CN101759152A - Method for removing impurities in process of extracting iodine by using iodine-contained phosphate ore as raw materials - Google Patents
Method for removing impurities in process of extracting iodine by using iodine-contained phosphate ore as raw materials Download PDFInfo
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- CN101759152A CN101759152A CN200910102856A CN200910102856A CN101759152A CN 101759152 A CN101759152 A CN 101759152A CN 200910102856 A CN200910102856 A CN 200910102856A CN 200910102856 A CN200910102856 A CN 200910102856A CN 101759152 A CN101759152 A CN 101759152A
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Abstract
The invention discloses a method for removing impurities in a process of extracting iodine by using iodine-contained phosphate ore as raw materials, relating to a process for extracting iodine by using iodine-contained phosphate ore as raw materials. The method comprises the steps of: 1, purifying crude iodine coming out of an extraction tower by using concentrated sulfuric acid after vacuum dehydration, separating to crude iodine water, inorganic impurities and organic impurities under the stirring; 2, heating the crude iodine to enable iodine simple substances to be sublimated and separated from the concentrated sulfuric acid and the impurities; and 3, condensing and crystallizing iodine steam sublimated by heating to obtain purer iodine. Aiming at the characteristics of the impurities in diluted phosphoric acid, the method is used for removing impurities by adopting the concentrated sulfuric acid, the concentrated sulfuric acid also removes the water in the iodine simple substances while oxidizing the inorganic or organic impurities in the iodine simple substances, the product is further dried; during the sublimation separation of the iodine by heating, the oxidized impurities are remained in the concentrated sulfuric acid, thereby effectively improving the product quality and enabling the iodine extracted from the phosphate ore to be applied to the high and new technical field.
Description
Technical field
The present invention relates to iodine, specifically, relating in to contain the iodine Rock Phosphate (72Min BPL) is the technological process that raw material extracts iodine, furthermore, relates to the method for removing impurity in this process.
Background technology
Iodine often is present in the multiple Mineral resources with the form of associated minerals, and phosphorus ore association iodine resource reclaims the appearance of industrialization technology, makes the iodine in the phosphorus ore obtain extracting and utilizing.
Extracting iodine from phosphorus ore mainly is to utilize the phosphoric acid of phosphorus ore production to carry out as raw material, this Technology has been documented in Chinese patent No. 200510003058.2 " extracting the method for iodine from contain the iodine phosphate ore production in the dilute phosphoric acid that produces " lining.Produce in the process of phosphoric acid at phosphorus ore, iodine as associated minerals enters into phosphoric acid with ionic forms, can make it from phosphoric acid, to separate behind the medicament with molecular conformation in addition, the phosphoric acid that will contain molecular iodine then pumps in the extraction tower, finally utilize its physico-chemical property, in extraction tower, it is extracted by adding extraction agent.But the composition of the dilute phosphoric acid that this technology is used is very complicated, contains the impurity of a lot of organic or inorganics in the thick iodine product, and the existence of these impurity has influenced the quality of iodine and limited the application of iodine in high frontier.
Summary of the invention
The object of the present invention is to provide a kind of is that raw material extracts the method for removing impurity in the iodine technology to contain the iodine Rock Phosphate (72Min BPL), to reduce the content of impurity in the iodine, improves the quality of iodine product.
For reaching this purpose, the contriver has invented one and has overlapped the Technology that can improve the iodine product quality preferably by constantly groping, and the method for removing impurity that provides comprises:
(1) after the thick iodine process vacuum hydro-extraction of coming out, purifies with the vitriol oil earlier, under agitation deviate from thick iodine moisture content, inorganic impurity and organic impurity from extraction tower;
(2) then, heat thick iodine, make the elemental iodine distillation and separate with the vitriol oil and impurity;
(3) iodine steam that comes out of heating sublimation passes through condensation-crystallization again, obtains comparatively purified iodine.
The above-mentioned vitriol oil that is used to purify is that massfraction is 93%～105% the vitriol oil, and the vitriol oil is 6: 1 with the mass ratio of thick iodine; Above-mentioned stir speed (S.S.) is 200r/min.
The intensification amplitude is controlled to be 10 ℃/min during the thick iodine of above-mentioned heating, and the heating-up time is 40min.
The condensation-crystallization temperature of above-mentioned iodine steam is 60 ℃～90 ℃.
The inventive method has adopted vitriol oil removal of impurities at the characteristics of impurity in the dilute phosphoric acid, and the vitriol oil is also sloughed the moisture in the elemental iodine in the organic or inorganic impurity in iodine oxide simple substance, and product is further dry; In the process of heating iodine sublimation separation, oxidized impurity is stayed in the vitriol oil, thereby improves the iodine product quality effectively, makes also can use in high frontier from the iodine of phosphorus ore extraction.
Embodiment further specifies beneficial effect of the present invention by following examples:
Wengfu Group Co., Ltd. adopts phosphorus ore iodine of the present invention to remove the technology of impurity:
(1) after the thick iodine process vacuum hydro-extraction of coming out from extraction tower, be that 98% the vitriol oil purifies earlier with massfraction, the vitriol oil is 6: 1 with the mass ratio of thick iodine, in stir speed (S.S.) is to deviate from thick iodine moisture content, inorganic impurity and organic impurity under the stirring of 200r/mi n;
(2) then, heat thick iodine, the intensification amplitude is controlled to be 10 ℃/min, and the heating-up time is 40min, makes the elemental iodine distillation and separates with the vitriol oil and impurity;
(3) iodine steam that comes out of heating sublimation is 60 ℃～90 ℃ following condensation-crystallizations in temperature, obtains purity and be 99.5% iodine product.
Claims (4)
1. be that raw material extracts the method for removing impurity in the iodine technology to contain the iodine Rock Phosphate (72Min BPL), its feature comprises:
(1) after the thick iodine process vacuum hydro-extraction of coming out, purifies with the vitriol oil earlier, under agitation deviate from thick iodine moisture content, inorganic impurity and organic impurity from extraction tower;
(2) then, heat thick iodine, make the elemental iodine distillation and separate with the vitriol oil and impurity;
(3) iodine steam that comes out of heating sublimation passes through condensation-crystallization again, obtains comparatively purified iodine.
2. according to the described method of removing impurity of claim 1, it is characterized in that the described vitriol oil that is used to purify is that massfraction is 93%～105% the vitriol oil, the vitriol oil is 6: 1 with the mass ratio of thick iodine; Described stir speed (S.S.) is 200r/min.
3. according to the described method of removing impurity of claim 1, the intensification amplitude is controlled to be 10 ℃/min when it is characterized in that the thick iodine of described heating, and the heating-up time is 40min.
4. according to the described method of removing impurity of claim 1, the condensation-crystallization temperature that it is characterized in that described iodine steam is 60 ℃～90 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910102856A CN101759152A (en) | 2009-11-17 | 2009-11-17 | Method for removing impurities in process of extracting iodine by using iodine-contained phosphate ore as raw materials |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910102856A CN101759152A (en) | 2009-11-17 | 2009-11-17 | Method for removing impurities in process of extracting iodine by using iodine-contained phosphate ore as raw materials |
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| Publication Number | Publication Date |
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| CN101759152A true CN101759152A (en) | 2010-06-30 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN200910102856A Pending CN101759152A (en) | 2009-11-17 | 2009-11-17 | Method for removing impurities in process of extracting iodine by using iodine-contained phosphate ore as raw materials |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103332654A (en) * | 2013-07-16 | 2013-10-02 | 瓮福（集团）有限责任公司 | High-purity iodine production device |
| CN103342344A (en) * | 2013-07-16 | 2013-10-09 | 瓮福（集团）有限责任公司 | Crude iodine purifying process |
| CN103663377A (en) * | 2013-12-13 | 2014-03-26 | 瓮福（集团）有限责任公司 | Method for refining crude iodine extracted from iodine-containing phosphate ore |
| CN108383405A (en) * | 2018-05-30 | 2018-08-10 | 中国地质大学（北京） | A method of preparing plasterboard with artificial hilllock stone cutting bits |
-
2009
- 2009-11-17 CN CN200910102856A patent/CN101759152A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103332654A (en) * | 2013-07-16 | 2013-10-02 | 瓮福（集团）有限责任公司 | High-purity iodine production device |
| CN103342344A (en) * | 2013-07-16 | 2013-10-09 | 瓮福（集团）有限责任公司 | Crude iodine purifying process |
| CN103663377A (en) * | 2013-12-13 | 2014-03-26 | 瓮福（集团）有限责任公司 | Method for refining crude iodine extracted from iodine-containing phosphate ore |
| CN108383405A (en) * | 2018-05-30 | 2018-08-10 | 中国地质大学（北京） | A method of preparing plasterboard with artificial hilllock stone cutting bits |
| CN108383405B (en) * | 2018-05-30 | 2020-10-30 | 中国地质大学（北京） | Method for preparing gypsum board by using artificial granite cutting scraps |
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Open date: 20100630 |