CN104140131A - Preparation method of potassium chloroplatinite - Google Patents
Preparation method of potassium chloroplatinite Download PDFInfo
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- CN104140131A CN104140131A CN201410412602.8A CN201410412602A CN104140131A CN 104140131 A CN104140131 A CN 104140131A CN 201410412602 A CN201410412602 A CN 201410412602A CN 104140131 A CN104140131 A CN 104140131A
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- platinum
- potassium chloroplatinite
- potassium
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Abstract
The invention discloses a preparation method of potassium chloroplatinite. The method comprises the following steps: by adopting a waste material namely tetraammineplatinum tetrachloroplatinate always generated in a platinum complex synthesis process as a raw material, performing heating reflux reaction in concentrated hydrochloric acid, filtering to obtain filtrate, and reacting the filtrate with potassium chloride to generate potassium chloroplatinite. The method disclosed by the invention can be used for improving the utilization rate of platinum, reducing the production cost, and reducing the environmental pollution.
Description
Technical field
The present invention relates to the preparation method of platinum compound potassium chloroplatinite, belong to fine chemical product production field.
Background technology
Potassium chloroplatinite, another name: potassium platinochloride; English name: Potassium tetrachloroplatinate (II); CAS:10025-99-7; Molecular weight: 415.09; Molecular formula: K
2ptCl
4, structural formula:
Potassium chloroplatinite is the synthetic conventional raw material of divalence platinum complex, is widely used in the fields such as automotive industry, petrochemical complex, electronic industry, platinum series antineoplastic medicament.The preparation method that potassium chloroplatinite is conventional is: spongy platinum is added in chloroazotic acid, generate Platinic chloride, react with Repone K again and generate potassium platinichloride, with reductive agent reduction potassium platinichlorides such as hydrazine hydrochloride, two hydrazine hydrochloride (CN101279772, JN03131529A) or hydrazine hydrate, hydrazonium sulfate, sulfurous gas, generate potassium chloroplatinite.
Tetramino platinum closes Tetrachloroplatinum; English name: Tetraammineplatinum (II) tetrachloroplatinate (II); Structural formula: [Pt (NH
3)
4] [PtCl
4], molecular weight: 596.0725.Tetramino platinum close Tetrachloroplatinum be the normal waste material producing in the process of synthetic platinum complex (Yu Jianmin. precious metal chemical complex and title complex synthesize handbook [M]. Beijing: Chemical Industry Press, 2009:158-159.), the general method of recycling is that direct-reduction goes out simple substance platinum, and the simple substance platinum of recovery is reused for production again.But in the process that reclaims simple substance platinum, produce a large amount of waste gas, waste water, not only cause environmental pollution, and the platinum loss in removal process is larger, thereby causes production cost higher.
Summary of the invention
The object of this invention is to provide a kind of method of preparing potassium chloroplatinite, the method be take and synthesized the platinum waste material tetramino platinum producing in the process of platinum complex and close Tetrachloroplatinum and prepare potassium chloroplatinite as raw material, the utilization ratio that improves platinum, is conducive to reduce production costs, and reduces environmental pollution.
Technical scheme of the present invention is as follows: a kind of preparation method of potassium chloroplatinite, it is characterized in that, and tetramino platinum closes Tetrachloroplatinum [Pt (NH
3)
4] [PtCl
4] heating reflux reaction in concentrated hydrochloric acid, the filtrate obtaining after filtration is reacted with Repone K and is generated potassium chloroplatinite.Synthetic route is as follows:
Specifically comprise the following steps: get tetramino platinum and close Tetrachloroplatinum, adding concentration is 36～38% concentrated hydrochloric acid reflux (being concentrated hydrochloric acid boiling) reaction 5～15 hours; Cooling down, to room temperature, is filtered the yellow insolubles of filtering, collects filtrate; Potassium chloride joins in above-mentioned filtrate after adding purified water stirring and dissolving, and at room temperature, after stirring reaction 30-60min, under ventilation condition, concentration of reaction solution is to there being dark brown solid to produce, and potassium chloroplatinite crystal is separated out in cooling, filters, and is dried to obtain potassium chloroplatinite.
In tetramino platinum, close the consumption of Tetrachloroplatinum, the add-on of described concentrated hydrochloric acid is 10～50ml/g; The add-on of described Repone K is 0.3～0.5g/g.
The invention has the beneficial effects as follows:
(1) compare existing chloro-platinous acid process for synthesis of potassium, the method be take waste material tetramino platinum and is closed Tetrachloroplatinum as raw material, saved cost, reactions steps of the present invention is simple simultaneously, and do not use chloroazotic acid (corrodibility is extremely strong, to equipment require high) and reductive agent hydrazine hydrochloride (poisonous, contaminate environment) etc., therefore, be more suitable for the carrying out of suitability for industrialized production.
(2) compare existing tetramino platinum and close Tetrachloroplatinum recoverying and utilizing method, the present invention directly produces potassium chloroplatinite with this waste material, save tetramino platinum and closed the reaction process that Tetrachloroplatinum reduction generates simple substance platinum, significantly saved cost, improved the utilization ratio of platinum.Avoid reclaiming the problem that produces large quantity of exhaust gas, waste water in the process of simple substance platinum simultaneously, reduced environmental pollution.
(3) to sum up, the present invention be take and synthesized the platinum waste material tetramino platinum producing in platinum complex process and close Tetrachloroplatinum and prepare potassium chloroplatinite as raw material, improve the utilization ratio of platinum, greatly simplified the production technique of potassium chloroplatinite, significantly reduced production cost, reduce environmental pollution, be more suitable for the carrying out of industrialization reaction.
Embodiment
Reagent and material that the present invention adopts: tetramino platinum closes Tetrachloroplatinum [Pt (NH
3)
4] [PtCl4] be the platinum waste material that produces during trichlorine ammonia potassium platinate is produced (Yu Jianmin. precious metal chemical complex and title complex synthesize handbook [M]. Beijing: Chemical Industry Press, 2009:158-159.), the concentrated hydrochloric acid that hydrochloric acid is 36～38%.Other reagent are domestic analytical pure, and institute's water is purified water.
Below by example, further illustrate the present invention.Example of the present invention is only used for the present invention is described and provides, is not limitation of the present invention.So, under method prerequisite of the present invention, simple modifications of the present invention is all belonged to protection scope of the present invention.
Embodiment 1:
Take tetramino platinum and close 20 grams of Tetrachloroplatinums, add 600ml concentrated hydrochloric acid, heating reflux reaction 8 hours, after cooling down, filters the yellow insolubles of filtering, collects filtrate.Take after 8 grams of Repone K add purified water stirring and dissolving and join in above-mentioned filtrate, at room temperature after stirring reaction 40min, under ventilation condition, boil concentrated (temperature 98-102 ℃) reaction solution to there being dark brown solid to produce, be down to room temperature, separate out potassium chloroplatinite crystal, filter, be dried to obtain 11.7 grams of (platinum contents 46.75% of potassium chloroplatinite, weight loss on drying 0.25%), productive rate 85%, the effective rate of utilization 42.3% of platinum.
Embodiment 2:
Take tetramino platinum and close 35 grams of Tetrachloroplatinums, add 1000ml concentrated hydrochloric acid, heating reflux reaction 10 hours, after cooling down, filters the yellow insolubles of filtering, collects filtrate.Take after 12 grams of Repone K add purified water stirring and dissolving and join in above-mentioned filtrate, at room temperature after stirring reaction 50min, under ventilation condition, boil concentrated (temperature 98-102 ℃) reaction solution to there being dark brown solid to produce, be cooled to room temperature, separate out potassium chloroplatinite crystal, filter, be dried to obtain 20 grams of (platinum contents 46.85% of potassium chloroplatinite, weight loss on drying 0.20%), productive rate 83%, the effective rate of utilization 40.9% of platinum.
Embodiment 3:
Take tetramino platinum and close 80 grams of Tetrachloroplatinums, add 2000ml concentrated hydrochloric acid, heating reflux reaction 15 hours, after cooling down, filters the yellow insolubles of filtering, collects filtrate.Take after 26 grams of Repone K add purified water stirring and dissolving and join in above-mentioned filtrate, at room temperature after stirring reaction 40min, under ventilation condition, boil concentrated (temperature 98-102 ℃) reaction solution to there being dark brown solid to produce, be cooled to room temperature and separate out potassium chloroplatinite crystal, filter, be dried to obtain 54.3 grams of potassium chloroplatinites (platinum content 46.7%, weight loss on drying 0.22%), productive rate 89%, the effective rate of utilization 49.1% of platinum.
Claims (4)
1. a preparation method for potassium chloroplatinite, is characterized in that, tetramino platinum closes Tetrachloroplatinum heating reflux reaction in concentrated hydrochloric acid, and the filtrate obtaining after filtration is reacted with Repone K and generated potassium chloroplatinite.
2. the preparation method of potassium chloroplatinite as claimed in claim 1, is characterized in that, gets tetramino platinum and closes Tetrachloroplatinum, and adding concentration is 36～38% concentrated hydrochloric acid, heating reflux reaction 5～15 hours; Cooling down, to room temperature, is filtered the yellow insolubles of filtering, collects filtrate; Potassium chloride joins in above-mentioned filtrate after adding purified water stirring and dissolving, and at room temperature, after stirring reaction 30-60min, concentration of reaction solution is to there being dark brown solid to produce, and potassium chloroplatinite crystal is separated out in cooling, filters, and is dried to obtain potassium chloroplatinite.
3. the preparation method of potassium chloroplatinite as claimed in claim 1 or 2, is characterized in that, closes the consumption of Tetrachloroplatinum in tetramino platinum, and the add-on of described concentrated hydrochloric acid is 10～50ml/g.
4. the preparation method of potassium chloroplatinite as claimed in claim 1 or 2, is characterized in that, closes the consumption of Tetrachloroplatinum in tetramino platinum, and the add-on of described Repone K is 0.3～0.5g/g.
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| CN201410412602.8A CN104140131B (en) | 2014-08-20 | 2014-08-20 | A kind of preparation method of potassium chloroplatinite |
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| CN201410412602.8A CN104140131B (en) | 2014-08-20 | 2014-08-20 | A kind of preparation method of potassium chloroplatinite |
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| CN104140131B CN104140131B (en) | 2015-09-16 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105293594B (en) * | 2015-12-08 | 2016-09-07 | 山东铂源药业有限公司 | A kind of synthetic method of cis-platinum |
| CN112279316A (en) * | 2020-11-11 | 2021-01-29 | 沈阳有色金属研究院有限公司 | Method for preparing trichloro-ammonio-platinate potassium by ultrasonic method |
| CN113173607A (en) * | 2021-05-07 | 2021-07-27 | 内江洛伯尔材料科技有限公司 | Synthesis method of trichloro ammino potassium platinate |
| CN113929158A (en) * | 2021-10-28 | 2022-01-14 | 浙江微通催化新材料有限公司 | Preparation method of platinum nitrate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101279772A (en) * | 2008-05-15 | 2008-10-08 | 金川集团有限公司 | Preparation of potassium platinochloride |
| CN102328962A (en) * | 2011-08-05 | 2012-01-25 | 昆明理工大学 | Preparation method of tetramine platinum chloride |
| CN102390874A (en) * | 2011-08-01 | 2012-03-28 | 山东铂源化学有限公司 | Preparation method of potassium chloroplatinite |
-
2014
- 2014-08-20 CN CN201410412602.8A patent/CN104140131B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101279772A (en) * | 2008-05-15 | 2008-10-08 | 金川集团有限公司 | Preparation of potassium platinochloride |
| CN102390874A (en) * | 2011-08-01 | 2012-03-28 | 山东铂源化学有限公司 | Preparation method of potassium chloroplatinite |
| CN102328962A (en) * | 2011-08-05 | 2012-01-25 | 昆明理工大学 | Preparation method of tetramine platinum chloride |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105293594B (en) * | 2015-12-08 | 2016-09-07 | 山东铂源药业有限公司 | A kind of synthetic method of cis-platinum |
| CN112279316A (en) * | 2020-11-11 | 2021-01-29 | 沈阳有色金属研究院有限公司 | Method for preparing trichloro-ammonio-platinate potassium by ultrasonic method |
| CN112279316B (en) * | 2020-11-11 | 2022-05-13 | 沈阳有色金属研究院有限公司 | Method for preparing trichloro-ammonio-platinate potassium by ultrasonic method |
| CN113173607A (en) * | 2021-05-07 | 2021-07-27 | 内江洛伯尔材料科技有限公司 | Synthesis method of trichloro ammino potassium platinate |
| CN113929158A (en) * | 2021-10-28 | 2022-01-14 | 浙江微通催化新材料有限公司 | Preparation method of platinum nitrate |
| CN113929158B (en) * | 2021-10-28 | 2023-10-03 | 浙江微通催化新材料有限公司 | Preparation method of platinum nitrate |
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|---|---|
| CN104140131B (en) | 2015-09-16 |
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Denomination of invention: A preparation method of potassium chloroplatinate Effective date of registration: 20211207 Granted publication date: 20150916 Pledgee: Qilu bank Limited by Share Ltd. Ji'nan science and technology innovation center sub branch Pledgor: SHANDONG BOYUAN PHARMACEUTICAL Co.,Ltd. Registration number: Y2021980014223 |
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Address after: 251400 No. 12, Taixing East Street, Jibei Economic Development Zone, Jiyang District, Jinan City, Shandong Province Patentee after: Shandong Baoyuan Pharmaceutical Co.,Ltd. Address before: Strong in Jiyang County of Ji'nan City, 251400 North Street, Shandong Province Economic Development Zone Patentee before: SHANDONG BOYUAN PHARMACEUTICAL Co.,Ltd. |