CN1924043A - Method of deep eliminating minute quantity organic solvent from inorganic salt solvent - Google Patents
Method of deep eliminating minute quantity organic solvent from inorganic salt solvent Download PDFInfo
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- CN1924043A CN1924043A CNA2006101527845A CN200610152784A CN1924043A CN 1924043 A CN1924043 A CN 1924043A CN A2006101527845 A CNA2006101527845 A CN A2006101527845A CN 200610152784 A CN200610152784 A CN 200610152784A CN 1924043 A CN1924043 A CN 1924043A
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- organic solvent
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention discloses a deep-grade removing method of trace organic solvent from inorganic solution (NiSO4, NiCl2, CuSO4, CoCl2 and so on), which is characterized by the following: adopting extracting technology to purify; clearing; floating through ultrasound; adsorbing through active charcoal and fiber; adopting XAD-4 large-aperture ionic exchanging resin to do organic adsorption disposal; making organic solvent less than 0.5ppm in the solution.
Description
Technical field
A kind of inorganic salt solution (NiSO
4, NiCl
2, CuSO
4, CoCl
2Deng) degree of depth removes the method for micro-organic solvent, relate to a kind of after non-ferrous metal inorganic salt solution employing organic solvent extraction technology purifying treatment, through carrying out the method that the degree of depth is removed micro-content organism again after the processing of methods such as clarification, air supporting, ultrasonic wave, gac, fiber absorption.
Background technology
The non-ferrous metal inorganic salt solution is in scavenging process, usually adopt the organic solvent extraction technology, but often contain residual micro-organic solvent in the solution after purification, adopt in the solution after combination organic matter removal technologies such as charcoal absorption or tubular fibre absorption are carried out in common clarification separation, ultrasonic wave air supporting again, generally contain organic solvent at 1～2ppm, can be satisfied with common electrolysis or electrodeposition and produce the requirement of pure metal product, also can crystallization produce the salt series products of general quality, but can not be satisfied with the requirement that direct crystallization is produced high-quality salt series products.
Summary of the invention
The present invention is directed to the deficiency that above-mentioned prior art exists, providing a kind of can remove the further degree of depth of the organic solvent in the inorganic salt solution, make to contain organic solvent in the solution and reach 0.1ppm, the method for a kind of deep eliminating minute quantity organic solvent from inorganic salt solvent of high 0.5ppm
Technology of the present invention realizes by following scheme.
A kind of method of deep eliminating minute quantity organic solvent from inorganic salt solvent, comprise solution carried out extracting and purifying after, adopt conventional clarification separation, ultrasonic wave air supporting, carry out the organic matter removal process of charcoal absorption or tubular fibre absorption again, it is characterized in that adopting again XAD-4 wide aperture adsorptive type ion exchange resin to carry out organic adsorption treatment, make to contain organic solvent in the solution less than 0.5ppm.
Method of the present invention with load the polymeric adsorbent of organic solvent with pure water washing and recycling inorganic salt solution after, again with about 2% NaOH solution drip washing resin, and then with the water purification wash residual behind the NaOH on the resin, can make resin holomorphosis, reuse.
Method of the present invention will contain the organic solution of 1～2ppm after will handling, adopt ion-exchange absorption resin, and XAD-4 wide aperture adsorptive type ion exchange resin is removed organic solvent in the inorganic salt solution, and equipment used is common ion-exchange unit dress.Load the polymeric adsorbent of organic solvent with pure water washing and recycling inorganic salt solution after, behind the NaOH on the resin, can make resin holomorphosis again with about 2% NaOH solution drip washing resin, and then with the water purification wash residual, reuse.
Adopt method of the present invention, can make the organic solvent content in the inorganic salt solution further be reduced to 0.1ppm, be satisfied with the requirement that high-quality non-ferrous metal salt series products is produced in crystallization.
Embodiment
A kind of method of deep eliminating minute quantity organic solvent from inorganic salt solvent, with the solution behind the extracting and purifying, adopt conventional clarification separation, ultrasonic wave air supporting, again carry out the organic matter removal technology of charcoal absorption or tubular fibre absorption after, adopt XAD-4 wide aperture adsorptive type ion exchange resin to carry out organic adsorption treatment again, make to contain organic solvent in the solution less than 0.5ppm.Method of the present invention with load the polymeric adsorbent of organic solvent with pure water washing and recycling inorganic salt solution after, again with about 2% NaOH solution drip washing resin, and then with the water purification wash residual behind the NaOH on the resin, can make resin holomorphosis, reuse.
Embodiment 1
Adopt used drum type brake ion exchange column in the conventional ion exchange process process, two ends are provided with the dusting cover formula tube sheet that the blocks ions exchange resin overflows or spills, or corrosion-resistant screen cloth, the middle part adds XAD-4 wide aperture nonionic adsorption resin, and is totally standby with clear water drip washing.The inorganic salt NiSO that will contain organic solvent
4Solution (concentration requirement of main metal content is with non-crystallizable exceeding under the typical temperature condition), containing organic solvent total amount is 2.0ppm, add ion exchange column slowly continuously and flow out continuously, the speed that solution stream is crossed is exceeded with the resin bed volume that per hour is no more than 4 times.Containing organism in the solution is 0.1-0.5ppm.After the solution total amount passed through of stream reaches 800 times of resin bed volumes, polymeric adsorbent with regard to complete saturated load organic solvent.
Be about the polymeric adsorbent of 4 times of drip washing load organic solvents of resin bed volume, the recyclable inorganic salt solution that remains on the resin bed with clear water or pure water.With 2.0% NaOH solution drip washing loaded resin, total consumption is about 6 times of resin bed volume then, and flow velocity is about per hour 2 times resin bed volume.And then be about 4 times of drip washing resins of resin bed volume with clear water or pure water, and make resin holomorphosis, be equipped with next loop cycle and used.
Embodiment 2
Adopt used drum type brake ion exchange column in the conventional ion exchange process process, two ends are provided with the dusting cover formula tube sheet that the blocks ions exchange resin overflows or spills, or corrosion-resistant screen cloth, the middle part adds XAD-4 wide aperture nonionic adsorption resin, and is totally standby with clear water drip washing.The inorganic salt NiCl that will contain organic solvent
2Solution (concentration requirement of main metal content is with non-crystallizable exceeding under the typical temperature condition), containing organic solvent total amount is 1.0ppm, add ion exchange column slowly continuously and flow out continuously, the speed that solution stream is crossed is exceeded with the resin bed volume that per hour is no more than 4 times.Containing organism in the solution is 0.1-0.5ppm.After the solution total amount passed through of stream reaches 9000 times of resin bed volumes, polymeric adsorbent with regard to complete saturated load organic solvent.
Be about the polymeric adsorbent of 5 times of drip washing load organic solvents of resin bed volume, the recyclable inorganic salt solution that remains on the resin bed with clear water or pure water.With 2.0% NaOH solution drip washing loaded resin, total consumption is about 7 times of resin bed volume then, and flow velocity is about per hour 3 times resin bed volume.And then be about 5 times of drip washing resins of resin bed volume with clear water or pure water, and make resin holomorphosis, be equipped with next loop cycle and used.
Embodiment 3
Adopt used drum type brake ion exchange column in the conventional ion exchange process process, two ends are provided with the dusting cover formula tube sheet that the blocks ions exchange resin overflows or spills, or corrosion-resistant screen cloth, the middle part adds XAD-4 wide aperture nonionic adsorption resin, and is totally standby with clear water drip washing.The inorganic salt CuSO that will contain organic solvent
4Solution (concentration requirement of main metal content is with non-crystallizable exceeding under the typical temperature condition), containing organic solvent total amount is 2.27ppm, add ion exchange column slowly continuously and flow out continuously, the speed that solution stream is crossed is exceeded with the resin bed volume that per hour is no more than 6 times; Containing organism in the solution is 0.1-0.5ppm.After the solution total amount passed through of stream reaches 1000 times of resin bed volumes, polymeric adsorbent with regard to complete saturated load organic solvent.
Be about the polymeric adsorbent of 6 times of drip washing load organic solvents of resin bed volume, the recyclable inorganic salt solution that remains on the resin bed with clear water or pure water.With 2.0% NaOH solution drip washing loaded resin, total consumption is about 8 times of resin bed volume then, and flow velocity is about per hour 4 times resin bed volume.And then be about 6 times of drip washing resins of resin bed volume with clear water or pure water, and make resin holomorphosis, be equipped with next loop cycle and used.
Embodiment 4
Adopt used drum type brake ion exchange column in the conventional ion exchange process process, two ends are provided with the dusting cover formula tube sheet that the blocks ions exchange resin overflows or spills, or corrosion-resistant screen cloth, the middle part adds XAD-4 wide aperture nonionic adsorption resin, and is totally standby with clear water drip washing.The inorganic salt CoCl that will contain organic solvent
2Solution (concentration requirement of main metal content is with non-crystallizable exceeding under the typical temperature condition), contain the about 1.5ppm of organic solvent total amount) add ion exchange column slowly continuously and flow out continuously, the speed that solution stream is crossed is exceeded with the resin bed volume that per hour is no more than 4 times.Containing organism in the solution is 0.1-0.5ppm.After the solution total amount passed through of stream reaches 800 times of resin bed volumes, polymeric adsorbent with regard to complete saturated load organic solvent.
Be about the polymeric adsorbent of 6 times of drip washing load organic solvents of resin bed volume, the recyclable inorganic salt solution that remains on the resin bed with clear water or pure water.With 2.0% NaOH solution drip washing loaded resin, total consumption is about 7 times of resin bed volume then, and flow velocity per hour is 3 times a resin bed volume.And then be about 5 times of drip washing resins of resin bed volume with clear water or pure water, and make resin holomorphosis, be equipped with next loop cycle and used.
The technical data sheet of embodiment 1 (loop cycle) table 1
| Preceding liquid organic content ppm | 1# 2# | 2.27 1.56 | |
| Back liquid organic content ppm | 1# 2# 5# 10# 15# 20# 25# 30# 35# 40# | 0.5 0.4 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 | Each sample number is equivalent to the solution amount of 20 times of resin bed volumes |
| Callable washing lotion metal ion g/l | 1# 2# 3# | 30.98 5.55 0.12 | Liquid behind 3 times of resin bed volumes of liquid wash water behind 2 times of resin bed volumes of liquid wash water behind 1 times of resin bed volume wash water |
Claims (2)
1. the method for a deep eliminating minute quantity organic solvent from inorganic salt solvent, comprise solution carried out extracting and purifying after, adopt conventional clarification separation, ultrasonic wave air supporting, carry out the organic matter removal process of charcoal absorption or tubular fibre absorption again, it is characterized in that adopting again XAD-4 wide aperture adsorptive type ion exchange resin to carry out organic adsorption treatment, make to contain organic solvent in the solution less than 0.5ppm.
2. according to requiring 1 described method on the right, the polymeric adsorbent that it is characterized in that with load organic solvent with pure water washing and recycling inorganic salt solution after, again with NaOH solution drip washing resin, and then after washing the NaOH that remains on the resin with water, make resin holomorphosis, reuse.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006101527845A CN1924043A (en) | 2006-09-29 | 2006-09-29 | Method of deep eliminating minute quantity organic solvent from inorganic salt solvent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006101527845A CN1924043A (en) | 2006-09-29 | 2006-09-29 | Method of deep eliminating minute quantity organic solvent from inorganic salt solvent |
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| Publication Number | Publication Date |
|---|---|
| CN1924043A true CN1924043A (en) | 2007-03-07 |
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|---|---|---|---|
| CNA2006101527845A Pending CN1924043A (en) | 2006-09-29 | 2006-09-29 | Method of deep eliminating minute quantity organic solvent from inorganic salt solvent |
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|---|---|
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102206752A (en) * | 2011-05-20 | 2011-10-05 | 昆明理工大学 | Method for removing organic matter contained in supernatant liquor obtained from zinc hydrometallurgy through active carbons |
| CN101784481B (en) * | 2007-08-23 | 2013-05-01 | 陶氏环球技术公司 | Process and apparatus for purification of industrial brine |
| CN107986317A (en) * | 2017-11-16 | 2018-05-04 | 厦门建霖健康家居股份有限公司 | A kind of preparation method of cupric sulfate purified |
| CN111424174A (en) * | 2019-04-22 | 2020-07-17 | 中国科学院过程工程研究所 | Method for removing surfactant in metal raw material leaching solution, purification device and application |
| CN111424170A (en) * | 2019-04-22 | 2020-07-17 | 中国科学院过程工程研究所 | Method and system for producing ammonium paratungstate by acidic extraction |
-
2006
- 2006-09-29 CN CNA2006101527845A patent/CN1924043A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101784481B (en) * | 2007-08-23 | 2013-05-01 | 陶氏环球技术公司 | Process and apparatus for purification of industrial brine |
| CN102206752A (en) * | 2011-05-20 | 2011-10-05 | 昆明理工大学 | Method for removing organic matter contained in supernatant liquor obtained from zinc hydrometallurgy through active carbons |
| CN102206752B (en) * | 2011-05-20 | 2012-11-28 | 昆明理工大学 | Method for removing organic matter contained in supernatant liquor obtained from zinc hydrometallurgy through active carbons |
| CN107986317A (en) * | 2017-11-16 | 2018-05-04 | 厦门建霖健康家居股份有限公司 | A kind of preparation method of cupric sulfate purified |
| CN107986317B (en) * | 2017-11-16 | 2022-06-21 | 厦门建霖健康家居股份有限公司 | Preparation method of electroplating-grade copper sulfate |
| CN111424174A (en) * | 2019-04-22 | 2020-07-17 | 中国科学院过程工程研究所 | Method for removing surfactant in metal raw material leaching solution, purification device and application |
| CN111424170A (en) * | 2019-04-22 | 2020-07-17 | 中国科学院过程工程研究所 | Method and system for producing ammonium paratungstate by acidic extraction |
| CN111424174B (en) * | 2019-04-22 | 2022-03-25 | 中国科学院过程工程研究所 | Method for removing surfactant in metal raw material leaching solution, purification device and application |
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