CN112851835B - Device for preparing strong acid sodium resin - Google Patents

Device for preparing strong acid sodium resin Download PDF

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Publication number
CN112851835B
CN112851835B CN202110261256.8A CN202110261256A CN112851835B CN 112851835 B CN112851835 B CN 112851835B CN 202110261256 A CN202110261256 A CN 202110261256A CN 112851835 B CN112851835 B CN 112851835B
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resin
transformation
solution tank
tank
sodium
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CN112851835A (en
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何艳红
周焱
王勇
伊成龙
李霄玺
景旭斌
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Shanghai Nuclear Engineering Research and Design Institute Co Ltd
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Shanghai Nuclear Engineering Research and Design Institute Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00Processes of polymerisation
    • C08F2/01Processes of polymerisation characterised by special features of the polymerisation apparatus used
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F8/00Chemical modification by after-treatment
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G85/00General processes for preparing compounds provided for in this subclass
    • C08G85/004Modification of polymers by chemical after-treatment

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Treatment Of Water By Ion Exchange (AREA)

Abstract

The invention aims to disclose a device for preparing strong acid sodium type resin, which comprises a transformation solution tank, a resin preparation bed, a recovery solution tank and a resin collecting tank, wherein the output end of the transformation solution tank is respectively connected with the water inlet of the resin preparation bed and the input end of the recovery solution tank through a pump; compared with the prior art, the sodium type group transformation is carried out on the strong acid cation resin by the NaOH solution which can rapidly carry out the neutralization ion exchange reaction, the reaction is thorough, the sodium type transformation rate of more than 99.9% is ensured, the reaction speed is high, the resin is not damaged, the resin preparation efficiency and the resin safety are improved, and the aim of the invention is realized.

Description

Device for preparing strong acid sodium resin
Technical Field
The invention relates to a device for preparing resin, in particular to a device for preparing strong acid sodium type resin, which is suitable for nuclear power plants, thermal power plants, frequency converter enterprises and the like.
Background
The water quality of the cold water system in the power plant and the insulation performance of the generator are closely related to the corrosion rate of the copper wire rod, and the operation safety of the unit is directly affected by the quality of water quality control. The national standard has strict requirements on the quality of the internal cooling water, mainly comprises a pH value, conductivity and copper content, wherein the pH value of the stator cooling water is 8.0-9.0, the conductivity is less than or equal to 2.0 mu s/cm (25 ℃) in the GB/T1039-2016 internal cooling water treatment guide rule of the generator, the copper ion content is less than or equal to 20 mu g/L, and the recommended value in the national standard is a water chemical control index which must be met, but in actual operation, the optimal water chemical control range is that the pH value is 8.0-8.5, the conductivity is less than or equal to 1.0 mu s/cm (25 ℃) and the copper ion content is less than or equal to 5 mu g/L in order to reduce the loop corrosion to the minimum extent. The adoption of the sodium resin bed to achieve the above-mentioned aim is the currently preferred process in the industry, the process is simple to operate and maintain, safe and reliable to operate, and the chemical regulation of the loop water can be achieved under the background of no impurity.
The internal cooling water purification loop adopts a sodium resin bed to exchange trace cations (such as impurity cations of copper, ammonia, iron and the like and ionized hydrogen ions of water) in the loop by sodium type cation resin, and release sodium ions to combine with trace hydroxide ions in water, so that trace NaOH is contained in the effluent, thereby ensuring that the requirement of the conductivity of the loop water is met and the requirement of the pH value is also met.
Typical ion exchange reaction equations are as follows: RNa+Cu 2+ /H + ----R 2 Cu+Na + OH -
The most core product of the process is sodium type positive resin, and the service life, the water outlet stability and the capacity of regulating the pH value and the conductivity of the loop water of the resin are directly determined by the integrity, the sodium type transformation rate and the transformation group distribution uniformity of the sodium type positive resin after transformation, so that how to ensure the transformation rate and the transformation group distribution uniformity of the sodium type positive resin has important significance for an internal cooling water alkalinity regulation market. Meanwhile, the sodium resin transformation process needs to consume a large amount of chemicals such as salt or alkali, and if a proper preparation device is not matched, the problems of resource waste, transformation cost increase, environmental pollution and the like can be caused.
The transformation device is also one of key factors for guaranteeing the integrity, the sodium transformation rate and the distribution uniformity of transformation groups after the sodium resin is transformed.
Therefore, there is a particular need for an apparatus for preparing a strongly acidic sodium type resin to solve the above existing problems.
Disclosure of Invention
The invention aims to provide a device for preparing strong acid sodium resin, which aims at the defects of the prior art, realizes automatic control of a transformation process based on the reaction rule and process of strong acid positive resin and sodium hydroxide, improves the resource utilization rate, ensures that each batch of products obtains sodium transformation rate of more than 99.9%, does not cause resin to be broken or crack in the transformation process, realizes no waste of transformation medicament, ensures that water discharged in all transformation processes does not contain acid and alkali, has low salt concentration, realizes zero discharge of waste liquid, and realizes resource optimization and environmental friendliness.
The technical problems solved by the invention can be realized by adopting the following technical scheme:
the device for preparing the strong acid sodium resin is characterized by comprising a transformation solution tank, a resin preparation bed, a recovery solution tank and a resin collecting tank, wherein the output end of the transformation solution tank is respectively connected with the water inlet of the resin preparation bed and the input end of the recovery solution tank through pumps, the output end of the recovery solution tank is connected with the input end of the transformation solution tank through pumps, the water outlet of the resin preparation bed is connected with the transformation solution tank, the output end of the resin preparation bed is connected with the resin collecting tank, and the water inlet and the water outlet of the resin preparation bed are respectively provided with an online pH meter and an online conductivity meter.
In one embodiment of the invention, the transformation solution tank is used for filling 1-8% NaOH solution, the volume of the transformation solution tank is 1-2 times of that of the resin to be transformed, and a stirring paddle for preparing the NaOH solution is arranged in the transformation solution tank.
In one embodiment of the invention, the bottom of the resin preparation bed is provided with a water cap, and the water outlet at the top of the resin preparation bed is provided with a resin interception filter screen for sodium resin transformation and cleaning.
In one embodiment of the invention, the recovery solution tank is used for collecting the NaOH solution which is not completely reacted in the later stage of sodium resin preparation, the volume of the recovery solution tank is 1-2 times of that of the transformation resin, and the stirring paddle is arranged in the recovery solution tank.
In one embodiment of the invention, the bottom of the resin collection tank is provided with a resin interception filter screen and a vacuum pump for quickly and efficiently removing free moisture after the sodium resin preparation is finished and before packaging.
Compared with the prior art, the device for preparing the strong acid sodium type resin can quickly perform sodium type group transformation on the strong acid positive resin by using the NaOH solution subjected to the neutralization ion exchange reaction, and the reaction is thorough, so that the sodium type transformation rate of the final product which is more than 99.9% is ensured, the reaction speed is high, and the resin preparation efficiency is improved; the transformation is realized by adopting the steps of the transformation chemical concentration from low to high and the resin reaction, and the high-concentration alkali liquor is contacted after the group reaction exceeds 50%, so that the severe volume shrinkage and reaction heat release caused by the rapid neutralization ion exchange reaction of the resin under the condition of the excessive alkali concentration in the initial stage are avoided, and the resin is prevented from being broken and generating cracks, thereby further avoiding the problems of resin loss, further post-treatment, high pressure difference in operation, water cap blockage, loop corrosion caused by leakage and the like in the transformation process, and realizing the purpose of the invention.
The features of the present invention will be apparent from the following detailed description of the preferred embodiments, taken in conjunction with the accompanying drawings.
Drawings
FIG. 1 is a schematic diagram of the apparatus for producing a strongly acidic sodium-type resin according to the present invention.
Detailed Description
The invention is further described with reference to the following detailed drawings in order to make the technical means, the creation characteristics, the achievement of the purpose and the effect of the implementation of the invention easy to understand.
Examples
As shown in fig. 1, the device for preparing the strong acid sodium resin comprises a transformation solution tank 1, a resin preparation bed 2, a recovery solution tank 3 and a resin collecting tank 4, wherein the output end of the transformation solution tank 1 is respectively connected with the water inlet of the resin preparation bed 2 and the input end of the recovery solution tank 3 through a pump 5, the output end of the recovery solution tank 3 is connected with the input end of the transformation solution tank 1 through the pump 5, the water outlet of the resin preparation bed 2 is connected with the transformation solution tank 1, the output end of the resin preparation bed 2 is connected with the resin collecting tank 4, and an online pH meter 6 and an online conductivity meter 7 are respectively arranged at the water inlet and the water outlet of the resin preparation bed 2.
In this embodiment, the transformation solution tank 1 is used for filling 1-8% NaOH solution, the volume of the transformation solution tank 1 is 1-2 times of the resin to be transformed, and a stirring paddle for NaOH solution configuration is disposed inside the transformation solution tank 1.
In this embodiment, the bottom of the resin preparation bed 2 is provided with a water cap, and the water outlet at the top of the resin preparation bed 2 is provided with a resin interception screen for sodium resin transformation and cleaning.
In this embodiment, the recovery solution tank 3 is used for collecting the NaOH solution which is not completely reacted in the later stage of the sodium resin preparation, the volume of the recovery solution tank 3 is 1-2 times of the volume of the transformation resin, and the inside of the recovery solution tank 3 is provided with a stirring paddle.
In this embodiment, the bottom of the resin collection tank 4 is provided with a resin-trapping filter screen and a vacuum pump for rapidly and efficiently removing free moisture before packaging after the sodium resin preparation is completed.
The working process of the device for preparing the strong acid sodium type resin is as follows:
when sodium type transformation preparation is carried out on a batch of strong acid positive resin, firstly, naOH solution with the target concentration of 1-3% and the volume of 1-2 times of the volume of the prepared resin is prepared by adding sodium hydroxide into a transformation solution tank 1, after 2 times of cyclic reaction, naOH solution with the concentration of 4-8% and the volume of 1-2 times of the resin is prepared into the transformation solution tank 1, whether the part of solution is recycled into a recycling solution tank 3 is determined according to the change trend of the reaction pH and the conductivity of the solution, whether the part of solution is discharged or fed into the recycling solution tank 3 is fed back through signals, and meanwhile, the reaction end point is also determined. And after the reaction of the sodium type group is finished, eluting the resin in the resin preparation bed 2 by using ultrapure water at a speed of 2-10BV/h, and determining an eluting end point according to the conductivity and the pH value of the effluent. And finally, hydraulically conveying the sodium-transformed resin in the resin preparation bed 2 to a resin collecting tank 4 by adopting ultrapure water, starting a vacuum suction pump to remove residual free water in the resin after the dewatering is finished, and finally, filling the resin into a packaging bag or a packaging barrel.
The device for preparing the strong acid sodium type resin solves the following problems:
1. the method solves the problems that the traditional sodium resin preparation adopts NaCl solution to easily cause ion exchange reverse reaction, so that the reaction speed is slow and the transformation is not thorough, and solves the problems that the transformation reaction speed is too fast, the resin is easy to shrink rapidly and the rapid heat release is easy to cause resin breakage and crack generation in the transformation process due to the adoption of high-concentration alkali solution;
2. the problems that the reaction speed is low, and the sodium group distribution of the resin particles is uneven in the traditional static soaking preparation mode are solved, and the problem that the transformation rate of the upper resin is superior to that of the lower resin in the traditional concurrent dynamic transformation mode, so that the transformation is uneven are solved;
3. solves the problems that the traditional preparation process is not easy to monitor the reaction end point, a great amount of salt or alkali waste liquid is generated in the transformation process, and the like.
4. Solves the problems that the stability of the resin during the preservation period is affected by partial free water residue caused by the traditional gravity drainage and the problem that the partial process needs to adopt a complex centrifugal process to remove the free water.
The device for preparing the strong acid sodium type resin has the following characteristics:
1. NaOH solution capable of rapidly carrying out neutralization ion exchange reaction carries out sodium group transformation aiming at strong acid cation resin, and the reaction is thorough so as to ensure the sodium transformation rate of the final product of more than 99.9%, and the reaction speed is high so as to improve the resin preparation efficiency; the transformation is realized by adopting the steps of the transformation chemical concentration from low to high and the resin reaction, and the high-concentration alkali liquor is contacted after the group reaction exceeds 50%, so that the problems of severe volume shrinkage and reaction heat release caused by the rapid neutralization ion exchange reaction of the resin under the condition of the excessive alkali concentration in the initial stage, resin breakage and crack generation are avoided, and further the problems of resin loss, further post-treatment, high pressure difference in operation, water cap blockage, loop leakage, corrosion and the like in the transformation process are avoided.
2. The mode that batch transfer solution passes through the resin bed from bottom to top is adopted, the resin transfer process is always in an up-down suspension state, the resin is uniformly and fully contacted with the transfer solution with the same concentration, the exchange of the resin and the solution is accelerated, the transfer uniformity among resin particles is ensured, and the stability of the water quality of the on-site running effluent of the sodium resin is finally ensured.
3. The method is characterized in that an on-line pH value and conductivity are arranged at an inlet and an outlet of a resin preparation bed so as to timely monitor the configuration condition of a transformation solution and the transformation reaction process, the automatic calculation of the chemical addition amount, the solution recovery reaction point and the final transformation end point can be realized through the relationship between the pH value and the concentration of NaOH solution, the transformation stability among batches is controlled, the unreacted NaOH solution is recovered while the high-concentration excessive transformation is ensured, the chemical consumption is saved, the neutral low-conductivity water and the final leaching water generated by the intermediate reaction are recovered to an ultrapure water preparation raw water tank, the zero discharge of wastewater in the transformation process is realized, and the economy and the environmental friendliness are improved;
4. through designing a resin receiving tank with a filter screen and a vacuum suction pump, most of free moisture of resin can be removed rapidly through gravity drainage, then residual free water which is difficult to remove at the bottom is removed through hollow suction, the residual free water in the resin to be packaged is ensured to be less than 1%, the quality guarantee period of the resin is prolonged, the resin bed is ensured to be started rapidly after filling, and the problem of loop water quality caused by organic acid release due to excessive free water residue is avoided.
The foregoing has shown and described the basic principles and main features of the present invention and the advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the foregoing embodiments, which have been described in the foregoing embodiments and description merely illustrates the principles of the invention, and that various changes and modifications may be effected therein without departing from the spirit and scope of the invention as defined in the appended claims and their equivalents.

Claims (4)

1. The device for preparing the strong acid sodium resin is characterized by comprising a transformation solution tank, a resin preparation bed, a recovery solution tank and a resin collecting tank, wherein the output end of the transformation solution tank is respectively connected with the water inlet of the resin preparation bed and the input end of the recovery solution tank through a pump, the output end of the recovery solution tank is connected with the input end of the transformation solution tank through a pump, the water outlet of the resin preparation bed is connected with the transformation solution tank, the output end of the resin preparation bed is connected with the resin collecting tank, and an online pH meter and an online conductivity meter are respectively arranged at the water inlet and the water outlet of the resin preparation bed; the bottom of the resin collecting tank is provided with a resin interception filter screen and a vacuum suction pump, and the resin collecting tank is used for rapidly and efficiently removing free moisture before packaging after sodium resin preparation is finished.
2. The apparatus for preparing a strongly acidic sodium type resin according to claim 1, wherein the transformation solution tank is used for filling 1-8% of NaOH solution, the volume of the transformation solution tank is 1-2 times of that of the resin to be transformed, and a stirring paddle for configuring the NaOH solution is arranged inside the transformation solution tank.
3. The apparatus for preparing a strong acid sodium type resin as set forth in claim 1, wherein the bottom of the resin preparation bed is provided with a water cap or a retention screen, and the water outlet at the top of the resin preparation bed is provided with a resin retention screen for transformation and washing of the sodium type resin.
4. The apparatus for preparing a strongly acidic sodium-type resin according to claim 1, wherein the recovery solution tank is used for collecting an unreacted NaOH solution in the late stage of the sodium-type resin preparation, the volume of the recovery solution tank is 1 to 2 times the volume of the converted resin, and a stirring paddle is disposed inside the recovery solution tank.
CN202110261256.8A 2021-03-10 2021-03-10 Device for preparing strong acid sodium resin Active CN112851835B (en)

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Application Number Priority Date Filing Date Title
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CN112851835B true CN112851835B (en) 2023-07-25

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Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1896009B (en) * 2006-06-09 2010-12-22 江西省电力科学研究院 Alkalescent water-quality treatment and treating system for double-internal water-cooled generator
JP2010502431A (en) * 2006-09-07 2010-01-28 ダウ グローバル テクノロジーズ インコーポレイティド Strong acid cation exchange resin
CN204454694U (en) * 2015-02-02 2015-07-08 神华神东电力有限责任公司技术研究院 A kind of for 1000MW set generator internal cooling water device
CN204752272U (en) * 2015-05-07 2015-11-11 长安益阳发电有限公司 Large -scale generator inner cooling water complete set processing apparatus
CN109201124A (en) * 2017-06-30 2019-01-15 上海轻工业研究所有限公司 Method is monitored and controlled in the transition of ion exchange resin
CN109174211A (en) * 2017-06-30 2019-01-11 上海轻工业研究所有限公司 Device is monitored and controlled in the transition of ion exchange resin
CN211733919U (en) * 2019-12-30 2020-10-23 上海核工程研究设计院有限公司 Be used for interior cold water alkalization governing system of power plant
CN111943318A (en) * 2020-08-28 2020-11-17 哈尔滨安泰利达科技开发有限公司 Special resin for generator inner cooling water and preparation method thereof

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