CN103820644B - Method for extracting zinc chloride from pharmaceutical waste liquid of vitamin E - Google Patents
Method for extracting zinc chloride from pharmaceutical waste liquid of vitamin E Download PDFInfo
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- CN103820644B CN103820644B CN201410104433.1A CN201410104433A CN103820644B CN 103820644 B CN103820644 B CN 103820644B CN 201410104433 A CN201410104433 A CN 201410104433A CN 103820644 B CN103820644 B CN 103820644B
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- zinc chloride
- vitamin
- pharmaceutical waste
- concentrated solution
- waste liquor
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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 method for extracting zinc chloride from pharmaceutical waste liquid of vitamin E. The method comprises the following steps: (1) extracting organic matters with high boiling points from the pharmaceutical waste liquid of the vitamin E by using a butyl acetate extracting agent at room temperature, so that the zinc chloride of the waste liquid is separated; (2) performing evaporation concentration on the extracted solution to obtain a concentrated solution containing a crude zinc chloride product; (3) adding hydrogen peroxide into the concentrated solution containing the crude zinc chloride product, and heating at 80 DEG C while stirring to convert the solution into a concentrated solution containing zinc chloride; (4) refluxing the concentrated solution containing the zinc chloride at 130 DEG C with chlorobenzene to obtain anhydrous zinc chloride. Compared with the prior art, the method disclosed by the invention has the advantages that the treatment cost is relatively low and the zinc chloride is relatively high in both recovery rate and purity.
Description
Technical field
The present invention relates to the method extracting zinc chloride from pharmaceutical waste liquor, being specifically related to from preparing the method extracting zinc chloride waste liquid that vitamin-E produces.
Background technology
Zinc chloride (ZnCl
2) usually one of catalyzer being used as pharmacy procedure, so, completing in the waste liquid that pharmacy produces, just have a large amount of zinc chloride.For saving resource avoids zinc chloride to the pollution of environment simultaneously, just zinc chloride again should be extracted from pharmaceutical waste liquor.The Measures compare again extracting at present zinc chloride is many, and its core point is all first allow the various organism in zinc chloride and pharmaceutical waste liquor reliably separate, and then extracts in zinc chloride never (or substantially not having) organic solution further.Method that what Qufu Normal University proposed be oxidized carbazole ketone pharmaceutical waste liquor with oxygenant Cui Peiying. and the comprehensive treating process of carbazole ketone pharmaceutical waste liquor and extract zinc chloride [J]. Chemical Engineering Technology and exploitation, 2007,36(5): 45-47} is exactly one of them.The method with the organism in oxidizing carbazole ketone pharmaceutical waste liquor, and after isolating the solution being substantially free of organic thing, then concentrates through heating evaporation, just can allow zinc chloride crystallization in this waste liquid.For carbazole ketone pharmaceutical waste liquor, the method can obtain good effect really.But it is comparatively large that the method but exists oxidant content requirement, the deficiency that processing costs is higher, and for the pharmaceutical waste liquor of vitamin-E, the rate of recovery that utilization the method extracts zinc chloride is also lower.Its reason is, the high boiling point organic compounds such as Trimethylhydroquinone, different vegetable alcohol and a small amount of vitamin-E be residual are included in the pharmaceutical waste liquor of vitamin-E, these high boiling point organic compounds are all with-OH or-COOH group, very easily form stable inner complex with zine ion generation chelatropic reaction, this just causes the extreme difficulties being separated these high boiling point organic compounds with mode of oxidizing, and then has had a strong impact on the rate of recovery of zinc chloride.
Summary of the invention
The object of the invention is, provide a kind of processing costs lower and the higher method extracting zinc chloride from vitamin-E pharmaceutical waste liquor of the zinc chloride rate of recovery.
For realizing described object, provide a kind of like this method extracting zinc chloride from vitamin-E pharmaceutical waste liquor, method same as the prior art is that the method includes oxidation step.Its improvements are, the oxygenant in described oxidation step is hydrogen peroxide, and the step of the method is as follows:
(1) under room temperature state, the vitamin-E pharmaceutical waste liquor through homogenizing process is fully mixed with extraction agent butylacetate, to extract the high boiling point organic compound in vitamin-E pharmaceutical waste liquor, and make it be separated with the zinc chloride in vitamin-E pharmaceutical waste liquor; Wherein, the volume ratio of butylacetate and vitamin-E pharmaceutical waste liquor is 1: (2 ~ 4); The concentration of butylacetate is 0.88 g/mL, and the content of zinc chloride in vitamin-E pharmaceutical waste liquor is 700 ~ 800 g/L;
(2) raffinate after step (1) being extracted carries out evaporation concentration, to obtain the concentrated solution of Containing Zinc Chloride crude product at 150 DEG C;
(3) in the concentrated solution of step (2) gained Containing Zinc Chloride crude product, add described hydrogen peroxide, and carry out heated and stirred at 80 DEG C; Churning time with the concentrated solution lighter of Containing Zinc Chloride crude product and no longer variable color is degree; Wherein, the volume ratio of the concentrated solution of hydrogen peroxide and Containing Zinc Chloride crude product is 1: (100 ~ 200); The massfraction of hydrogen peroxide is 30%;
(4) the concentrated solution chlorobenzene of step (3) gained Containing Zinc Chloride is refluxed at 130 DEG C, to obtain Zinc Chloride Anhydrous; Wherein, in chlorobenzene and concentrated solution, the mol ratio of zinc chloride is 1: 1, and return time is all converted into Zinc Chloride Anhydrous for degree with described zinc chloride; The concentration of chlorobenzene is 1.10g/mL.
As can be seen from scheme, the present invention is extracting in zinc chloride process from vitamin-E pharmaceutical waste liquor, purity and the color and luster of oxygenant used just for improving isolated zinc chloride, and reliably and effectively zinc chloride and high boiling point organic compound (Trimethylhydroquinone, different vegetable alcohol and a small amount of vitamin-E are residual) are separated in vitamin-E pharmaceutical waste liquor, employing be solvent extration---specifically extract the high boiling point organic compound in vitamin-E pharmaceutical waste liquor with butylacetate in step (1).It will be apparent to those skilled in that, extraction process is actual is exactly the process be dissolved into by high boiling point organic compound in butylacetate, because zinc chloride is insoluble to butylacetate, so, just reliable and have effectively achieved both separation.After evaporation concentration being carried out to raffinate in step (2), low-boiling-point organic compound (methyl alcohol, acetic acid etc.) in vitamin-E pharmaceutical waste liquor and a large amount of water are also all evaporated, and so just obtain substantially not containing organism and the concentrated solution of the also few Containing Zinc Chloride crude product of other residual impurity.After this, ability hydrogen peroxide improves the zinc chloride color and luster in concentrated solution, and zinc chloride of purifying further, also create condition for an in the end step chlorobenzene backflow carrys out obtained Zinc Chloride Anhydrous simultaneously.It will be apparent to those skilled in that, butylacetate can recycle after eliminating the high boiling point organic compound be dissolved in wherein, and can see that from scheme the consumption only for the hydrogen peroxide improving zinc chloride purity and color and luster is few, so, relative to prior art, the present invention has the lower advantage of processing costs.According to above-mentioned analysis, the present invention can overcome prior art and extract the lower deficiency of the rate of recovery of zinc chloride from vitamin-E pharmaceutical waste liquor; Experimental verification proves, the zinc chloride rate of recovery of the present invention is really higher, reaches more than 95%; Purity is also higher, minimumly reaches 94%.
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment
From vitamin-E pharmaceutical waste liquor, extract a method for zinc chloride, the method includes oxidation step.In the present invention, the oxygenant in described oxidation step is hydrogen peroxide (H
2o
2), the step of the method is as follows:
(1) under room temperature state, by through the vitamin-E pharmaceutical waste liquor of homogenizing process and extraction agent butylacetate ［ CH
3cOO (CH
2)
3cH
3fully mix, to extract the high boiling point organic compound in vitamin-E pharmaceutical waste liquor, and make it be separated with the zinc chloride in vitamin-E pharmaceutical waste liquor; Wherein, the volume ratio of butylacetate and vitamin-E pharmaceutical waste liquor is 1: (2 ~ 4); The concentration of butylacetate is 0.88g/mL, and the content of zinc chloride in vitamin-E pharmaceutical waste liquor is 700 ~ 800g/L;
(2) raffinate after step (1) being extracted carries out evaporation concentration, to obtain the concentrated solution of Containing Zinc Chloride crude product at 150 DEG C;
(3) in the concentrated solution of step (2) gained Containing Zinc Chloride crude product, add described hydrogen peroxide, and carry out heated and stirred at 80 DEG C; Churning time with the concentrated solution lighter of Containing Zinc Chloride crude product and no longer variable color is degree (usually stirring about 30 minutes, the zinc chloride that zinc chloride crude product in concentrated solution all can be changed into); Wherein, the volume ratio of the concentrated solution of hydrogen peroxide and Containing Zinc Chloride crude product is 1: (100 ~ 200); The massfraction of hydrogen peroxide is 30%;
(4) by the concentrated solution chlorobenzene (C of step (3) gained Containing Zinc Chloride
6h
5cl) reflux at 130 DEG C, to obtain Zinc Chloride Anhydrous; Wherein, in chlorobenzene and concentrated solution, the mol ratio of zinc chloride is 1: 1, and return time is all converted into Zinc Chloride Anhydrous for degree with described zinc chloride; The concentration of chlorobenzene is that 1.10g/mL(usually stirs 2 hours and can complete; Those skilled in the art can find out, the chlorobenzene in said ratio is excessive use, so just can ensure that the zinc chloride in concentrated solution all changes into Zinc Chloride Anhydrous; Obviously, after reflux operation terminates, the chlorobenzene of excessive portion is pourable to be re-used).
Further, for improving extraction efficiency, the mode of described extraction is in step (1) counter current contact extraction mode.
The present invention have passed the experimental verification done in laboratory, and verification step is identical with the step of above-mentioned embodiment.
Before checking, to the vitamin-E pharmaceutical waste liquor of checking, first adopt yellow prussiate of potash volumetry in HB/T2323-2004 " industrial chlorinations zinc ", measure the content of zinc in vitamin-E pharmaceutical waste liquor.The content of the Zinc Chloride Anhydrous that the Zn content after step (1) extraction in raffinate and step (4) obtain also adopts yellow prussiate of potash titration measuring in B/T2323-2004 " industrial chlorinations zinc ", then calculates the rate of recovery of zinc chloride and the purity of zinc chloride respectively.The result is shown in proof list (note: " zinc chloride content " expression " content of zinc chloride in vitamin-E pharmaceutical waste liquor " in proof list, " water oil ratio " expression " volume ratio of butylacetate and vitamin-E pharmaceutical waste liquor ", " liquid liquor ratio " expression " volume ratio of the concentrated solution of hydrogen peroxide and Containing Zinc Chloride crude product "; For abridgment of table, in technical scheme, technical characteristic is only fixed value, does not fill in into).
As can be seen from above-mentioned checking example, the present invention can make the rate of recovery of zinc chloride reach more than 95%, and the loss of zinc is few, and the purity of zinc chloride can reach more than 94%, reaches general industry zinc chloride standard.
Claims (2)
1. from vitamin-E pharmaceutical waste liquor, extract a method for zinc chloride, the method includes oxidation step, it is characterized in that, the oxygenant in described oxidation step is hydrogen peroxide, and the step of the method is as follows:
(1) under room temperature state, the vitamin-E pharmaceutical waste liquor through homogenizing process is fully mixed with extraction agent butylacetate, to extract the high boiling point organic compound in vitamin-E pharmaceutical waste liquor, and make it be separated with the zinc chloride in vitamin-E pharmaceutical waste liquor; Wherein, the volume ratio of butylacetate and vitamin-E pharmaceutical waste liquor is 1: (2 ~ 4); The concentration of butylacetate is 0.88g/mL, and the content of zinc chloride in vitamin-E pharmaceutical waste liquor is 700 ~ 800g/L;
(2) raffinate after step (1) being extracted carries out evaporation concentration, to obtain the concentrated solution of Containing Zinc Chloride crude product at 150 DEG C;
(3) in the concentrated solution of step (2) gained Containing Zinc Chloride crude product, add described hydrogen peroxide, and carry out heated and stirred at 80 DEG C; Churning time with the concentrated solution lighter of Containing Zinc Chloride crude product and no longer variable color is degree; Wherein, the volume ratio of the concentrated solution of hydrogen peroxide and Containing Zinc Chloride crude product is 1: (100 ~ 200); The massfraction of hydrogen peroxide is 30%;
(4) the concentrated solution chlorobenzene of step (3) gained Containing Zinc Chloride is refluxed at 130 DEG C, to obtain Zinc Chloride Anhydrous; Wherein, in chlorobenzene and described concentrated solution, the mol ratio of zinc chloride is 1: 1, and return time is all converted into Zinc Chloride Anhydrous for degree with described zinc chloride; The concentration of chlorobenzene is 1.10g/mL.
2. from vitamin-E pharmaceutical waste liquor, extract the method for zinc chloride according to claim 1, it is characterized in that, the mode of extraction described in step (1) is counter current contact extraction mode.
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| CN201410104433.1A CN103820644B (en) | 2014-03-20 | 2014-03-20 | Method for extracting zinc chloride from pharmaceutical waste liquid of vitamin E |
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| CN201410104433.1A CN103820644B (en) | 2014-03-20 | 2014-03-20 | Method for extracting zinc chloride from pharmaceutical waste liquid of vitamin E |
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| CN103820644B true CN103820644B (en) | 2015-05-13 |
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| CN110386712B (en) * | 2019-08-02 | 2021-10-22 | 山东新和成维生素有限公司 | Method for comprehensively utilizing zinc-containing wastewater |
| CN113501607B (en) * | 2021-07-05 | 2023-02-03 | 山东新和成维生素有限公司 | Recycling method of zinc-containing wastewater |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1061763A (en) * | 1990-11-27 | 1992-06-10 | 彭长 | A kind of production zinc chloride novel process |
| CN101875504A (en) * | 2009-04-30 | 2010-11-03 | 内蒙古神舟硅业有限责任公司 | Method for preparing high-purity anhydrous zinc chloride |
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2014
- 2014-03-20 CN CN201410104433.1A patent/CN103820644B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1061763A (en) * | 1990-11-27 | 1992-06-10 | 彭长 | A kind of production zinc chloride novel process |
| CN101875504A (en) * | 2009-04-30 | 2010-11-03 | 内蒙古神舟硅业有限责任公司 | Method for preparing high-purity anhydrous zinc chloride |
Non-Patent Citations (2)
| Title |
|---|
| "从咔唑酮制药废液提取氯化锌";刘西德等;《山东化工》;20061231;第35卷(第1期);第1-3页 * |
| "咔唑酮制药废液的综合处理及提取氯化锌";崔培英;《化工技术与开发》;20070531;第36卷(第5期);第45-47、51页 * |
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