CN105439089A - Method for recovering iodine from wastewater in medicine production - Google Patents
Method for recovering iodine from wastewater in medicine production Download PDFInfo
- Publication number
- CN105439089A CN105439089A CN201610015836.8A CN201610015836A CN105439089A CN 105439089 A CN105439089 A CN 105439089A CN 201610015836 A CN201610015836 A CN 201610015836A CN 105439089 A CN105439089 A CN 105439089A
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- China
- Prior art keywords
- iodine
- acid
- factory effluent
- hydrogen peroxide
- recovery method
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-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/13—Iodine; Hydrogen iodide
- C01B7/14—Iodine
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The invention discloses a method for recovery iodine from wastewater in medicine production. The method comprises the following steps: acidifying the wastewater in the medicine production with an acid, then reducing inorganic iodine with a reductant, adding a composite oxidant for oxidizing organic iodine, continuously dropwise adding hydrogen peroxide to oxidize iodine negative ions, and simultaneously introducing water vapor to heat and bubble, such that elementary iodine overflows in purple haze; continuously heating till no purple haze overflows, introducing the purple haze to an absorption container, reducing the elementary iodine with a reducible absorption solution, oxidizing the absorption solution with hydrogen peroxide, and filtering and separating to obtain coarse iodine. The acid for acidifying is any one of sulfuric acid, hydrochloric acid or nitric acid; the reductant is one or any two of or a mixture of iron powder, zinc powder, sodium hydrogen sulfite, sodium sulfite or sodium thiosulfate; the composite oxidant is one of C/Fe<2+> or Fe/Fe<3+> in a mixture; the reducible absorption solution is any one of a sulphurous acid solution, a sodium hydrogen sulfite solution or a sodium sulfite solution.
Description
Technical field
The present invention relates to a kind of recovery method of iodine, particularly relate to the recovery method of iodine in medical factory effluent.
Background technology
Iodine produces the basic raw material of medicine intermediate, and usual iodine has very major part to be as catalyzer, hydroxyl protecting group or excessively to add in medicine production, causes medicine to produce in waste liquid containing a large amount of I
2, I
+, IO
3 -and organic iodine, if do not recycle, a large amount of waste will be caused and to environment.
At present, the recovery method about iodine mainly contains:
1) oxidation style: the iodine namely by oxygenant or electrooxidation method, iodide ion being oxidized to free state, then be separated.Conventional oxygenant has hypochlorite, oxymuriate, trivalent iron salt, nitrite and hydrogen peroxide etc.(as CN101041422A, CN1147348C, US2385483, US1881487, US2090866, CN85107208B etc.).
Aforesaid method is generally suitable only for process containing iodine negative ion (I
-) recovery of iodine in waste liquid, and need the consumption of strict controlled oxidization agent, otherwise further elemental iodine can be oxidized to high price iodide ion.
2) reduction method: namely use reductive agent as S-WAT, Sulfothiorine or electrochemical reduction method etc., will high price iodine (I
+, I
3+, I
5+, I
7+) be reduced to the free precipitation of iodine, reach and the object of solution separating (environmental science, 1992,13 (6): 43-48; NuclearInstrumentsandMethodsinPhysicsResearchB, 1997,123:352-355; Talanta, 1997,44:577-583; I1Farmaco, 2003,58:285-292; Deng).This method is only suitable for process containing high price iodine (I
n+) recovery of iodine in waste liquid, also need the consumption strictly controlling reductive agent simultaneously, otherwise elemental iodine can be reduced to iodine negative ion (I further
-).
3) ion exchange method: will be adsorbed by the ion exchange resin electrically contrary with iodide ion containing iodine waste liquid, and then reclaim iodine (CN1331733C, US1058429 through the operation such as resolving, iodine is analysed, US1075049, US4131645, CA763352, CN1300599A etc.).Though this method can play the effect of enrichment iodine, what only applicable process iodine content was relatively low contains iodine waste liquid, otherwise the consumption of resin and regeneration are costly.
4) Air blowing method: first containing iodine waste liquid hcl acidifying, then chlorine oxidation will be passed into, and be blown into air simultaneously and free-iodine is blown out, after absorbing with sulfurous gas, logical chlorine makes iodine dissociate (US4013780, US3346331, US6004465, CN101323434A etc.).Though this method is applicable to the recovery of iodine in process high iodine-containing amount waste liquid, need specific installation, and use chlorine in operating process, therefore environmental pollution is relatively more serious, general this method of less use.
5) flotation process: by I
-be transformed into I
3-or the compound of iodine, then add collecting agent as cetyl trimethylammonium bromide etc. and I
3-form hydrophobic nonionic compound; Again solution is proceeded in flotation column, add inert organic solvents, pass into nitrogen flotation, make iodine be enriched in organic phase; Finally carrying out iodine again analyses process (DE1363491, US3219409 etc.).This method equally can enrichment iodine, is applicable to the low amount of iodine waste liquid of process, but collecting agent is expensive, organic solvent consumption large, cost recovery is higher.
6) active carbon adsorption: utilize the significant absorption property of gac, huge specific surface area, flourishing pore texture and stable chemical property, directly adsorb the iodine (I in waste liquid with gac
2), then reclaim iodine (US1944423 through distillation crystallization; BiomassandBioengergy, 2004,27:89-96; TetrahedronLetters, 2002,43:879-882; Speciality Petrochemicals, 2003,5:30-31 etc.).This method is simple to operate, cost is low, but general be applicable to process content low and with elemental iodine form exist containing iodine waste liquid.
7) extract a distillation method: extracted by iodine to containing the organic solvent adding iodine solubleness larger in iodine waste liquid, then adopt distillation method iodine and organic solvent to be separated, thus reach the object (CA815975, DE1164691 etc.) reclaiming iodine.This method is generally only applicable to process with elemental iodine (I
2) form exist containing iodine waste liquid, and due to the sublimability of iodine, be difficult to thoroughly separate with extraction agent organic solvent.
8) liquid film technology: add proper amount of surfactant in neutral oil, form water-in-oil type emulsion, again with the dispersion system forming water-in-oil-in-water containing iodine waste liquid, selectively be separated and enrichment waste liquid in iodine, iodine is in interior middle generation irreversible reaction mutually simultaneously, generate the product (MicrochemicalJournal, 2001, the 69:45-50 that are difficult to reverse diffusion; Chemistry circular, 1995,1:28-30; Chemical propellant and macromolecular material 2000,2:37-39 etc.).This is the new way of a kind of separation and enrichment iodine, but this technology also imperfection, need to be furtherd investigate further.
As can be seen here, above-mentioned various iodine recovery technology or be suitable for process that single form exists containing iodine waste liquid, complex process, energy consumption and production cost higher, therefore research is a kind of economical, easy and simple to handle, yield is high, and cost is low and can iodine in effective medical factory effluent and to reduce the technique of COD in waste water very necessary.
Summary of the invention
Technical problem to be solved by this invention is, the recovery method of iodine in a kind of medical factory effluent is newly provided, by the method process, not only can iodine in efficient recovery waste water, also effectively can remove the COD in waste water, there is economic environmental protection, the advantage such as easy and simple to handle.
For solving above technical problem, in medical factory effluent of the present invention, the recovery method of iodine, comprises and medical factory effluent is first used acidifying, then with reductive agent by inorganic states iodine (I
2, I
+, IO
3 -) be reduced into iodine negative ion (I
-), then add the composite oxidant for organic iodine being oxidized to elemental iodine or iodine negative ion, and drip hydrogen peroxide continuously by iodine negative ion (I
-) be oxidized to elemental iodine (I
2), pass into steam heating and bubbling simultaneously, make elemental iodine be that purple smoke slowly overflows, till continuing to be heated to overflow without purple smoke, purple smoke passes into and absorbs in container, with the absorption liquid of reductibility by elemental iodine (I
2) be reduced into iodine negative ion (I
-), absorption liquid hydrogen peroxide oxidation, filtering separation obtains thick iodine;
Described acidifying acid is any one in sulfuric acid, hydrochloric acid or nitric acid;
Described reductive agent is a kind of or any two kinds and above mixture in iron powder, zinc powder, sodium bisulfite, S-WAT or Sulfothiorine;
Described composite oxidant is C/Fe
2+or Fe/Fe
3+one in mixture;
The absorption liquid of described reductive agent is any one in sulfurous acid solution, sodium sulfite solution or sodium sulfite solution.
Further, the method comprises the steps:
(1), medical factory effluent is placed in non-pressure vessel, stirs, with acid, waste water is adjusted to pH=2-4;
(2), toward regulating in the waste water after pH value adding reductive agent, stirring 10-30min, making inorganic states iodine (I
2, I
+, IO
3 -) be reduced into iodine negative ion (I
-);
(3), add composite oxidant, stir;
(4), continuously drip hydrogen peroxide, pass into steam heating and bubbling simultaneously, the elemental iodine (I of generation
2) slowly overflow in purple smoke, continue heating bubbling to overflowing without purple smoke;
(5), the purple smoke that overflows passes into and absorbs in container, absorbs purple smoke, make elemental iodine (I with the absorption liquid of reductibility
2) be reduced to iodine negative ion (I
-);
(6), absorption liquid hydrogen peroxide oxidation makes iodine negative ion (I
-) be oxidized to elemental iodine (I
2) separate out completely, suction filtration obtains thick iodine.
Further, described acidifying sulfuric acid, hydrochloric acid or nitric acid are respectively Waste Sulfuric Acid, waste hydrochloric acid or waste nitric acid.
Further, the quality consumption of step (2) described reductive agent is the 0.3%-0.5% of waste water total mass.
Further, the quality consumption of step (3) described composite oxidant is the 0.1%-0.8% of waste water total mass.
Further, described C/Fe
2+in, gac and ferrous sulfate or iron protochloride in mass ratio for 1:3-1:5 mixes, described Fe/Fe
3+middle iron powder and trivalent iron salt are in mass ratio for 1:3-1:5 mixes.
Further, described sulfurous acid solution is passed in water to mix by sulfurous gas and obtains.
Produce in waste liquid due to medicine and contain a large amount of organic iodines, add reductive agent by the I of inorganic states in waste water
2, I
+, IO
3 -be reduced into I
-, then add composite oxidant, organic iodine is oxidized to elemental iodine or iodine negative ion ((I
-)) and destroy the object that organic substance reaches reduction COD.In recyclable waste liquid more than 95% iodine, and remove the COD of in waste liquid more than 60%, both achieved the recycle of iodine, again reduced the content of COD in waste liquid.
Method of the present invention overcomes the deficiency of existing iodine recovery process, compared with prior art, and the advantage such as there is environmental protection, economically feasible, easy and simple to handle, with low cost, the rate of recovery is high and applied widely.
Embodiment
Embodiment 1
Get medicine and produce waste liquid 500g, containing iodine 1.2% (mass content, other embodiments are same), COD content 45000mg/L, regulates pH=2, adds zinc powder 1.5g, stir 10 minutes, add composite oxidant C/Fe
2+0.5g (by gac 0.1g, iron protochloride 0.4g mixing match obtains), stirs 5 minutes; Slowly drip hydrogen peroxide continuously, pass into steam heating and bubbling simultaneously, the purple smoke that elemental iodine is formed overflows slowly, continue to pass into steam heating and bubbling, to overflowing without purple smoke, purple smoke passes into and absorbs in container, absorbs with the absorption liquid (passing into obtained sulfurous acid solution in water by sulfur dioxide gas) of reductibility; Absorption liquid hydrogen peroxide oxidation is separated out to without iodine, and suction filtration obtains thick iodine 6.2g.
Thick iodine purity 94.3% after testing, the total yield of iodine reaches 97.44%, and after process, waste liquid COD content is 13500mg/L, COD clearance is 81.3%.
Embodiment 2:
Get medicine and produce waste liquid 1000g, containing iodine 3.7%, COD content 75000mg/L, regulate pH=2, add S-WAT 4g, stir 10 minutes, add composite oxidant C/Fe
2+2g (by gac 0.5g, ferrous sulfate 1.5g mixing match obtains), stirs 5 minutes; Slowly drip hydrogen peroxide continuously, pass into steam heating and bubbling simultaneously, elemental iodine purple smoke overflows slowly, till continuing to be heated to overflow without purple smoke, purple smoke passes into and absorbs in container, absorbs with the absorption liquid (by sodium bisulfite obtained sulfurous acid solution soluble in water) of reductibility; Absorption liquid hydrogen peroxide oxidation is separated out to without iodine, and suction filtration obtains thick iodine 38g.
Thick iodine purity 95.6% after testing, the total yield of iodine reaches 98.2%, and after process, waste liquid COD content is 14000mg/L, COD clearance is 81.3%.
Embodiment 3
Get medicine and produce waste liquid 2000g, containing iodine 10%, COD content 100000mg/L, regulate pH=2, add with arbitrarily than the iron powder of mixing and the mixture 10g of zinc powder, stir 10 minutes, add composite oxidant Fe/Fe
3+8g (by iron powder 2g, ferric sulfate 6g mixing match obtains), stirs 5 minutes; Drip hydrogen peroxide, pass into steam heating and bubbling simultaneously, elemental iodine purple smoke overflows slowly, and till continuing to be heated to overflow without purple smoke, purple smoke passes into and absorbs in container, absorbs with the absorption liquid (sodium sulfite solution) of reductibility; Absorption liquid hydrogen peroxide oxidation is separated out to without iodine, and suction filtration obtains thick iodine 210g.
Thick iodine purity 92.7% after testing, the total yield of iodine reaches 97.33%, and after process, waste liquid COD content is 25000mg/L, COD clearance is 75%.
Embodiment 4
Get medicine and produce waste liquid 3000g, containing iodine 5.2%, COD content 80000mg/L, regulate pH=2, add Sulfothiorine 10g, stir 10 minutes, add composite oxidant Fe/Fe
3+9g (by iron powder 2g, iron(ic) chloride 7g mixing match obtains), stirs 5 minutes; Slowly drip hydrogen peroxide continuously, pass into steam heating and bubbling, elemental iodine purple smoke overflows slowly simultaneously, till continuing to be heated to overflow without purple smoke, purple smoke passes into and absorbs in container, absorbs with the absorption liquid (sodium sulfite solution) of reductibility; Absorption liquid hydrogen peroxide oxidation is separated out to without iodine, and suction filtration obtains thick iodine 163.5g.
Thick iodine purity 93.5% after testing, the total yield of iodine reaches 98%, and after process, waste liquid COD content is 16500mg/L, COD clearance is 79.37%.
Claims (7)
1. the recovery method of iodine in a medical factory effluent, it is characterized in that comprising and medical factory effluent is first used acidifying, with reductive agent, inorganic states iodine is reduced into iodine negative ion again, then the composite oxidant for organic iodine being oxidized to elemental iodine or iodine negative ion is added, and iodine negative ion is oxidized to elemental iodine by dropping hydrogen peroxide continuously, pass into steam heating and bubbling simultaneously, elemental iodine is made to be that purple smoke overflows, till continuing to be heated to overflow without purple smoke, purple smoke passes into and absorbs in container, with the absorption liquid of reductibility, elemental iodine is reduced into iodine negative ion, absorption liquid hydrogen peroxide oxidation, filtering separation obtains thick iodine,
Described acidifying acid is any one in sulfuric acid, hydrochloric acid or nitric acid;
Described reductive agent is a kind of or any two kinds and above mixture in iron powder, zinc powder, sodium bisulfite, S-WAT or Sulfothiorine;
Described composite oxidant is C/Fe
2+or Fe/Fe
3+one in mixture;
The absorption liquid of described reductibility is any one in sulfurous acid solution, sodium sulfite solution or sodium sulfite solution.
2. the recovery method of iodine in medical factory effluent according to claim 1, is characterized in that the method comprises the steps:
(1), medical factory effluent is placed in non-pressure vessel, stirs, with acid, waste water is adjusted to pH=2-4;
(2), toward regulating in the waste water after pH value adding reductive agent, stirring 10-30min;
(3), add composite oxidant, stir;
(4), continuously drip hydrogen peroxide, pass into steam heating and bubbling, purple smoke slowly overflows simultaneously, continues heating bubbling to overflowing without purple smoke;
(5) purple smoke, overflowed passes into and absorbs in container, with the absorption liquid absorption purple smoke of reductive agent;
(6), absorption liquid hydrogen peroxide oxidation separates out completely to iodine, and suction filtration obtains thick iodine.
3. the recovery method of iodine in medical factory effluent according to claim 1 or 2, is characterized in that: described acidifying sulfuric acid, hydrochloric acid or nitric acid are respectively Waste Sulfuric Acid, waste hydrochloric acid or waste nitric acid.
4. the recovery method of iodine in medical factory effluent according to claim 1 or 2, is characterized in that: the quality consumption of step (2) described reductive agent is the 0.3%-0.5% of waste water total mass.
5. the recovery method of iodine in medical factory effluent according to claim 2, is characterized in that: the quality consumption of step (3) described composite oxidant is the 0.1%-0.8% of waste water total mass.
6. the recovery method of iodine in medical factory effluent according to claim 1 or 2 or 5, is characterized in that: described C/Fe
2+in, gac and ferrous sulfate or iron protochloride in mass ratio for 1:3-1:5 mixes, described Fe/Fe
3+middle iron powder and trivalent iron salt are in mass ratio for 1:3-1:5 mixes.
7. the recovery method of iodine in medical factory effluent according to claim 1, is characterized in that: it is obtained that described sulfurous acid solution passes into mixing in water by sulfurous gas.
Priority Applications (1)
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|---|---|---|---|
| CN201610015836.8A CN105439089A (en) | 2016-01-11 | 2016-01-11 | Method for recovering iodine from wastewater in medicine production |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610015836.8A CN105439089A (en) | 2016-01-11 | 2016-01-11 | Method for recovering iodine from wastewater in medicine production |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106517252A (en) * | 2016-10-10 | 2017-03-22 | 无锡易水元资源循环科技有限公司 | Analytical pure potassium iodide preparation method using waste liquid containing iodine |
| CN109368594A (en) * | 2018-11-22 | 2019-02-22 | 山东罗欣药业集团股份有限公司 | The recovery method of iodine in a kind of cephalosporins medicine waste liquid |
| CN110194501A (en) * | 2019-04-30 | 2019-09-03 | 凯莱英医药化学（阜新）技术有限公司 | From the continuous process and continuous device for recycling iodide in waste water containing iodine |
| CN110662713A (en) * | 2017-06-07 | 2020-01-07 | 伯拉考成像股份公司 | Process for recovering iodine from aqueous solutions |
| CN112028020A (en) * | 2020-09-02 | 2020-12-04 | 山东博苑医药化学股份有限公司 | Process for recovering iodine from iodine bromide-containing medical organic waste liquid |
| CN113461230A (en) * | 2021-06-11 | 2021-10-01 | 浙江工业职业技术学院 | Treatment method for iodine-containing organic wastewater |
| CN115159588A (en) * | 2021-04-02 | 2022-10-11 | 中冶长天国际工程有限责任公司 | Method for catalytically recovering elemental sulfur and ammonium ferrous sulfate from sulfur dioxide flue gas |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106517252A (en) * | 2016-10-10 | 2017-03-22 | 无锡易水元资源循环科技有限公司 | Analytical pure potassium iodide preparation method using waste liquid containing iodine |
| CN110662713A (en) * | 2017-06-07 | 2020-01-07 | 伯拉考成像股份公司 | Process for recovering iodine from aqueous solutions |
| CN110662713B (en) * | 2017-06-07 | 2023-11-28 | 伯拉考成像股份公司 | Method for recovering iodine from aqueous solutions |
| CN109368594A (en) * | 2018-11-22 | 2019-02-22 | 山东罗欣药业集团股份有限公司 | The recovery method of iodine in a kind of cephalosporins medicine waste liquid |
| CN110194501A (en) * | 2019-04-30 | 2019-09-03 | 凯莱英医药化学（阜新）技术有限公司 | From the continuous process and continuous device for recycling iodide in waste water containing iodine |
| CN112028020A (en) * | 2020-09-02 | 2020-12-04 | 山东博苑医药化学股份有限公司 | Process for recovering iodine from iodine bromide-containing medical organic waste liquid |
| CN112028020B (en) * | 2020-09-02 | 2021-06-22 | 山东博苑医药化学股份有限公司 | Process for recovering iodine from iodine bromide-containing medical organic waste liquid |
| CN115159588A (en) * | 2021-04-02 | 2022-10-11 | 中冶长天国际工程有限责任公司 | Method for catalytically recovering elemental sulfur and ammonium ferrous sulfate from sulfur dioxide flue gas |
| CN115159588B (en) * | 2021-04-02 | 2023-12-29 | 中冶长天国际工程有限责任公司 | Method for catalytically recycling elemental sulfur and ferrous ammonium sulfate from sulfur dioxide flue gas |
| CN113461230A (en) * | 2021-06-11 | 2021-10-01 | 浙江工业职业技术学院 | Treatment method for iodine-containing organic wastewater |
| CN113461230B (en) * | 2021-06-11 | 2022-09-30 | 浙江工业职业技术学院 | Treatment method for iodine-containing organic wastewater |
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Application publication date: 20160330 |