A method for treating a boron-removing resin and related applications

Abstract

The application discloses a treatment method of boron-removing resin and related application thereof, and relates to the field of boron-removing resin. The boron-removing resin can realize deep removal of ion-grade boron after the treatment through specific cleaning and purifying treatment steps, and the boron-removing efficiency and effectiveness of the boron-removing resin are improved compared with the prior art, thereby providing a path for efficient preparation of electronic-grade ultrapure water.

Description

Technical Field

[0001] This invention relates to the field of boron removal resins, and more specifically, to a method for treating boron removal resins and its related applications. Background Technology

[0002] Electronic-grade ultrapure water is an essential material for the production of high-end semiconductors, such as chips and panels. Ultrapure water used in chip manufacturing has extremely low ion content and extremely low organic matter leaching (according to ASTM standards, all metal ions should be <0.005 μg / L, and specifically, boron content should be less than 0.001 μg / L, TOC <1 ppb). Conventional treatment processes use a polishing mixed-bed mode to achieve deep removal of ions and boron. To improve the service life of the polishing resin, an additional electronic-grade boron removal resin stage can be added to remove trace ions.

[0003] Conventional boron removal resins are generally used for boron removal before seawater desalination and for boron removal in drinking water. Resins without special treatment have problems such as low conversion rate, low cleanliness, and insufficient treatment precision. When used in electronic-grade ultrapure water, they can cause a decrease in the resistivity of the original ultrapure water, a significant increase in TOC, and excessive metal ions at the outlet, resulting in a significant decline in water quality. Therefore, they are not suitable for electronic-grade applications.

[0004] In view of this, the present invention is proposed. Summary of the Invention

[0005] The purpose of this invention is to provide a method for treating boron-removing resin and its related applications.

[0006] This invention is implemented as follows:

[0007] In a first aspect, embodiments of the present invention provide a method for treating boron-removing resin, comprising: purifying an ion exchange resin for boron removal after deep cleaning; wherein the deep cleaning includes rinsing the ion exchange resin with an acid solution and an alkaline solution; the purification process includes rinsing the deeply cleaned ion exchange resin with a first solution, a second solution, and a third solution respectively; the first solution is an aqueous solution at 20–40°C, the second solution is an aqueous solution at 40–90°C, and the third solution is an aqueous solution at 20–40°C.

[0008] Secondly, embodiments of the present invention provide a method for preparing boron-removing resin, which includes: treating the prepared boron-removing resin using the processing method described in the foregoing embodiments.

[0009] Thirdly, the embodiments of the present invention provide the application of the boron-removing resin prepared by the processing method described in the foregoing embodiments in boron removal or preparation of electronic-grade ultrapure water.

[0010] The present invention has the following beneficial effects:

[0011] This invention employs specific cleaning and purification steps to treat boron-removing resin, enabling the resin to achieve deep removal of ionic boron. Compared to existing technologies, this improves the boron removal efficiency and effectiveness of the resin, providing a pathway for the efficient preparation of electronic-grade ultrapure water. Detailed Implementation

[0012] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall apply. Reagents or instruments whose manufacturers are not specified are all conventional products that can be purchased commercially.

[0013] This invention provides a method for treating boron-removing resin, which includes: purifying ion exchange resin used for boron removal after deep cleaning;

[0014] The deep cleaning step includes rinsing the ion exchange resin with an acid solution and an alkaline solution.

[0015] The purification process includes rinsing the deeply cleaned ion exchange resin with a first solution, a second solution, and a third solution, respectively; the first solution is an aqueous solution at 20–40°C, the second solution is an aqueous solution at 40–90°C, and the third solution is an aqueous solution at 20–40°C.

[0016] This invention addresses resins treated with acid and alkali solutions by sequentially cleaning them with a low-temperature-high-temperature-low-temperature aqueous solution. This process enables deep purification of the resin, achieving thorough removal of ionic boron and extending its service life.

[0017] Specifically, the temperature of the second solution can be any one or any two of the following: 40, 42, 44, 46, 48, 50, 52, 54, 56, 58, 60, 62, 64, 66, 68, 70, 72, 74, 76, 78, 80, 82, 84, 86, 88, and 90°C.

[0018] In some embodiments, the second solution is an aqueous solution at 45–85°C, preferably 40–70°C. This range is beneficial for further improving the boron removal efficiency of the boron removal resin.

[0019] Specifically, the temperature of the first solution and / or the third solution can be any one or any two of the following: 20, 22, 24, 26, 28, 30, 32, 34, 36, 38, 40°C.

[0020] In some embodiments, the first solution is an aqueous solution at 20–30°C.

[0021] In some embodiments, the third solution is an aqueous solution at 20–30°C.

[0022] In some embodiments, during the purification process, the rinsing is terminated when the ion exchange resin is rinsed until the resistivity of the effluent from the resistivity resin column is ≥15 MΩ·cm.

[0023] In some embodiments, the total flushing volume of the first solution, the second solution, and the third solution is 90–650 bv. The total flushing volume is the sum of the flushing volumes of the first solution, the second solution, and the third solution, and can specifically be any one or a range between any two of the following: 90, 100, 120, 140, 160, 180, 200, 220, 240, 260, 280, 300, 320, 340, 360, 380, 400, 420, 440, 460, 480, 500, 520, 540, 560, 580, 600, 620, 640, and 650 bv.

[0024] In some embodiments, the flushing volume of the first solution is 20 to 50 bv. Specifically, the flushing volume can be any one or any two of 20, 30, 40, and 50 bv.

[0025] In some embodiments, the rinsing volume of the second solution is 20–100 bv. Specifically, the rinsing volume can be any one or a range between any two of 20, 40, 60, 80, and 100 bv. Preferably, the rinsing volume is 20–50 bv, which achieves effective rinsing while reducing the amount of water used for rinsing.

[0026] In some embodiments, the rinsing volume of the third solution is 50–500 bv. Specifically, this rinsing volume can be any one or a range between any two of the following: 50, 100, 150, 200, 250, 300, 350, 400, 450, and 500 bv. This range effectively achieves a deep rinsing effect.

[0027] In some embodiments, any one or more aqueous solutions of the first solution, the second solution, and the third solution are ultrapure water. Specifically, the ultrapure water is ultrapure water with a resistivity >18 MΩ·cm.

[0028] In some embodiments, any one or more aqueous solutions of the first solution, the second solution, and the third solution are electronic-grade ultrapure water. Using electronic-grade pure ultrapure water can further improve the removal efficiency of the resin for boron removal after purification, thereby improving the cleanliness of the treated solution.

[0029] Using acid and alkali solutions with a mass fraction of 3% to 6% to clean the ion exchange resin is beneficial for achieving deep cleaning of the ion exchange resin, which in turn is more conducive to subsequent boron removal.

[0030] In this article, "electronic grade" refers to reagents with very high purity, typically above 99.9%, and containing almost no impurities or harmful substances.

[0031] In this article, "chemical grade" or "chemically pure" usually refers to reagents with a purity of 98% or higher, with fewer impurities and strictly controlled within a certain range.

[0032] In some embodiments, the acid solution is an acid solution with a mass fraction of 3% to 6%. Specifically, the mass fraction of the acid solution can be any one or a range between any two of 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, and 6%.

[0033] In some embodiments, the acid solution includes an HCl solution.

[0034] In some embodiments, the acid solution is an electronic-grade acid solution.

[0035] In some embodiments, the rinsing volume of the acid solution is 1 to 5 bv. Specifically, the rinsing volume of the acid solution can be any one or a range between any two of 1, 2, 3, 4, and 5 bv.

[0036] In some embodiments, after rinsing with an acid solution, the deep cleaning further includes rinsing the ion exchange resin with an aqueous solution to a pH of 6.5–7.5. Specifically, the pH can be any one or a range between any two of 6.5, 6.6, 6.7, 6.8, 6.9, 7.0, 7.1, 7.2, 7.3, 7.4, and 7.5.

[0037] In some embodiments, the aqueous solution is ultrapure water.

[0038] In some embodiments, the aqueous solution is electronic-grade ultrapure water.

[0039] In some embodiments, the alkaline solution is an alkaline solution with a mass fraction of 3% to 6%. Specifically, the mass fraction of the alkaline solution can be any one or a range between any two of 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, and 6%.

[0040] In some embodiments, the alkaline solution includes: NaOH solution;

[0041] In some embodiments, the alkaline solution is an electronic-grade alkaline solution;

[0042] In some embodiments, the rinsing volume of the alkaline solution is 1 to 5 bv; specifically, the rinsing volume of the alkaline solution can be any one or any two of 1, 2, 3, 4, and 5 bv.

[0043] In some embodiments, during the deep cleaning, the rinsing rate of the alkaline solution is 1 to 5 bv / h.

[0044] In some embodiments, after rinsing with an alkaline solution, the deep cleaning further includes rinsing the ion exchange resin with an aqueous solution until the resistivity of the resin column effluent is >5 MΩ·cm.

[0045] In some embodiments, prior to deep cleaning, the treatment method further includes: pre-cleaning the ion exchange resin; the pre-cleaning process includes rinsing the ion exchange resin with an aqueous solution.

[0046] In some embodiments, during the pre-cleaning process, the rinsing volume of the aqueous solution is such that the ion exchange resin is rinsed until the resistivity of the effluent from the resin column is >5 MΩ·cm.

[0047] In some embodiments, the aqueous solution is ultrapure water;

[0048] In some embodiments, the aqueous solution is electronic-grade ultrapure water.

[0049] In some embodiments, the ion exchange resin has any one of the following functional groups: N-methylglucosamine, trimethylamine, and triethylamine. Resins having any of the above functional groups are suitable for the boron removal resin treatment method provided in this application, and the treated resin has good boron removal efficiency, enabling the preparation of electronic-grade ultrapure water that meets standards.

[0050] In some embodiments, the ion exchange resin is an anion exchange resin. This application does not specifically limit the preparation process of ion exchange resins having the above-mentioned functional groups; the preparation of ion exchange resins can be based on existing disclosed related processes.

[0051] Specifically, when the ion exchange resin is an ion exchange resin having a methylglucosamine functional group, the preparation of the ion exchange resin includes: synthesizing an intermediate for the exchange resin, wherein the intermediate is obtained by crosslinking styrene and divinylbenzene; chloromethylating the intermediate; and N-methylglucosamine functionalizing the chloromethylated product.

[0052] In some embodiments, the step of synthesizing the intermediate of the exchange resin includes: mixing an oil phase and an aqueous phase; wherein the oil phase includes styrene, divinylbenzene, an initiator and a porogen, and the aqueous phase includes a solution of water (saturated saline), hydroxyethyl methyl cellulose (HEMC) and gelatin (the dissolution temperature may be 40–50°C); heating the mixture of the oil phase and the aqueous phase to 75–80°C within 60–70 min, holding at that temperature for 2–4 h, heating to 80–88°C within 5–20 min, holding at that temperature for 1–3 h, and heating to 90–95°C within 10–30 min, holding at that temperature for 4–6 h, to obtain the intermediate.

[0053] In some embodiments, the mass ratio of styrene to divinylbenzene is 10–14:90–100. Specifically, this mass ratio can be 10:90, 12:90, 14:90, 10:95, 12:95, etc.

[0054] The range between any one or any two of 14:95, 10:100, 12:100, and 14:100.

[0055] In some embodiments, the initiator includes benzoyl peroxide.

[0056] In some embodiments, the porogen includes toluene.

[0057] In some embodiments, the purity of divinylbenzene (DVB) is 60-70%.

[0058] In some embodiments, for every 10-14 g of divinylbenzene with a purity of 63% (wt%), 90-100 g of styrene (ST), 65-70 g of toluene, and 0.8-1 g of benzoyl peroxide (BPO) are added.

[0059] In some embodiments, 1-2g HEMC and 2-3g gelatin are added to every 300-450mL of saturated saline solution, and the solution is heated to 40-45°C to dissolve and obtain an aqueous phase.

[0060] In some embodiments, the step of chloromethylating the intermediate includes:

[0061] Chloromethyl ether is prepared by adding thionyl chloride or sulfonyl chloride dropwise to a mixture of methyl acetal and paraformaldehyde and stirring. Chloromethyl ether is then prepared by adding thionyl chloride or sulfonyl chloride dropwise to the mixture of methyl acetal and paraformaldehyde. The intermediate is added to the prepared chloromethyl ether and soaked for 2–4 hours. After reacting with a catalyst for 0.5–1.5 hours, paraformaldehyde is added and stirred until homogeneous. Thionyl chloride or sulfonyl chloride is added to convert the methyl acetal produced in the side reaction back into chloromethyl ether. Chloromethylation is completed when the chlorine content of the chlorospheres reaches 10%–20%.

[0062] In some embodiments, the catalyst comprises any one or two of ferric chloride, zinc chloride, and tin chloride.

[0063] In some embodiments, the step of functionalizing the chloromethylated product with N-methylglucosamine includes: drying the chloromethylated product at 60-80°C for 20-28 hours to obtain dried resin-based spheres; soaking the dried resin-based spheres in ethanol to allow them to swell fully; adding an N-methylglucosamineizing agent; heating to 60-75°C and reacting at a constant temperature for 24-30 hours to obtain an N-methylglucosamine-functionalized resin.

[0064] In some embodiments, 8-25g of N-methylglucosamine reagent is added per 100-200g of resin-based balls.

[0065] On the other hand, embodiments of the present invention also provide a method for preparing boron-removing resin, which includes: treating the prepared boron-removing resin using the processing method described in any of the foregoing embodiments.

[0066] Furthermore, the embodiments of the present invention also provide the application of boron-removing resin obtained by the processing method described in any of the foregoing embodiments or boron-removing resin prepared by the preparation method described in any of the foregoing embodiments in boron removal or preparation of electronic-grade ultrapure water;

[0067] In some embodiments, the preparation of electronic-grade ultrapure water includes: removing boron from the ultrapure water using the boron removal resin.

[0068] In some embodiments, the boron removal step includes: passing the reagent to be removed through a resin column of the boron removal resin at a set flow rate of 40–100 bv / h. Specifically, the set flow rate can be any one or any combination of 40, 50, 60, 70, 80, 90, and 100 bv / h. Within this set flow rate range, the boron concentration can be reduced to below 5 ng / L. Exceeding this range may result in an increase in the boron concentration after treatment, failing to meet application requirements.

[0069] In some preferred embodiments, the set flow rate is 40–60 bv / h.

[0070] In some embodiments, the boron removal includes using a boron removal system, which may include: a nitrogen-sealing water tank, a boron removal resin column, a water supply system (pressurization pump), a TOC digestion device, and a terminal polishing resin column.

[0071] When performing boron removal, the boron removal resin can be filled in the boron removal resin column between the nitrogen sealing water tank and the terminal polishing resin column, or mixed with the terminal polishing resin in the terminal polishing resin column.

[0072] The features and performance of the present invention will be further described in detail below with reference to embodiments.

[0073] Example 1

[0074] A method for preparing an electronic-grade boron removal resin, comprising the following steps:

[0075] (1) Preparation of ion exchange resins with N-methylglucosamine functional groups

[0076] 1.1 Polymerization of white spheres (intermediate)

[0077] Prepare the aqueous phase for polymerization according to the following composition: 320 mL saturated brine, 1.2 g HEMC, and 2.3 g gelatin. Add them to a 1000 mL reactor and heat to 45 °C to dissolve.

[0078] The polymerization oil phase is prepared according to the following composition: 63% pure DVB: 12g, ST: 85.3g, toluene 68g, benzoyl peroxide BPO: 0.85g.

[0079] Mix the aqueous and oil phases, raise the temperature to 78°C within about 65 minutes, hold at 78°C for 3 hours, raise the temperature to 88°C within 5-20 minutes and hold for 2 hours, and finally raise the temperature to 95°C within the last 20 minutes and hold for 5 hours.

[0080] Washing: Filter mother liquor, wash 3-5 times with hot water, and boil in water to remove toluene.

[0081] 1.2 Chloromethylation of white spheres

[0082] The white spheres obtained in step 1.1 were soaked in chloromethyl ether and stirred at 40°C (100 rpm).

[0083] 10 hours; add zinc chloride (1% of the mass of the white ball); then add paraformaldehyde (40% of the mass of the white ball) and stir evenly; add thionyl chloride again (40% of the mass of the white ball; in other embodiments, sulfonyl chloride can be added) to convert the methyl acetal produced by the side reaction back into chloromethyl ether. When the chloro acetal content reaches more than 10% (in other embodiments, it can be 10%-20%), the chloromethylation is complete.

[0084] 1,3N-methylglucosamine functionalization

[0085] Weigh the resin obtained in step 1.2 and dry it in a constant temperature oven at 60℃ for 24 hours to obtain resin-based spheres. Take 100g of the dried resin-based spheres into a reactor, soak the resin in ethanol to make it fully swollen, and rinse the resin-based spheres with deionized water or pure water. After stirring for 1 hour, add 18g of N-methylglucosamine reagent, raise the temperature to 75℃ and react at a constant temperature for 24 hours. Filter out the solution and wash it with pure water to obtain N-methylglucosamine functionalized resin.

[0086] In other embodiments, other commercially available N-methylglucosamine functionalized resins may also be used.

[0087] (2) Pre-cleaning

[0088] Weigh 800 ml of the ion exchange resin with N-methylglucosamine functional group obtained in the preparation and place it in a 1 L PVDF exchange column. Rinse with electronic grade ultrapure water until the resistivity of the water effluent from the resin column is >5 MΩ·cm.

[0089] (3) Deep cleaning

[0090] The resin was pretreated with a 4wt% dilute hydrochloric acid solution prepared with electronic grade HCl, with a treatment volume of 2bv, and then rinsed with ultrapure water until neutral.

[0091] Then, the resin was cleaned with electronic-grade NaOH at a concentration of 4 wt% at a rate of 2 bv / h, with a treatment volume of 2 bv.

[0092] The resin is cleaned with electronic-grade ultrapure water until the resistivity of the effluent is >5 MΩ·cm.

[0093] (4) Purification treatment

[0094] The resin obtained in step (3) was cleaned with electronic-grade ultrapure water at 25°C, 80°C, and 25°C, respectively. The total rinsing volumes of electronic-grade ultrapure water at 25°C, 80°C, and 25°C were 40bv, 20bv, and 440bv, respectively, until the resistivity was not less than 17MΩ·cm. Electronic-grade boron-removing resin was obtained.

[0095] The application performance of the prepared electronic-grade boron removal resin was investigated.

[0096] 0.3 μg / L boron ion ultrapure water was prepared using electronic-grade ultrapure water and flowed through the resin column at 50 bv / h via an ultra-clean pipeline. After stable operation for 1 hour, the boron ion concentration at the resin column outlet was detected using a boron meter. The outlet boron concentration was <0.002 μg / L. The TOC at the resin column inlet and outlet was measured using a TOC meter to evaluate the boron removal resin delta TOC <4 ppb.

[0097] Example 2

[0098] A method for preparing an electronic-grade boron-removing resin, the preparation method being the same as in Example 1, and the application performance of the prepared electronic-grade boron-removing resin being investigated:

[0099] 0.3 μg / L boron ion ultrapure water was prepared using electronic-grade ultrapure water and flowed through the resin column at 60 bv / h via an ultra-clean pipeline. After stable operation for 1 hour, the boron ion concentration at the resin column outlet was detected using a boron meter. The outlet boron concentration was <0.003 μg / L. The TOC at the resin column inlet and outlet was measured using a TOC meter to evaluate the boron removal resin delta TOC <2 ppb.

[0100] Example 3

[0101] A method for preparing an electronic-grade boron removal resin, the steps are roughly the same as in Example 1, the difference being step (4), which is as follows:

[0102] The resin obtained in step (3) was cleaned with electronic-grade ultrapure water at 25°C, 60°C and 25°C respectively. The rinsing volumes of electronic-grade ultrapure water at 25°C, 60°C and 25°C were 40bv, 40bv and 420bv respectively, until the resistivity was not less than 17MΩ·cm.

[0103] The application performance of the prepared electronic-grade boron removal resin was investigated.

[0104] 0.3 μg / L boron ion ultrapure water was prepared using electronic-grade ultrapure water and flowed through the resin column at 60 bv / h via an ultra-clean pipeline. After stable operation for 1 hour, the boron ion concentration at the resin column outlet was detected using a boron meter. The outlet boron concentration was <0.005 μg / L. The TOC at the resin column inlet and outlet was evaluated using a TOC meter. The delta TOC of the boron-removing resin was <5 ppb.

[0105] Example 4

[0106] The effect of the temperature of the first, second, and third solutions on the boron removal efficiency was verified.

[0107] Multiple experimental groups were set up, and each group provided a method for preparing electronic-grade boron removal resin. The steps were roughly the same as in Example 1, except for step (4), which is as follows:

[0108]

[0109]

[0110] The application performance of the electronic-grade boron removal resins prepared in the experimental groups was investigated respectively:

[0111] A 0.3 μg / L concentration of boron ion ultrapure water was prepared using electronic-grade ultrapure water and flowed through a resin column at 60 bv / h via an ultra-clean pipeline. After stable operation for 1 hour, the boron ion concentration at the resin column outlet was measured using a boron meter. The results are as follows:

[0112]

[0113]

[0114] Example 5

[0115] A method for preparing an electronic-grade boron removal resin, the steps are roughly the same as in Example 1, the difference being step (3), which is as follows:

[0116] The resin was pretreated with a 4wt% dilute hydrochloric acid solution prepared with chemically pure HCl at a treatment volume of 2 bv, and then rinsed with ultrapure water until neutral. Then, a 4wt% dilute hydrochloric acid solution prepared with chemically pure NaOH was used for deep conversion at a rate of 2 bv / h, with a treatment volume of 2 bv, followed by rinsing with electronic-grade ultrapure water until the resistivity was >5 MΩ·cm.

[0117] The application performance of the prepared electronic-grade boron removal resin was investigated.

[0118] 0.3 μg / L boron ion ultrapure water was prepared using electronic-grade ultrapure water and flowed through the resin column at 60 bv / h via an ultra-clean pipeline. After stable operation for 1 hour, the boron ion concentration at the resin column outlet was detected using a boron meter. The outlet boron concentration was <0.058 μg / L. The TOC at the resin column inlet and outlet was measured using a TOC meter to evaluate the boron removal resin delta TOC <10 ppb.

[0119] Example 6

[0120] A method for preparing an electronic-grade boron removal resin is generally the same as that in Example 1, except that the ion exchange resin with N-methylglucosamine functional group is selected from commercially available foreign brand D, which has a polypropylene backbone structure and N-methylglucosamine functional group.

[0121] After obtaining the resin, the resin was subjected to deep cleaning and purification treatment according to steps (2), (3), and (4) in Example 1.

[0122] The application performance of the treated resin was investigated:

[0123] 0.3 μg / L boron ion ultrapure water was prepared using electronic-grade ultrapure water and flowed through the resin column at 50 bv / h via an ultra-clean pipeline. After stable operation for 1 hour, the boron ion concentration at the resin column outlet was detected using a boron meter. The outlet boron concentration was <0.005 μg / L. The TOC at the resin column inlet and outlet was measured using a TOC meter to evaluate the boron removal resin delta TOC <4.4 ppb.

[0124] Comparative Example 1

[0125] A method for preparing an electronic-grade boron removal resin, the steps are roughly the same as those in Example 1, except that steps (3) and (4) of Example 1 are omitted.

[0126] The application performance of the prepared electronic-grade boron removal resin was investigated.

[0127] 0.3 μg / L boron ion ultrapure water was prepared using electronic-grade ultrapure water and flowed through the resin column at 60 bv / h via an ultra-clean pipeline. After stable operation for 1 hour, the boron ion concentration at the resin column outlet was detected using a boron meter. The outlet boron concentration was <0.290 μg / L. The TOC at the resin column inlet and outlet was measured using a TOC meter to evaluate the boron removal resin delta TOC <800 ppb.

[0128] The above description is merely a preferred embodiment of the present invention and is not intended to limit the invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A method for treating a boron-removing resin, characterized by, It comprises: The ion exchange resin for removing boron after deep cleaning is subjected to a purification treatment; The deep cleaning step comprises: using an acid solution and an alkali solution to rinse the ion exchange resin; The purification treatment comprises: using a first solution, a second solution and a third solution to rinse the ion exchange resin after deep cleaning, respectively; the first solution is an aqueous solution at 20-30℃, the second solution is an aqueous solution at 45-85℃, and the third solution is an aqueous solution at 20-30℃; The rinsing volume of the first solution is 20-50bv; The rinsing volume of the second solution is 20-100bv; The rinsing volume of the third solution is 50-500bv.

2. The treatment method according to claim 1, characterized in that, In the process of the purification treatment, the end condition of rinsing is to rinse the ion exchange resin to a resin column water outlet resistivity≥15MΩ·cm.

3. The treatment method of claim 1, wherein Any one or more of the aqueous solutions of the first solution, the second solution and the third solution is ultrapure water.

4. The treatment method according to claim 3, characterized in that, The ultrapure water is ultrapure water with a resistivity>18MΩ·cm.

5. The treatment method of claim 1, wherein The acid solution is an acid solution with a mass fraction of 3%-6%.

6. The treatment method of claim 5, wherein, The acid solution comprises: an HCl solution.

7. The treatment method of claim 5, wherein The acid solution is an electronic grade acid solution.

8. The treatment method of claim 1, wherein, The rinsing volume of the acid solution is 1-5bv.

9. The treatment method of claim 1, wherein, After rinsing with the acid solution, the deep cleaning further comprises using an aqueous solution to rinse the ion exchange resin to a pH of 6.5-7.

5.

10. The processing method according to claim 9, wherein The aqueous solution is ultrapure water.

11. The treatment method of claim 9, wherein, The aqueous solution is electronic grade ultrapure water.

12. The treatment method of claim 1, wherein, The alkali solution is an alkali solution with a mass fraction of 3%-6%.

13. The treatment method according to claim 12, characterized in that, The alkali solution comprises: an NaOH solution.

14. The processing method of claim 12, wherein, The alkali solution is an electronic grade alkali solution.

15. The treatment method of claim 1, wherein, The rinsing volume of the alkali solution is 1-5bv.

16. The treatment method of claim 1, wherein When performing the deep cleaning, the rinsing speed of the alkali solution is 1-5bv / h.

17. The treatment method of claim 1, wherein, After rinsing with the alkali solution, the deep cleaning further comprises using an aqueous solution to rinse the ion exchange resin to a resin column water outlet resistivity>5MΩ·cm.

18. The treatment method according to any one of claims 1 to 17, characterized in that, Before performing the purification treatment, the treatment method comprises the step of performing the deep cleaning.

19. The treatment method of claim 18, wherein, Before performing the deep cleaning, the treatment method further comprises: performing a pre-cleaning treatment on the ion exchange resin; the pre-cleaning treatment comprises using an aqueous solution to rinse the ion exchange resin.

20. The processing method according to claim 19, wherein, In the process of the pre-cleaning, the rinsing volume of the aqueous solution is to rinse the ion exchange resin to a resin column water outlet resistivity>5MΩ·cm.

21. The treatment method of claim 19, wherein, The aqueous solution is ultrapure water.

22. The treatment method of claim 19, wherein, The aqueous solution is electronic grade ultrapure water.

23. The treatment method according to any one of claims 1 to 17, characterized in that, The ion exchange resin has any one of the following functional groups: N-methyl glucosamine, trimethylamine and triethylamine.

24. The treatment method of claim 23, wherein, The ion exchange resin is an anion exchange resin.

25. A method for preparing a boron-removing resin, characterized by, It comprises: The treatment method of any one of claims 1-24 is used to treat the boron-removing resin prepared.

26. The application of the boron-removing resin treated by the treatment method of any one of claims 1-24 or the boron-removing resin prepared by the preparation method of claim 25 in boron removal or preparation of electronic grade ultrapure water.

27. The use according to claim 26, characterized in that, The preparation of electronic grade ultrapure water comprises: using the boron-removing resin to remove boron from ultrapure water.

28. The use according to claim 27, characterized in that, The step of removing boron includes flowing the boron-removal reagent through the resin column of the boron-removal resin at a set flow rate of 40-100 bv / h.

29. The use according to claim 28, characterized in that, The set flow rate is 40-60 bv / h.

Images