BV / h, and the second effluent is collected. Separation Step 1: The effluent from the second stage is passed into the pre-treated styrene-based gel-type strong acid cation exchange resin SA-2 (converted to H-form) to adsorb betaine at a flow rate of 0.5 BV / h. After adsorption, the resin is rinsed with 2-3 BV of purified water at a flow rate of 0.9-1.1 BV / h. Then, it is eluted with 0.7-0.8 mol / L ammonia solution, and the eluent is collected. The eluent is then passed into the pre-treated styrene-based gel-type strong base anion exchange resin HZ (converted to OH-form). In step 202, anions are removed at a flow rate of 0.4-0.6 BV / h. The effluent is collected and concentrated under reduced pressure at 70℃-80℃ until no obvious ammonia odor is detected. Then, it is evaporated and crystallized at 60℃-65℃ to obtain crude crystals. The crude crystals are dissolved in ethanol, separated, filtered, and allowed to crystallize naturally. The naturally crystallized crystals are dried at 110℃-120℃ to obtain betaine. The content of the obtained betaine is ≥95%, and the yield is ≥75.75%.

2. The preparation method according to claim 1, characterized in that, Before using macroporous strong basic type II styrene-based anion exchange resin D202 and macroporous strong acid styrene-based cation exchange resin D001 to remove impurities from the supernatant, the process also includes a step of treating the two resins.

3. The preparation method according to claim 2, characterized in that, The specific treatment of macroporous strong basic type II styrene-based anion exchange resin D202 is as follows: First, soak the macroporous strong base type II styrene-based anion exchange resin D202 in 8%-12% sodium chloride solution for 3-5 hours, then soak it in 0.2% H2O2 for 3 minutes, quickly wash it with water until no yellow liquid flows out, then soak it in 98%-95% ethanol for 3-5 hours, and wash it with purified water until there is no obvious alcohol smell. Soak the resin in a 2N-3N NaOH solution for 2-3 hours, then continue rinsing the resin with a 2-3 BV sodium hydroxide solution at a flow rate of 1 BV / h, and then wash with purified water until the pH of the effluent is 7.0-8.0; Soak the resin in 2N-3N HCl solution for 2-3 hours, then continue to rinse the resin with 2-3BV hydrochloric acid solution at a flow rate of 1BV / h, and then wash with purified water until the pH of the effluent is 6.0-7.

0. Soak the resin in a 2N-3N NaOH solution for 2-3 hours, then continue rinsing the resin with a 2-3BV sodium hydroxide solution at a flow rate of 1BV / h, and then wash with purified water until the pH of the effluent is 7.0-8.

0.

4. The preparation method according to claim 2, characterized in that, The specific treatment of macroporous strong acid styrene-based cation exchange resin D001 is as follows: First, soak the styrene-based macroporous strong acid cation exchange resin D001 in a solution containing 4-6% sodium chloride and 4-6% potassium chloride for 2-3 hours, and then wash it with purified water until no yellow liquid flows out. Soak the resin in 2N-3N NaOH solution for 2-3 hours, then continue to rinse the resin with 2-3BV sodium hydroxide solution at a flow rate of 1BV / h, and then wash with purified water until the pH of the effluent is 7.0-8.

0. Soak the resin in 2N-3N HCl solution for 2-3 hours, then continue rinsing the resin with 2-3BV hydrochloric acid solution at a flow rate of 1BV / h, and then wash with purified water until the pH of the effluent is 6.0-7.0.

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