Preparation method and system of gel type anion exchange resin

Abstract

The invention provides a preparation method and system of gel type anion exchange resin, and belongs to the technical field of production control, and the preparation method specifically comprises the following steps: cooling an amination kettle by taking a target temperature as a control target, neutralizing the amination kettle according to a preset neutralization strategy and liquid caustic soda, adding an amination mother liquor, determining that the pH value is not changed, and then adding the amination mother liquor into the amination kettle; dropwise adding trimethylamine according to a preset dropwise adding strategy, carrying out heat preservation treatment according to a preset temperature after dropwise adding is finished, starting cooling water after heat preservation is finished, sampling and detecting data of residual amine and exchange capacity are qualified, carrying out acidification transformation on the resin according to a preset acidification strategy, and after the pH value reaches a target and is kept unchanged, putting the material into a washing bucket, starting to wash the material until the material is neutral, sampling, detecting data of a finished product, and discharging to obtain the finished product, so that the purity of a preparation result of the gel type anion exchange resin is improved.

Description

Technical Field

[0001] The invention belongs to the technical field of data processing, and in particular relates to a method for preparing a gel-type anion exchange resin. Background Art

[0002] Gel-type ion exchange resin is a type of ion exchange resin. Ion exchange resins with a transparent homogeneous gel structure, which are formed by condensation or polymerization of a pure monomer mixture, are collectively referred to as gel-type resins. They are generally synthesized into a spherical matrix using a suspended co-condensation or copolymerization process, and then activated by a chemical reaction and introduced with ion exchange groups. Therefore, how to prepare and process gel-type anion exchange resins has become a technical problem that needs to be solved urgently.

[0003] In view of the above technical problems, the present application specifically provides a method for preparing a gel-type anion exchange resin. Summary of the invention

[0004] To achieve the purpose of the present invention, the present invention adopts the following technical solutions: According to one aspect of the present invention, a method for preparing a gel-type anion exchange resin is provided.

[0005] A method for preparing a gel-type anion exchange resin, specifically comprising: Put the white ball into the reaction kettle, open the vacuum, add a specified amount of chloromethyl ether under reduced pressure, swell the white ball in the chloromethyl ether, add zinc chloride, and heat it according to the preset strategy. After reaching the target temperature, keep it warm until the chlorine content test result is qualified, cool the temperature in the kettle, filter the mother liquor, vacuum control the reaction kettle, extract it according to the preset strategy, and then discharge it into the amination kettle; After cooling the amination kettle with the target temperature as the control target, neutralizing the amination kettle with liquid alkali according to the preset neutralization strategy, adding the amination mother liquor to determine that the pH value does not change, and then dripping trimethylamine according to the preset dripping strategy; After the addition is completed, the temperature is kept at the preset temperature until the end of the insulation. After the residual amine and exchange capacity data are sampled and tested and qualified, the cooling water is turned on, and the resin is acidified and transformed according to the preset acidification strategy. After the pH value reaches the target and remains unchanged, the material is placed in the washing barrel and the washing operation is started. After washing to neutrality, the finished product data is sampled and tested and the material is discharged to obtain the finished product.

[0006] The beneficial effects of the present invention are: Through vacuum control and heat preservation treatment, the material exchange with the external environment is reduced, and the reliability of the preparation and treatment results of the gel-type anion exchange resin is improved. At the same time, through heat preservation treatment, the material properties of the chemical substances can be kept stable, thereby improving the reliability of the preparation results.

[0007] By performing extraction treatment according to a preset strategy and then discharging the material into an amination kettle for amination treatment, the influence of unnecessary impurities on the reliability of the amination treatment result and the influence of impurities in the preparation result are avoided, thereby ensuring that the quality of the preparation result can meet the requirements.

[0008] A further technical solution is to add a prescribed amount of chloromethyl ether under reduced pressure, specifically comprising: Close the cooler of the reactor and the valve of the tail gas main pipe, then open the vacuum and add chloromethyl ether under reduced pressure; After adding the specified amount of chloromethyl ether, turn off the vacuum, open the vent valve, release the vacuum in the kettle and then close the vent valve, then open the valve of the tail gas main pipe, and finally start stirring to allow the white ball to swell in chloromethyl ether for 1 hour.

[0009] A further technical solution is to perform a temperature increase process according to a preset strategy, specifically including: After adding the catalyst zinc chloride, control the temperature to slowly rise to 40 ± 1°C within 1.5 hours and start timing. If the heating rate does not meet the requirements, use the amount of cooling water to adjust the temperature until the chlorination temperature is reached; The chlorination temperature was controlled at 45±1℃ and the chlorination holding time was 12 hours.

[0010] A further technical solution is to perform extraction processing according to a preset strategy, specifically including: Pour in 1 ton of the first extraction liquid, stir for 1 hour, and then filter out the first extraction liquid; Then add 1 ton of the second extract, stir for 10 minutes and then filter; The third extraction uses methylal solution, which is then discharged into the amination kettle.

[0011] A further technical solution is to perform a material washing operation, which specifically includes: Put the material into the washing bucket and start the material washing operation. Wash the resin in eight levels until it is neutral. Then use tap water to pump the material into the packager and take samples to test the finished product data.

[0012] In a second aspect, the present invention provides a computer system comprising: a memory and a processor that are communicatively connected, and a computer program stored in the memory and capable of running on the processor, wherein the processor executes the above-mentioned method for preparing a gel-type anion exchange resin when running the computer program.

[0013] Other features and advantages will be described in the following description, and partly become apparent from the description, or understood by practicing the invention. The purpose and other advantages of the invention are realized and obtained by the structures particularly pointed out in the description and the drawings.

[0014] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, preferred embodiments are given below and described in detail with reference to the accompanying drawings. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] The above and other features and advantages of the present invention will become more apparent by describing in detail exemplary embodiments thereof with reference to the attached drawings.

[0016] Figure 1 It is a flow chart of a method for preparing a gel-type anion exchange resin; Figure 2 It is a flow chart for judging that the heating rate does not meet the requirements; Figure 3 It is a flow chart of the method of controlling the dropping speed of the hydrochloric acid solution. DETAILED DESCRIPTION

[0017] Example embodiments will now be described more fully with reference to the accompanying drawings. However, example embodiments can be implemented in a variety of forms and should not be construed as limited to the embodiments set forth herein; rather, these embodiments are provided so that the present invention will be comprehensive and complete and fully convey the concepts of the example embodiments to those skilled in the art. The same reference numerals in the figures represent the same or similar structures, and thus their detailed description will be omitted.

[0018] The terms "a", "an", "the", and "said" are used to indicate the presence of one or more elements / components / etc.; the terms "comprising" and "having" are used to express an open-ended inclusive meaning and mean that additional elements / components / etc. may be present in addition to the listed elements / components / etc.

[0019] To solve the above problems, according to one aspect of the present invention, Figure 1 According to one aspect of the present invention, a method for preparing a gel-type anion exchange resin is provided, which specifically comprises: Put the white ball into the reaction kettle, open the vacuum, add a specified amount of chloromethyl ether under reduced pressure, swell the white ball in the chloromethyl ether, add zinc chloride, and heat it according to the preset strategy. After reaching the target temperature, keep it warm until the chlorine content test result is qualified, cool the temperature in the kettle, filter the mother liquor, vacuum control the reaction kettle, extract it according to the preset strategy, and then discharge it into the amination kettle; After cooling the amination kettle with the target temperature as the control target, neutralizing the amination kettle with liquid alkali according to the preset neutralization strategy, adding the amination mother liquor to determine that the pH value does not change, and then dripping trimethylamine according to the preset dripping strategy; After the addition is completed, the temperature is kept at the preset temperature until the end of the insulation. After the residual amine and exchange capacity data are sampled and tested and qualified, the cooling water is turned on, and the resin is acidified and transformed according to the preset acidification strategy. After the pH value reaches the target and remains unchanged, the material is placed in the washing barrel and the washing operation is started. After washing to neutrality, the finished product data is sampled and tested and the material is discharged to obtain the finished product.

[0020] Further, a prescribed amount of chloromethyl ether is added under reduced pressure, specifically comprising: Close the cooler of the reactor and the valve of the tail gas main pipe, then open the vacuum and add chloromethyl ether under reduced pressure; After adding the specified amount of chloromethyl ether, turn off the vacuum, open the vent valve, release the vacuum in the kettle and then close the vent valve, then open the valve of the tail gas main pipe, and finally start stirring to allow the white ball to swell in chloromethyl ether for 1 hour.

[0021] Optionally, the temperature is raised according to a preset strategy, specifically including: After adding the catalyst zinc chloride, control the temperature to slowly rise to 40 ± 1°C within 1.5 hours and start timing. If the heating rate does not meet the requirements, use the amount of cooling water to adjust the temperature until the chlorination temperature is reached; The chlorination temperature was controlled at 45±1℃ and the chlorination holding time was 12 hours.

[0022] Specifically, the extraction process is performed according to a preset strategy, including: Pour in 1 ton of the first extraction liquid, stir for 1 hour, and then filter out the first extraction liquid; Then add 1 ton of the second extract, stir for 10 minutes and then filter; The third extraction uses methylal solution, which is then discharged into the amination kettle.

[0023] Further, the amination kettle is neutralized according to the preset neutralization strategy and liquid alkali, specifically including: Add liquid alkali to the reactor dropwise. The dropping speed should strictly follow the principle of slow first and fast later. The first hour should not be more than 80 kg, and the following hour should not be more than 120 kg. When the pH value reaches 8, stop dropping and start stirring for 1 hour. Measure the pH value of the bottom liquid again. It must stably reach pH 8, otherwise continue to add liquid alkali.

[0024] It is understandable that after the neutralization treatment, a small amount of resin particles need to be taken and observed under a microscope to see if there are any broken balls.

[0025] Further, trimethylamine is added dropwise according to a preset dropping strategy, specifically comprising: The dripping speed should strictly follow the principle of slow first and then fast, 120kg in the first hour, 180kg in the second hour, 250kg in the third hour, and gradually increase the dripping speed; The specific amount of dropwise addition is 1500 kg. If the pressure in the amination reactor is not within the preset pressure range during the dropwise addition, the dropwise addition speed should be slowed down or suspended. The reaction temperature should be controlled not to be higher than 32° C. during the dropwise addition.

[0026] It should be noted that the data of residual amine and exchange capacity tested by sampling are qualified, including: The residual amine should be ≤1%, and the exchange volume should be ≥3.5mmoL / g. If the residual amine is too low, trimethylamine can be added. If it is too high, continue to keep warm for 1 hour and then test again.

[0027] Specifically, the acidification transformation of the resin is carried out according to the preset acidification strategy, which specifically includes: Turn on the cooling water to lower the temperature in the kettle to below 30°C, and add hydrochloric acid solution into the kettle for 2 hours to carry out acidification transformation of the resin. The dropping speed also follows the principle of slow first and then fast. The temperature in the kettle is controlled below 30°C. The end point pH value after transformation is controlled at 3~4, and it is stabilized for 1 hour to ensure that the pH remains stable.

[0028] It is understandable that the material washing operation specifically includes: Put the material into the washing bucket and start the material washing operation. Wash the resin in eight levels until it is neutral. Then use tap water to pump the material into the packager and take samples to test the finished product data.

[0029] It should be noted that if Figure 2 As shown, it is judged that the heating rate does not meet the requirements, specifically including: Determine the temperature data at different heating moments based on the analysis results of the temperature data at different heating moments; Based on the temperature data, the addition data of the catalyst zinc chloride and chloromethyl ether, determining the data similarity coefficients of the addition data and the temperature data with different historical heating treatment times; The similar processing times in the historical heating processing times are determined according to the data similarity coefficient, and whether the heating data meets the requirements is determined according to the temperature change data in the similar processing times.

[0030] Furthermore, the similarity processing times are the historical temperature rise processing times in which the data similarity coefficient is greater than a preset similarity coefficient.

[0031] Optionally, determining whether the temperature rise data meets the requirements based on the temperature change data in similar processing times includes: The abnormal temperature change moments in different similar processing times are determined according to the temperature change data in similar processing times, and whether the temperature rise data meets the requirements is determined by the quantitative average value of the abnormal temperature change moments in different similar processing times.

[0032] Further, when the quantity average value is greater than a preset quantity threshold, it is determined that the temperature rise data does not meet the requirements.

[0033] Optionally, judging that the heating rate does not meet the requirement includes: S11 determines the temperature data at different heating moments based on the analysis results of the temperature data at different heating moments, and determines the temperature change moment in the heating process stage based on the analysis results of the temperature data; Optionally, the above step S11 includes the following contents: S111 determines the temperature data at different heating moments based on the analysis results of the temperature data at different heating moments, and determines the temperature change moments in the heating process using the analysis results of the temperature data. When the number of the temperature change moments does not meet the requirement, it is determined that the temperature speed does not meet the requirement. When the number of the temperature change moments meets the requirement, the process proceeds to step S112. S112 determines the temperature variation in different unit time periods according to the number of temperature variation moments in different unit time periods and the temperature variation at different temperature variation moments. When the number of unit time periods in which the temperature variation does not meet the requirement is greater than the number of preset time periods, it is determined that the temperature speed does not meet the requirement. When the number of unit time periods in which the temperature variation does not meet the requirement is not greater than the number of preset time periods, the process proceeds to step S113. S113 determines the change of the temperature change in different adjacent unit time periods based on the temperature change in different unit time periods, and determines the changing unit time period within the unit time period based on the change. When the changing unit time period changes with time, the change of the temperature change gradually increases, then it is determined that the temperature speed does not meet the requirements. When the changing unit time period changes with time, the change of the temperature change does not gradually increase, then go to step S12.

[0034] S12: based on the temperature data, the addition data of the catalyst zinc chloride and chloromethyl ether, determining the data similarity coefficients of the addition data and the temperature data with different historical heating treatment times, determining similar treatment times in the historical heating treatment times according to the data similarity coefficients, and determining the temperature change moments in different similar treatment times and the temperature change amounts at different temperature change moments according to the temperature change data in the similar treatment times, and determining the temperature change abnormality coefficients in different similar treatment times using the temperature change moments and the temperature change amounts at different temperature change moments; Optionally, the above step S12 includes the following contents: S121, based on the temperature data, the addition data of the catalyst zinc chloride and chloromethyl ether, determining the data similarity coefficients of the addition data and the temperature data with different historical heating treatment times, determining similar treatment times in the historical heating treatment times according to the data similarity coefficients, and determining the temperature change moments in different similar treatment times according to the temperature change data in the similar treatment times; S122: When there is a similar processing number of times when the number of temperature change moments is greater than the preset number of change moments, it is determined that the temperature speed does not meet the requirement; when there is no similar processing number of times when the number of temperature change moments is greater than the preset number of change moments, the process proceeds to step S123; S123 uses the temperature change moment and the temperature change amount at different temperature change moments to determine the temperature change anomaly coefficient in different similar processing times. When there are similar processing times whose temperature change anomaly coefficient does not meet the requirements, it is determined that the temperature speed does not meet the requirements. When there are no similar processing times whose temperature change anomaly coefficient does not meet the requirements, go to step S13.

[0035] S13 determines the weight coefficients of different similar processing times based on the data similarity coefficients of different similar processing times, and determines the comprehensive change abnormality coefficient based on the temperature change abnormality coefficients of different similar processing times, and judges whether the heating rate meets the requirements according to the comprehensive change abnormality coefficient.

[0036] Specifically, Figure 3 As shown, the method for controlling the dripping speed of the hydrochloric acid solution is: Determine the temperature variation interval of the kettle temperature within a preset period of time determined by the monitoring data of the kettle temperature based on the analysis results of the monitoring data of the kettle temperature and the pH value, and determine the preset droplet acceleration corresponding to the number of temperature variation moments within the preset period of time under the temperature variation interval by using the number of temperature variation moments within the preset period of time under the temperature variation interval; According to the pH value interval corresponding to the pH value in the preset time period, determine the number of pH value change moments in the preset time period under the pH value interval, and use the number of pH value change moments in the preset time period under the pH value change interval to determine the preset dripping speed corresponding to the number of pH value change moments in the pH value change interval; The minimum value of the preset drop acceleration corresponding to the number of temperature change moments and the preset drop acceleration corresponding to the number of pH value change moments is used as the control method of the drop acceleration of the hydrochloric acid solution.

[0037] Furthermore, the method for controlling the dripping acceleration of the hydrochloric acid solution is to control the dripping acceleration according to the minimum value.

[0038] Optionally, the method for controlling the dropping speed of the hydrochloric acid solution is: Determine the temperature change moment of the kettle temperature within a preset time period based on the monitoring data of the kettle temperature and the pH value according to the analysis results of the monitoring data of the kettle temperature, and when the number of the temperature change moments does not meet the requirement, determine the dripping speed of the hydrochloric acid solution using the preset dripping speed; When the number of temperature change moments meets the requirement: Determine the number of pH value change moments within the preset period of time according to the monitoring data of the pH value within the preset period of time, and when the number of pH value change moments does not meet the requirement, determine the dripping speed of the hydrochloric acid solution using the preset dripping speed; When the number of pH value change moments meets the requirement: Determine the temperature variation range of the temperature in the kettle within a preset period of time based on the monitoring data of the temperature in the kettle, and determine the basic dripping acceleration of the hydrochloric acid solution according to the pH value range and the temperature variation range corresponding to the pH value within the preset period of time; When the basic dropping acceleration is within a preset dropping acceleration range, the dropping acceleration of the hydrochloric acid solution is determined using the basic dropping acceleration; When the basic dripping speed is not within the preset dripping speed range: The temperature variation coefficient is determined by using the number of temperature variation moments within the preset time period under the temperature variation interval and combining the variation amounts of different temperature variation moments, and the pH variation coefficient is determined by using the number of pH variation moments within the preset time period under the pH variation interval and the variation amount of pH at the pH variation moments; When the temperature variation coefficient and the pH variation coefficient both meet the requirements, the basic dropping speed is used to determine the dropping speed of the hydrochloric acid solution; When any one of the temperature variation coefficient and the pH variation coefficient does not meet the requirements, the temperature variation coefficient and the pH variation coefficient are used to correct the basic dripping acceleration to determine the dripping acceleration control value, and the dripping acceleration control value is used to determine the control method of the dripping acceleration of the hydrochloric acid solution.

[0039] In one embodiment: 3.1 Raw material ratio White ball: 1100kg Chloromethyl methyl ether: 2200kg (chlorine content 40%~42%, aldehyde content ≧35%) Zinc chloride: 250kg Methylal: 1100kg Liquid caustic soda: (100~400) kg Trimethylamine solution: (1400~1550) kg (concentration is 30%). When the concentration of trimethylamine is 40%, the dosage should be reduced proportionally.

[0040] Hydrochloric acid: (300~400) kg 3.2 Process control indicators 3.2.1 During the chlorination reaction, allow the white ball to swell in chloromethyl ether for 1 hour.

[0041] 3.2.2 During chlorination insulation, control the temperature at 45±1℃ and the insulation time for 12h.

[0042] 3.2.3 After chlorination and heat preservation, sampling and testing are qualified if the chlorine content is ≥17%.

[0043] 3.2.4 During the neutralization process of amination reaction, the temperature in the kettle shall not be higher than 20°C. After neutralization, the mother liquor of amination shall be added. The pH value of the solution was then controlled at 8.

[0044] 3.2.5 During the amination reaction, the temperature in the kettle must not be higher than 32°C.

[0045] 3.2.6 During the insulation process of the amination reaction, the temperature in the kettle was controlled at 31±1℃ and the insulation time was 3h.

[0046] 3.2.7 When sampling and testing the amination reaction, the residual amine should be ≤1% and the exchange capacity should be ≥3.5mmoL / g.

[0047] 3.2.8 During the acidification transformation of the amination reaction, the temperature in the kettle is controlled below 30°C, and the pH value at the end point after the transformation is controlled At 3~4.

[0048] 4. Production operation methods 4.1 Preparation before feeding 4.1.1 Rinse the reactor clean and wipe it dry or bake it to ensure that there is no water on the reactor wall.

[0049] 4.1.2 Open the discharge valve of the chloromethyl ether storage tank, the feed valve of the sedimentation tank, and the inlet and outlet valves of the chloromethyl ether pump at once, and then Start the chloromethyl ether pump and pump the chloromethyl ether into the sedimentation tank. After standing for 5 hours, put the chloromethyl ether sediment into the lower In the sinking liquid storage tank, make sure the sinking liquid is drained clean.

[0050] 4.1.3 Pump chloromethyl ether and methylal into their respective high-level metering tanks, and fill in the detailed operation instructions after correct measurement. Keep records.

[0051] 4.1.4 During all the material processing, you must concentrate your mind and not leave your post to do other work to prevent the original Material spill accidents occurred.

[0052] 4.1.5 Close the discharge valve at the bottom of the chlorination kettle and each filter discharge valve, open the cooler and cooling water, and open The space and size vary with the temperature and season.

[0053] 4.1.6 Place the white balls and zinc chloride raw materials next to the chlorination kettle, check the model and quantity, and fill in the operation details. Record.

[0054] 4.2 Chloromethylation reaction 4.2.1 Feed the white balls into the reactor. The model and quantity shall be strictly in accordance with the process parameters. The valves of the reactor and tail gas main pipe are closed, and then the vacuum is turned on, and chloromethyl ether is added under reduced pressure. After adding the specified amount of chloromethyl ether, the vacuum is turned off, the vent valve is opened, and the vacuum in the kettle is completely released, and then the vent valve is closed, and then the valve of the tail gas main pipe is opened. Finally, stirring is turned on, and the white ball is swollen in chloromethyl ether for 1 hour.

[0055] 4.2.2 After swelling, add 250 kg of zinc chloride into the chlorination kettle.

[0056] 4.2.3 After adding the catalyst zinc chloride, control the temperature to rise slowly to 40±1℃ within 1.5 hours and start timing. If the temperature rises too fast or is too high, use the amount of cooling water to adjust the temperature. Pay attention to frequent opening and closing and observation during operation. Control the chlorination temperature at 45±1℃ and the chlorination insulation time is 12 hours.

[0057] 4.2.4 After the holding time is up, take a sample to test the chlorine content. If the test result shows that the chlorine content is ≥ 17%, it is qualified. 4.2.5 After passing the test, turn on the cooling water to cool the temperature inside the kettle to below 30℃.

[0058] 4.2.6 Filter the mother liquor. After the mother liquor is filtered naturally for 1 hour, start the vacuum for 0.5 hour. When no mother liquor is filtered out, stop the vacuum.

[0059] 4.2.7 Extraction: After the mother liquor is filtered, add 1 ton of the first extraction liquid, stir for 1 hour, then filter out the first extraction liquid, then add 1 ton of the second extraction liquid, stir for 10 minutes and filter. The third extraction uses methylal solution and then discharges it into the amination kettle. The extract can be recycled after filtration.

[0060] 4.3 Amination reaction 4.3.1 Turn on the cooling water of the amination kettle to control the temperature of the materials in the kettle at 12~20℃.

[0061] 4.3.2 Neutralization, add liquid alkali to the reactor, the adding speed should strictly follow the principle of slow first and fast later, no more than 80kg in the first hour, no more than 120kg per hour thereafter, when the pH value reaches 8, stop adding and start stirring for 1 hour, then measure the pH of the bottom liquid again, it must reach pH 8 stably, otherwise continue to add liquid alkali. After neutralization, take a small amount of resin particles and observe whether there are broken balls under a microscope.

[0062] 4.3.3 Add 700~800kg of amination mother liquor and re-determine the pH value in the kettle to ensure that there is no change.

[0063] 4.3.4 Trimethylamine was added dropwise. The speed of addition should strictly follow the principle of slow first and fast later. The first hour was about 120 kg, the second hour was about 180 kg, and the third hour was about 250 kg. The speed of addition should be gradually increased. The specific amount of addition should be 1500 kg. If the pressure is too high during the addition process, the speed of addition should be slowed down or the addition should be stopped. The reaction temperature should be controlled not higher than 32°C during the addition process.

[0064] 4.3.5 After the addition is completed, continue to keep warm for 3 hours and control the temperature at 31±1℃.

[0065] 4.3.6 After the insulation is completed, take samples for testing. The residual amine should be ≤1% and the exchange volume should be ≥3.5mmoL / g. If the residual amine is too low, trimethylamine can be added as appropriate. If it is too high, continue to incubate for 1 hour and then test again.

[0066] 4.3.7 After the data is qualified, turn on the cooling water to reduce the temperature in the kettle to below 30℃, and add hydrochloric acid solution to the kettle for 2 hours to acidify the resin. The dropping speed also follows the principle of slow first and then fast. The temperature in the kettle is controlled below 30℃, and the end point pH value after the transformation is controlled at 3~4. And stabilize for 1 hour to ensure that the pH is stable.

[0067] 4.3.8 Pump the mother liquor into the corresponding storage tank, put the material into the washing bucket, start the material washing operation, wash the resin in eight levels until it is washed to neutrality, pump the material into the packager with tap water and take samples to test the finished product data.

[0068] 4.3.9 Release the materials and package them to obtain the finished products.

[0069] In a second aspect, the present invention provides a computer system comprising: a memory and a processor that are communicatively connected, and a computer program stored in the memory and capable of running on the processor, wherein the processor executes the above-mentioned method for preparing a gel-type anion exchange resin when running the computer program.

[0070] Each embodiment in this specification is described in a progressive manner, and the same or similar parts between the embodiments can be referred to each other, and each embodiment focuses on the differences from other embodiments. In particular, for the device, equipment, and non-volatile computer storage medium embodiments, since they are basically similar to the method embodiments, the description is relatively simple, and the relevant parts can be referred to the partial description of the method embodiment.

[0071] The above is a description of a specific embodiment of the specification. Other embodiments are within the scope of the appended claims. In some cases, the actions or steps recorded in the claims can be performed in an order different from that in the embodiments and still achieve the desired results. In addition, the processes depicted in the drawings do not necessarily require the specific order or continuous order shown to achieve the desired results. In some embodiments, multitasking and parallel processing are also possible or may be advantageous.

[0072] The above description is only one or more embodiments of this specification and is not intended to limit this specification. For those skilled in the art, one or more embodiments of this specification may have various changes and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of one or more embodiments of this specification shall be included in the scope of the claims of this specification.

Claims

1. A method for preparing a gel-type anion exchange resin, characterized in that: Specifically include: Put the white ball into the reaction kettle, open the vacuum, add a specified amount of chloromethyl ether under reduced pressure, swell the white ball in the chloromethyl ether, add zinc chloride, and heat it according to the preset strategy. After reaching the target temperature, keep it warm until the chlorine content test result is qualified, cool the temperature in the kettle, filter the mother liquor, vacuum control the reaction kettle, extract it according to the preset strategy, and then discharge it into the amination kettle; After cooling the amination kettle with the target temperature as the control target, neutralizing the amination kettle with liquid alkali according to the preset neutralization strategy, adding the amination mother liquor to determine that the pH value does not change, and then dripping trimethylamine according to the preset dripping strategy; After the addition is completed, the temperature is kept at the preset temperature until the end of the insulation. After the residual amine and exchange capacity data are sampled and tested and qualified, the cooling water is turned on, and the resin is acidified and transformed according to the preset acidification strategy. After the pH value reaches the target and remains unchanged, the material is placed in the washing barrel and the washing operation is started. After washing to neutrality, the finished product data is sampled and tested and the material is discharged to obtain the finished product.

2. The method for preparing a gel-type anion exchange resin according to claim 1, wherein: Add a specified amount of chloromethyl ether under reduced pressure, specifically including: Close the cooler of the reactor and the valve of the tail gas main pipe, then open the vacuum, and add chloromethyl ether under reduced pressure; After adding the specified amount of chloromethyl ether, turn off the vacuum, open the vent valve, release the vacuum in the kettle and then close the vent valve, then open the valve of the tail gas main pipe, and finally start stirring to allow the white ball to swell in chloromethyl ether for 1 hour.

3. The method for preparing a gel-type anion exchange resin according to claim 1, characterized in that: The temperature is raised according to the preset strategy, including: After adding the catalyst zinc chloride, control the temperature to slowly rise to 40 ± 1°C within 1.5 hours and start timing. If the heating rate does not meet the requirements, use the amount of cooling water to adjust the temperature until the chlorination temperature is reached; The chlorination temperature was controlled at 45±1℃ and the chlorination holding time was 12 hours.

4. The method for preparing a gel-type anion exchange resin according to claim 1, wherein: The extraction process is carried out according to the preset strategy, including: Pour in 1 ton of the first extraction liquid, stir for 1 hour, and then filter out the first extraction liquid; Then add 1 ton of the second extract, stir for 10 minutes and then filter; The third extraction uses methylal solution, which is then discharged into the amination kettle.

5. The method for preparing a gel-type anion exchange resin according to claim 1, wherein: The amination kettle is neutralized according to the preset neutralization strategy and liquid alkali, specifically including: Add liquid alkali to the reactor dropwise. The dropping speed should strictly follow the principle of slow first and fast later. The first hour should not be more than 80 kg, and the following hour should not be more than 120 kg. When the pH value reaches 8, stop dropping and start stirring for 1 hour. Measure the pH value of the bottom liquid again. It must stably reach pH 8, otherwise continue to add liquid alkali.

6. The method for preparing a gel-type anion exchange resin according to claim 1, wherein: Trimethylamine is added dropwise according to a preset addition strategy, specifically including: The dripping speed should strictly follow the principle of slow first and then fast, 120kg in the first hour, 180kg in the second hour, 250kg in the third hour, and gradually increase the dripping speed; The specific amount of dropwise addition is 1500 kg. If the pressure in the amination reactor is not within the preset pressure range during the dropwise addition, the dropwise addition speed should be slowed down or suspended. The reaction temperature should be controlled not to be higher than 32° C. during the dropwise addition.

7. The method for preparing a gel-type anion exchange resin according to claim 1, characterized in that: The data of sampling and testing of residual amine and exchange capacity are qualified, including: The residual amine should be ≤1%, and the exchange volume should be ≥3.5mmoL / g. If the residual amine is too low, add trimethylamine. If it is too high, keep warm for 1 hour and then test again.

8. The method for preparing a gel-type anion exchange resin according to claim 1, wherein: The acidification transformation of the resin is carried out according to the preset acidification strategy, including: Turn on the cooling water to lower the temperature in the kettle to below 30°C, and add hydrochloric acid solution into the kettle for 2 hours to carry out acidification transformation of the resin. The dropping speed also follows the principle of slow first and then fast. The temperature in the kettle is controlled below 30°C. The end point pH value after transformation is controlled at 3~4, and it is stabilized for 1 hour to ensure that the pH remains stable.

9. The method for preparing a gel-type anion exchange resin according to claim 1, wherein: Carry out material washing operations, including: Put the material into the washing bucket and start the material washing operation. Wash the resin in eight levels until it is neutral. Then use tap water to pump the material into the packager and take samples to test the finished product data.

10. The method for preparing a gel-type anion exchange resin according to claim 3, characterized in that: It is judged that the heating rate does not meet the requirements, including: Determine the temperature data at different heating moments based on the analysis results of the temperature data at different heating moments; Based on the temperature data, the addition data of the catalyst zinc chloride and chloromethyl ether, determining the data similarity coefficients of the addition data and the temperature data with different historical heating treatment times; The similar processing times in the historical heating processing times are determined according to the data similarity coefficient, and whether the heating data meets the requirements is determined according to the temperature change data in the similar processing times.

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