CN1047269A - Ion exchange resin specialty regeneration system rapidly and product - Google Patents

Ion exchange resin specialty regeneration system rapidly and product Download PDF

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Publication number
CN1047269A
CN1047269A CN90101481A CN90101481A CN1047269A CN 1047269 A CN1047269 A CN 1047269A CN 90101481 A CN90101481 A CN 90101481A CN 90101481 A CN90101481 A CN 90101481A CN 1047269 A CN1047269 A CN 1047269A
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resin
regeneration
product
water
specialty
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CN90101481A
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仝静亭
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Beijing Semiconductor Devices Factory No12
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Beijing Semiconductor Devices Factory No12
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Abstract

The present invention relates to a kind of professional regeneration system rapidly to ion exchange resin (hereinafter to be referred as resin) manipulation of regeneration and products thereof.This system is become by six groups of subsystems such as pure water preparation, regenerated liquid preparation, resin layering, regeneration, mixing and treating waste liquid.Constitute a complete production system, be suitable in enormous quantities, continuity production, help realizing specialized production, the product of resin specialty regeneration system rapidly is directly to use the type resin, can make the user break away from regenerative operation, utilize existing equipment to obtain the technology innovation effect, the present invention provides favourable condition for producing 18M Ω cm (25 ℃) ultrapure water.

Description

Ion exchange resin specialty regeneration system rapidly and product
The present invention relates to ion exchange resin<hereinafter to be referred as resin a kind of professional regeneration system rapidly of manipulation of regeneration and products thereof.Resin regeneration is the essential condition that resin is used, and wherein strong acid, strong base resin are widely used, and technological condition of regeneration requires high, is emphasis of the present invention.
The current domestic resin regeneration method that generally adopts can reduce two classes substantially:
1, static regeneration method: be mainly used in the regeneration that small-sized exchange column and terminal are mixed bed.Pour exhausted resin into big basin, add acid, add the alkali immersion, artificial flood is washed, and labor condition is abominable, contaminate environment, and regeneration effect is poor.
2, dynamic method of reproduction: in ion exchange column, carry out.The regenerated liquid for preparing is sent into exchange columns such as the sun bed of inefficacy, cloudy bed and mixed bed, discharged behind the resin of flowing through, finish regeneration.Wash then.Be uninterrupted production, exchange columns such as positive and negative, mixed bed all are provided with two components parts for assembly of a machine, an operation, a regeneration is used alternatingly, and forms " economy of double-track general layout.The actifier column because the work post is held concurrently causes disadvantageous effect to technological condition of regeneration, forms and drops into high, the low disadvantage of producing effects.
More than two kinds of renovation process continued to use 30 at home surplus year, the more and more incompatible development of producing of the regeneration that disperse to fall behind.It is reported, the resin regeneration method in the imported technology is similar to domestic dynamic method, only remedies defective workmanship to improve regenerated liquid purity and to increase consumption, and is less economical.
Purpose of the present invention is the problem that exists in the current resin regeneration, in conjunction with the Future Development direction, to optimize processing condition, improve regeneration and consume, reduce regeneration and consume, the minimizing environmental pollution is a target, proposes a kind of resin specialty regeneration system rapidly, promotes that resin regeneration develops to specialized direction.In addition, the present invention directly provides prerequisite with the type resin for developing, and helps improving the resin application level, and is development 18M Ω, cm<25 ℃〉ultrapure water favourable condition is provided.
The resin specialty regeneration system rapidly that the present invention proposes is to be become by pure water preparation, regenerated liquid preparation, resin layering, 6 groups of subsystems such as the series connection of resin multicolumn regeneration, mixed with resin and treating waste liquid.Constitute a complete production system.<see accompanying drawing one〉existing that the effect and the structure division of each subsystem is as follows:<see accompanying drawing two 〉.
1, pure water preparation subsystem:<1-1~1-9〉be the important component part of resin specialty regeneration system rapidly, its effect is to provide pure water for resin regeneration technique, adopt multiple bed<1-2,1-3 〉-mixed bed<1-6~1-7〉technology, prime is established raw water filtration device<1-1 〉, is imported and exported tensimeter is housed.Establish intermediate water tank<1-4〉behind the multiple bed, supply water for mixing bed by water pump<1-5 〉, water outlet is delivered to through under meter, tensimeter and hydraulic pipe-line and is respectively used water spot.And realize dynamic circulation through water return pipeline, by circling water flow rate, pressure-controlling is adjustable, and the homogeneous tube net send the regimen condition, backwater flow to pure water case<1-8 〉.Available in case of necessity water pump<1-9〉is delivered to each with the water of pure water case or intermediate water tank and is used water spot, is applicable to the pre-treatment and the situation not high to water quality requirement of new resin.The ion exchange column of this subsystem all adopts the straight type resin of using, and positive and negative, mixed bed are all established one, must not continue to use " economy of double-track general layout, work post are not held concurrently and are regenerated, and the resin inefficacy can in time be changed, save time conveniently, and be pollution-free source water station.
2, regenerated liquid preparation subsystem:<2-1~2-8〉provides regenerated liquid for layering post and actifier column.Adopt header tank<2-1,2-2〉or negative-pressure adsorption pipe<2-3,2-4 〉, make raw material acid, alkali be diluted to predetermined concentration, store in regenerated liquid poor<2-5,2-6 〉.By sour pump<2-7〉alkali pump<2-8〉regenerated liquid being delivered to each need use a little.On conveying regenerated liquid pipeline, be provided with connection line<A〉and cut-out line<B, C〉and can adjust regenerated liquid conveying scope, increase mobility, to satisfy the production needs.
3, resin layering subsystem:<3-1〉be used to lose efficacy layering of hybrid resin, for dividing column regeneration, prepares the positive and negative resin.Be provided with the water-feeding ﹠ drainaging pipeline of layering post<3-1 〉, alkaline regeneration solution and water.
4, resin multicolumn series connection regeneration subsystem<4-1~4-8 〉: be the core of resin specialty regeneration system rapidly, the positive and negative resin respectively is one group, and every group of actifier column by proper amt is connected into a closed circuit circulatory system in proper order, is suitable for continuity production.For the reduced representation accompanying drawing is drawn 4 post series connection group structures, there are positive resin series connection actifier column group<4-1~4-4〉and negative resin series connection actifier column group<4-5~4-8〉can suitably increase columns in series quantity and group number greatly as turnout, desirable arbitrary post is as first post each post UNICOM successively thereafter during use, also sectional series connection or use separately are to adapt to arts demand.Little or only solve our unit regeneration needs as turnout, also can reduce the columns in series number, as the series connection of 2~3 posts, or only establish one group, the positive and negative resin is regenerated in batches and double layering, mixing also can obtain regeneration effect preferably.
5, mixed with resin subsystem<5-1~5-2 〉: be used for the positive and negative resin and realize uniform mixing in proportion.Be provided with mixing column<5-1 〉, be furnished with, nitrogen<5-2〉is fed the mixing column bottom, stir and finish mixing by flexible pipe and union to, discharge pipe line.
6, treating waste liquid subsystem<6-1~6-3 〉: this system is set by environmental requirement.Salkali waste groove<6-1 〉, spent acid groove<6-2〉are housed to be connected by pipeline and layering post, actifier column discharge outlet.Acid, alkali wasteliquid are collected into waste liquid tank, import neutralizing well<6-3〉again and regulate pH value, qualified discharge.
Positively effect of the present invention at first has been to propose a complete orderly resin specialty, and regeneration system rapidly can replace the static regeneration method of original backwardness, also is better than dynamic single-column method of reproduction.Overcome defective workmanship and the high investment that has renovation process now and be difficult to avoid, the disadvantage of hanging down output.Especially mix bed regeneration, existing method is the collection layering, regenerates, is mixed in the same post and carry out, and positive and negative regeneration of resin liquid failure source each other, be difficult to control, not only cause near the resin of branch aspect to lose efficacy, and cause whole exchange capacity decay, regeneration effect is poorer.The resin specialty regeneration system rapidly that the present invention proposes, according to the design of resin regeneration technique characteristics, be not subjected to other constraints, help optimizing processing condition, the disadvantage of existing reclaiming process can be reduced and avoid, and production increases with quality up and cost of production down effect can be obtained.As follows to the advantage division of resin specialty regeneration system rapidly below:
1, multicolumn series connection effect makes exhausted resin be able to abundant regeneration, and regenerated liquid is fully utilized: resin regeneration is a chemical reaction process, makes strong acid, strong base resin be able to regenerated H +, and OH -The avidity of ion and resin is lower than foreign ion<as Fe +++, Ca ++, Mg ++, Na +And SO -- 4, CO -- 3, HCO - 3, Ce -Deng〉with the avidity of resin, so permutizer condition is relatively more difficult.Static immersing regeneration easily produces reversed reaction, so regeneration effect is poor.Though dynamically method of reproduction can be avoided reversed reaction, desires to make reaction conditions abundant, the regeneration effect that obtains, often need regenerated liquid than high several times even tens times of theoretical consumption, this regenerates to existing single-column and is that very uneconomic, excessive regenerated liquid is first-class and mistake makes enterprise be difficult to bear.Current resin user's regenerated liquid consumption is mostly far below above-mentioned requirements, and the regenerated resin has only the part exchange capacity to be recovered like this, though energy usefulness, exchange capacity is poor, and life cycle is short, and the meeting premature failure forms the vicious cycle of frequent regeneration.Cause supplies consumption big, the hydroelectric resources waste is serious, increases labour intensity, the weighting ring environment pollution.The multicolumn series connection regeneration that the present invention proposes can overcome the above problems preferably.The placed in-line effect of multicolumn is exactly that excessive regenerated liquid is fully utilized.Flow through behind the first post when making resin be able to the excessive regenerated liquid of abundant regenerated, order flows into columns in series thereafter, and the regenerated liquid that must make full use of can not proceeded regeneration to exhausted resin in these columnss in series, makes it obtain in various degree exchange capacity.When first column regeneration rate reaches 90%, the regeneration rate Yue Keda 65% of secondary post, more about thereafter 30% etc.When secondary post is done first post, desire to make its regeneration rate to reach 90%.About 60% of a required regenerated liquid quite former first post, by that analogy, each post only needs 60% of former first column regeneration liquid that resin is fully regenerated later on.In addition, multicolumn series connection regeneration can realize continuous production, finished a post regeneration of resin in 1~2 hour, and existing renovation process is finished a post regeneration of resin in about 1~2 day.The production increases with quality up and cost of production down net effect of more than obtaining is exactly a multicolumn series connection effect.
2, the pure water preparation subsystem can be resin regeneration technique pure water is provided, and helps the raising of exchange capacity: resin is after acid, alkali regeneration, and the acid, the alkali that also need water to adhere to wash down, so the quality of water quality has material impact to regeneration effect.Existing reclaiming process due to limited conditions, big polyphyly is with the prime water of water manufacturing system, water quality is relatively poor, have in addition wash with tap water.A large amount of foreign ions will be replaced the H and the OH ion of resins exchange gene in the water, cause the reduction of exchange capacity.Make resin be in disadvantageous weak tendency working order.The present invention is provided with the pure water preparation system, by multiple bed-mixed bed process, can produce the very high water of purity, is used for reclaiming process, will reduce the loss of exchange capacity greatly, obtains good regeneration effect.In addition, the water loss of flushing resin is quite big, is about 1: 20, i.e. 1m 3Resin needs 20m approximately 3Wash-down water.As adopting multicolumn series connection effect, the water that the first post acid of flushing, alkali content are reduced gradually seals in secondary property, and it is made full use of, than the water loss reduction about 35% of single-column flushing.This will reduce the consumption of water resources.In addition, the pure water preparation system that the present invention proposes has adopted novel texture, directly uses the type resin owing to adopt, broken through existing " traditional pattern of economy of double-track, promptly to positive and negative, mix a bed plasma switching equipment, two components parts for assembly of a machine must be set; but respectively establish one; resin lost efficacy and can in time change, the regeneration of not holding concurrently of work post needn't be set up regeneration liquid dispensing device and transfer line; simplified system; made things convenient for operation, has eliminated acid, alkali pollution source, and investment and take up an area of and can reduce about 40%.
3, the application of layering post, mixing column can be avoided the existing bed regenerated disadvantage of mixing: existingly mix bed regeneration and carry out mostly, layering, positive and negative resin regeneration and be blended in the same post in the work post.Because positive and negative regeneration of resin liquid, failure source is difficult to avoid cause mutually and lost efficacy or decay each other, because flushing terminal point controlled deviation is big, fails to wash down and promptly does mixing again, further reduces exchange capacity, still needs big water gaging flushing after the mixing, just can come into operation.Because processing condition are unfavorable, the tooling incompatibility causes mixed bed reproducer many, the disadvantage of weak effect.Adopt the present invention can avoid above drawback, can be to the inefficacy hybrid resin earlier in the layering of layering post, then with sun, negative resin is respectively charged into multicolumn series connection actifier column, using multicolumn series connection effect makes resin obtain good regeneration, divide the post flushing to be convenient to control flushing terminal point, make sun, negative resin mixes under neutrallty condition, use resin blend sub system, contact acid not, alkali can keep good processing condition, owing to there is professional tooling to do assurance, mixed resin can obtain good effect, as is used to produce pure water, can use the water resistance value and reach 16~18M Ω, cm<25 ℃ 〉.
4, help improving working conditions, reduce environmental pollution: resin regeneration need be used strong acid, highly basic, strong, poisonous, the health risk of corrodibility, contaminate environment.Existing static big basin infusion method is mainly by manual operation, and condition is simple and crude, and harm is serious.Though existing dynamically regeneration has improvement than stationary method.But how acid, alkali preparation are by artificial, and the shortage of condition difference is ventilated and treating waste liquid, and the present invention has done technical finesse in this respect, header tank or negative-pressure adsorption can reduce the disperse of acid, alkali aerosol, waste liquid is discharged to be provided with and is collected pipeline importing waste liquid tank, regulates pH value, qualified discharge at neutralizing well.Can reduce the pollution of strong acid, highly basic to environment as far as possible.
5, product of the present invention is directly to use the type resin, this is the processed goods of raw material type resin, function with direct use, after user's buying, need not carry out pre-treatment and regeneration transition, can thoroughly break away from heavy deleterious regenerative operation, work such as cancellation regeneration facility and acid, alkali buying, transportation, storage utilize existing equipment can obtain the technology innovation effect.Resin lost efficacy and can in time change, and just as changing oxygen cylinder, gas tank, promptly economy is convenient again, has also eliminated environmental pollution.The straight type resin of using can be divided into premium grade and general level two classes by the service requirements difference again, to satisfy the needs of different user simultaneously corresponding to raw material type resin formation strong acid, highly basic, weak acid, weak base type series product.The establishment of resin specialty regeneration system rapidly and straight Application and Development with the type resin, for a change current dispersion, the regeneration that falls behind open up a new way, and meet get twice the result with half the effort principle and professional development direction, have tangible economic benefit and social benefit.
6, help producing the ultrapure water of 18M Ω, Cm<25 ℃ 〉: ultrapure water is one of base mateiral of electronic industry large-scale integrated circuit production.The present domestic research of technique stage that still is in.Some emphasis research institutes rely on from states such as U.S., day, West Europe and introduce, and cost dearly.Resin is an important means of producing ultrapure water, because existing resin regeneration is backward in technique, regeneration effect is poor, and exchange capacity is low, easily causes ion to leak in use, influences the water quality refining effect, is difficult to produce ultrapure water.Adopt resin specialty regeneration system rapidly, can make resin be able to abundant regeneration, obtain good regeneration effect; exchange capacity is strong, and protective layer is reliable, can prevent effectively that ion from leaking; make the water quality resistance reach 18M Ω, Cm<25 ℃ 〉, provide favourable condition for producing ultrapure water.
About realizing best way of the present invention: at first be to set up resin specialty regeneration system rapidly, should determine lectotype selection and topology layout, now lift example explanation in conjunction with the accompanying drawings according to industrial scale and objective condition:
One, main equipment selection:
Multiple bed: organic glass ion exchange column φ 400 * 2000
Mix bed: " " φ 300 * 2000
Layering post: " " φ 400 * 2000
Actifier column: " " φ 300 * 2000
Mixing column: " " φ 400 * 2000
More than the resin discharge outlet of each post ball be installed cut down.
Two, the filling of resin: with vacuum pump the ion exchange column of loading resin is found time, form negative-pressure adsorption.Be handled easily, establish mobile vacuum pump and union.The resin amount of fill is about 75% of column volume.
Three, each subsystem is furnished with necessary Measuring and testing means: as to water quality resistivity, the dense amount of regenerated liquid and consumption, and the projects such as exchange capacity of resin detect, so that the relevant technologies index is controlled.
Four, about processing condition: according to resin regeneration mechanism, factors such as situation of binding resin own and service requirements are selected.In general should note following some:
(1) technology pure water resistance:>2M Ω, Cm<25 ℃ 〉.
(2) regenerated liquid concentration: about 6%.
(3) regenerated liquid consumption: detect regeneration rate when sampling Detection regeneration rate during 500 liters of first post consumptions, 300 liters of secondary post consumptions, take the circumstances into consideration to adjust to guarantee regeneration effect.
(4) resin flushing: terminal point control PH7.
(5) water flowing in time detects resistivity after the mixed with resin.Back barrelling up to standard.

Claims (4)

1, the manipulation of regeneration of ion exchange resin (hereinafter to be referred as resin) is the essential condition that resin is used, and existing renovation process mainly is static regeneration method and the dynamic method of reproduction of single-column that adopts big basin to soak.Feature of the present invention is to propose a kind of professional renovation process, promptly set up a resin specialty regeneration system rapidly, this system is by pure water preparation, regenerated liquid preparation, resin layering, resin multicolumn series connection regeneration, mixed with resin and 6 groups of subsystems for the treatment of waste liquid become, constitute a complete production system, be suitable in enormous quantities, continuity production, the core of resin specialty regeneration system rapidly is a multicolumn sub-series system, this is that actifier column by proper amt is connected into a closed circuit circulatory system in proper order, makes resin regeneration obtain high quality, high-level efficiency and low consumed good effect.
2, the resin multicolumn sub-series system in the claim 1 also can be used for small serial production separately or only solve our unit's resin regeneration, and columns in series quantity can suitably reduce, even gets the series connection of 2~3 posts.The positive and negative resin is regenerated in batches, actifier column also can hold concurrently layering, mixing, and this small-sized series connection renovation process also can be obtained the effect of connecting preferably to some extent.
3, the pure water preparation subsystem in the claim 1 need can be used to other position of pure water separately, it is characterized in that ion exchange column all adopts the straight type resin of using, the work post is not held concurrently and is regenerated, exchange columns such as positive and negative, mixed bed must not be provided with two components parts for assembly of a machine, respectively establishing one gets final product, water manufacturing system does not contact soda acid, has simplified system, and having made things convenient for operation is pollution-free source water station.
4, product of the present invention is directly to use the type resin, it is characterized in that having the function of direct use, this is the processed goods of raw material type resin, can be used as product market is provided, also can set up stable relation of the supply with the user, the straight type resin of using can be corresponding to raw material type resin formation strong acid, highly basic, weak acid, weak base type series product, also can be divided into two kinds of premium grade and general levels by service requirements, adopt this product can make the user thoroughly break away from heavy regenerative operation and corresponding establishment, utilize existing equipment to obtain good effect.Through good regenerated premium grade is to produce cm(25 ℃ of 18M Ω with the type resin directly) important materials of ultrapure water.
CN90101481A 1990-03-24 1990-03-24 Ion exchange resin specialty regeneration system rapidly and product Pending CN1047269A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100425541C (en) * 2005-03-30 2008-10-15 鞠鹏涛 Tech for regenerating cation exchanger for water treatment ion-exchange salt removing system
CN101711997A (en) * 2009-06-16 2010-05-26 上海轻工业研究所有限公司 Batch regeneration device of ion-exchange resins
CN103611583A (en) * 2013-10-16 2014-03-05 浙江宇达化工有限公司 Exchange resin regeneration treatment apparatus and use method thereof
CN104310530A (en) * 2014-11-20 2015-01-28 许天浩 Protection unit preventing resin leakage
CN111068361A (en) * 2018-10-22 2020-04-28 中国石油化工股份有限公司 Caprolactam ion exchange device and regeneration method thereof

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100425541C (en) * 2005-03-30 2008-10-15 鞠鹏涛 Tech for regenerating cation exchanger for water treatment ion-exchange salt removing system
CN101711997A (en) * 2009-06-16 2010-05-26 上海轻工业研究所有限公司 Batch regeneration device of ion-exchange resins
CN103611583A (en) * 2013-10-16 2014-03-05 浙江宇达化工有限公司 Exchange resin regeneration treatment apparatus and use method thereof
CN104310530A (en) * 2014-11-20 2015-01-28 许天浩 Protection unit preventing resin leakage
CN104310530B (en) * 2014-11-20 2016-01-20 许天浩 Prevent the protected location that resin is revealed
CN111068361A (en) * 2018-10-22 2020-04-28 中国石油化工股份有限公司 Caprolactam ion exchange device and regeneration method thereof
CN111068361B (en) * 2018-10-22 2022-02-11 中国石油化工股份有限公司 Caprolactam ion exchange device and regeneration method thereof

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