CN101254459A - Reinforced regeneration method of big-hole adsorption resin - Google Patents

Reinforced regeneration method of big-hole adsorption resin Download PDF

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Publication number
CN101254459A
CN101254459A CNA2008100604218A CN200810060421A CN101254459A CN 101254459 A CN101254459 A CN 101254459A CN A2008100604218 A CNA2008100604218 A CN A2008100604218A CN 200810060421 A CN200810060421 A CN 200810060421A CN 101254459 A CN101254459 A CN 101254459A
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China
Prior art keywords
resin
purified water
per ton
eluate
regeneration
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CNA2008100604218A
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Chinese (zh)
Inventor
胡季强
鲍建伟
姚德中
巫雷
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Zhejiang Conba Pharmaceutical Co., Ltd.
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ZHEJIANG CONBA PHARMACEUTICAL CO Ltd
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Priority to CNA2008100604218A priority Critical patent/CN101254459A/en
Publication of CN101254459A publication Critical patent/CN101254459A/en
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Abstract

A method for the reinforcement and the regeneration of macroporous adsorbent resins is provided. The method includes the following steps: loading an aged resin into a resin column with upper and lower stainless steel sieves provided with 120 meshes at a diameter/high ratio of 1:1-1:3, washing with purified water at a flow rate of 1m<3>/h per ton of resins until the eluate is colorless, back-washing with compressed air or purified water for 3-5 times in the washing process, washing again with 0.1-5.0% hypochloric acid or hypochlorite solution at a flow rate of 1m<3>/h per ton of resins until the eluate is colorless, further washing with purified water at flow rate of 1m<3>/h per ton of resins until the pH value of the eluate is 7 or reaches a pre-determined value, optionally neutralizing the hypochloric acid or hypochlorite residues in resin with 0.5-3.0% hydrochloric acid solution at a flow rate of 0.5-1.5 m<3>/h per ton of resins and washing with purified water until the pH value is 7. The hypochloric acid or hypochlorite solution is sodium hypochlorite and has a concentration of 1.0-3.0% preferably. The inventive method has the advantages of easy operation, low cost, good regeneration effect and waster reutilization.

Description

A kind of intensifying regeneration of macroporous absorbent resin
Technical field
The present invention relates to the intensifying regeneration of macroporous absorbent resin.
Background technology
Macroporous absorbent resin is a kind of manually synthetic polymer absorbant of porous three dimensional structure that has, it is a class new type resin that on ion-exchanger and other adsorbent application foundation, grows up, be Van der Waals force and the hydrogen bond action that relies between it and the molecule that is adsorbed, undertaken by huge specific area that physical absorption works, in actual applications to some molecules close such as the very strong adsorption capacity of the outstanding tool of aromatic series ring-type compound with its skeleton structure.
Macroporous absorbent resin has had application study more widely at aspects such as the extraction of Natural Medicine Chemistry composition, separation and purification, preparation process reform, quality of the pharmaceutical preparations analyses in recent years, and clearly demonstrates the effect of its uniqueness.This technological operation is easy, and cost is lower, and resin can use repeatedly, is fit to suitability for industrialized production.Simultaneously, macroporous absorbent resin is to industrial wastewater, and the processing of waste liquid also has a wide range of applications, and can realize that harmful substance reclaims the purpose of using, turning harm into good, turn waste into wealth in the industrial production.
Macroporous absorbent resin is an organic high molecular polymer, thereby in use can make the resin adsorption ageing of performance because of the Irreversible Adsorption and the impurities accumulation of macromolecular substances such as pigment, by the processing of regenerating of NaOH and HCl solution conventional regeneration solvent, adsorptivity can not be recovered, thereby causes adsorbance to descend gradually.When range of decrease degree 30% is above instantly, will produces the adsorbing separation of active ingredient and have a strong impact on, cause the production cost waste.
" economizing on resources the protection environment " is a big theme of current society, at present; the resin that loses adsorption capacity is mostly arbitrarily abandoned; not only cause the wasting of resources, and can cause environmental pollution, this is the macroporous absorbent resin prolonged application is needed solution badly in Chinese medicine preparation a problem.
The content of invention
The technical problem to be solved in the present invention provides a kind of intensifying regeneration of ageing of performance macroporous absorbent resin, to recover the absorption property of resin to the full extent, realize recycling of waste resin, make the macroporous absorbent resin can prolonged application, reduce application cost, reduce the wasting of resources and environmental pollution.
Technical scheme of the present invention is achieved in that the discarded macroporous absorbent resin with ageing of performance is an object, and purified water is cleaned, and cleans with hypochlorous acid or hypochlorite solutions, is washed to neutrality, adds acid in case of necessity and carries out neutralisation treatment to neutral.
The intensifying regeneration that the present invention proposes may further comprise the steps:
(1) resin of ageing of performance is packed into be equipped with up and down in the resin column of 120 order stainless steel mesh, blade diameter length ratio was controlled at 1: 1~1: 3, with resin 1m per ton 3The flow velocity of/h is washed till the eluate clear, colorless with purified water, recoils 3~5 times with compressed air or purified water in the cleaning process, makes resin loose evenly;
(2) treat that the purifying water surface drops to resin surface in the resin, with resin 1m per ton 3The flow velocity of/h is washed till the eluate clear, colorless with 0.1~5.0% hypochlorous acid or hypochlorite solutions, again with resin 1m per ton 3The flow velocity of/h with purified water be washed till the eluate pH value be 7 or the setting value;
(3) because behind intensifying regenerating, the regenerative agent residual quantity is bigger, it is longer to be washed to the neutral time, and therefore not reaching at 7 o'clock at pH value can also increase following steps: the hydrochloric acid solution with 0.5~3.0% is according to resin 0.5~1.5m per ton 3In the flow velocity of/h and resin in residual hypochlorous acid or hypochlorite, being washed till pH value with purified water again is 7.
Hypochlorous acid or hypochlorite solutions are regenerated solvent, clorox (NaClO) preferably, and the concentration of hypochlorous acid or hypochlorite is preferably 1.0~3.0%.
Resin model commonly used among the present invention is D101, DM131, AB-8, ADS-16, ADS-17, YWD13C macroporous absorbent resin or polyamide polymeric adsorbent.
The macroporous absorbent resin intensifying regeneration that the present invention proposes, have following advantage: this invention has simple to operate, consumables cost is low again, favorable regeneration effect, can remove some and remain in the composition that causes resin " dead absorption " in the resin, make the macroporous absorbent resin absorption property be promoted to 90%~95%, realize that the recovery again of salvage property is used by about 65%, resin per ton can be saved 2~30,000 yuan cost consumption, and avoids waste resin burning or buried environment is polluted.
The specific embodiment
Example 1
Take by weighing the DM131 macroporous absorbent resin of 1000 kilograms of ageing of performance, pack into be fixed with 120 order stainless steel mesh up and down, volume is 1.5m 3The stainless steel resin column in, with 1m 3The flow velocity of/h is washed till the eluate clear, colorless with purified water, recoils 3~5 times with compressed air or purified water in the cleaning process, makes resin loose evenly; Treat that the purifying water surface drops to resin surface in the resin, with 1m 3The flow velocity of/h is washed till the eluate clear, colorless with 1.0% NaClO solution, again with 1m 3It is colourless that the flow velocity of/h is washed till eluate with purified water, uses 0.5% hydrochloric acid solution according to 1m then 3In the flow velocity of/h and resin in residual NaClO, being washed till pH value with purified water again is 7.Contrast before and after handling, untreated macroporous absorbent resin is a yellowish-brown, and bright in vain through the resin color and luster of intensifying regenerating, adsorption capacity is promoted to 95% by 68% before handling.
Example 2
Take by weighing the ADS-16 macroporous absorbent resin of 1000 kilograms of ageing of performance, pack into be fixed with 120 order stainless steel mesh up and down, volume is 1.5m 3The stainless steel resin column in, with 1m 3The flow velocity of/h is washed till the eluate clear, colorless with purified water, recoils 3~5 times with compressed air or purified water in the cleaning process, makes resin loose evenly; Treat that the purifying water surface drops to resin surface in the resin, with 1m 3The flow velocity of/h is washed till the eluate clear, colorless with 2.0% NaClO solution, again with 1m 3It is 7 that the flow velocity of/h is washed till pH value with purified water.Contrast before and after handling, untreated macroporous absorbent resin color and luster is black dull, and bright in vain through the resin color and luster of intensifying regenerating, adsorption capacity is promoted to 90% by 65% before handling.
Example 3
Take by weighing the polyamide polymeric adsorbent of 1000 kilograms of ageing of performance, pack into be fixed with 120 order stainless steel mesh up and down, volume is 1.5m 3The stainless steel resin column in, with 1m 3The flow velocity of/h is washed till the eluate clear, colorless with purified water, recoils 3~5 times with compressed air or purified water in the cleaning process, makes resin loose evenly; Treat that the purifying water surface drops to resin surface in the resin, with 1m 3The flow velocity of/h is washed till the eluate clear, colorless with 3.0% NaClO solution, again with 1m 3It is colourless that the flow velocity of/h is washed till eluate with purified water, uses 3.0% hydrochloric acid solution according to 1m then 3In the flow velocity of/h and resin in residual NaClO, being washed till pH value with purified water again is 7.Contrast before and after handling, untreated macroporous absorbent resin color and luster is black dull, and bright in vain through the resin color and luster of intensifying regenerating, adsorption capacity is promoted to 92% by 60% before handling.

Claims (4)

1. the intensifying regeneration of a macroporous absorbent resin is characterized in that, this method may further comprise the steps:
A. the resin of ageing of performance is packed into and be equipped with up and down in the resin column of 120 order stainless steel mesh, blade diameter length ratio was controlled at 1: 1~1: 3, with resin 1m per ton 3The flow velocity of/h is washed till the eluate clear, colorless with purified water, recoils 3~5 times with compressed air or purified water in the cleaning process, makes resin loose evenly;
B. treat that the purifying water surface drops to resin surface in the resin, with resin 1m per ton 3The flow velocity of/h is washed till the eluate clear, colorless with 0.1~5.0% hypochlorous acid or hypochlorite solutions, again with resin 1m per ton 3The flow velocity of/h with purified water be washed till the eluate pH value be 7 or the setting value.
2. the intensifying regeneration of macroporous absorbent resin according to claim 1 is characterized in that, this method is further comprising the steps of: the hydrochloric acid solution with 0.5~3.0% is according to resin 0.5~1.5m per ton 3In the flow velocity of/h and resin in residual hypochlorous acid or hypochlorite, being washed till pH value with purified water again is 7.
3. the intensifying regeneration of macroporous absorbent resin according to claim 1 and 2 is characterized in that: described hypochlorous acid or hypochlorite solutions are the liquor natrii hypochloritis.
4. the intensifying regeneration of macroporous absorbent resin according to claim 1 and 2, it is characterized in that: the concentration of described hypochlorous acid or hypochlorite solutions is 1.0~3.0%.
CNA2008100604218A 2008-04-08 2008-04-08 Reinforced regeneration method of big-hole adsorption resin Pending CN101254459A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101985102A (en) * 2010-10-28 2011-03-16 内蒙古金达威药业有限公司 Online regeneration method for chromatographic silica gel of coenzyme Q10
CN102228844A (en) * 2011-07-21 2011-11-02 南华大学 Cleaning method of uranium hydrometallurgy fixed bed ion exchange resin
CN102815820A (en) * 2012-08-14 2012-12-12 攀钢集团攀枝花钢铁研究院有限公司 Apparatus for removing SO4<2-> and Cl<-> from flue gas desulfurization solution, and process thereof
CN102815819A (en) * 2012-08-14 2012-12-12 攀钢集团攀枝花钢铁研究院有限公司 Low loss desulfurization solution purification process
CN102861559A (en) * 2012-09-24 2013-01-09 浙江工商大学 Production method of polyacrylonitrile chelating resin metal adsorbent
CN109967136A (en) * 2019-03-08 2019-07-05 中核通辽铀业有限责任公司 A kind of fixed-bed resin washing and detoxifying integral method
CN111659363A (en) * 2020-06-13 2020-09-15 劲牌有限公司 Regeneration method of macroporous adsorption resin
CN112717904A (en) * 2020-12-28 2021-04-30 宜宾丝丽雅股份有限公司 Recovery process method of resin activator by bipolar membrane pretreatment process

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101985102A (en) * 2010-10-28 2011-03-16 内蒙古金达威药业有限公司 Online regeneration method for chromatographic silica gel of coenzyme Q10
CN101985102B (en) * 2010-10-28 2012-09-05 内蒙古金达威药业有限公司 Online regeneration method for chromatographic silica gel of coenzyme Q10
CN102228844A (en) * 2011-07-21 2011-11-02 南华大学 Cleaning method of uranium hydrometallurgy fixed bed ion exchange resin
CN102228844B (en) * 2011-07-21 2012-11-28 南华大学 Cleaning method of uranium hydrometallurgy fixed bed ion exchange resin
CN102815820A (en) * 2012-08-14 2012-12-12 攀钢集团攀枝花钢铁研究院有限公司 Apparatus for removing SO4<2-> and Cl<-> from flue gas desulfurization solution, and process thereof
CN102815819A (en) * 2012-08-14 2012-12-12 攀钢集团攀枝花钢铁研究院有限公司 Low loss desulfurization solution purification process
CN102861559A (en) * 2012-09-24 2013-01-09 浙江工商大学 Production method of polyacrylonitrile chelating resin metal adsorbent
CN102861559B (en) * 2012-09-24 2014-10-08 浙江工商大学 Production method of polyacrylonitrile chelating resin metal adsorbent
CN109967136A (en) * 2019-03-08 2019-07-05 中核通辽铀业有限责任公司 A kind of fixed-bed resin washing and detoxifying integral method
CN111659363A (en) * 2020-06-13 2020-09-15 劲牌有限公司 Regeneration method of macroporous adsorption resin
CN112717904A (en) * 2020-12-28 2021-04-30 宜宾丝丽雅股份有限公司 Recovery process method of resin activator by bipolar membrane pretreatment process

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