CN104140131B - A kind of preparation method of potassium chloroplatinite - Google Patents
A kind of preparation method of potassium chloroplatinite Download PDFInfo
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- CN104140131B CN104140131B CN201410412602.8A CN201410412602A CN104140131B CN 104140131 B CN104140131 B CN 104140131B CN 201410412602 A CN201410412602 A CN 201410412602A CN 104140131 B CN104140131 B CN 104140131B
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Abstract
The invention discloses a kind of preparation method of potassium chloroplatinite.The method closes Tetrachloroplatinum for raw material with the waste material tetramino platinum produced normal in the process of synthesis platinum complex, and heating reflux reaction in concentrated hydrochloric acid, the filtrate obtained after filtration and Repone K react and generates potassium chloroplatinite.Method of the present invention improves platinum utilization, not only reduces production cost, and decreases 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 raw material that synthesis divalence platinum complex is conventional, 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: added by spongy platinum in chloroazotic acid, generate Platinic chloride, react with Repone K again and generate potassium platinichloride, generate potassium chloroplatinite with reductive agent reduction potassium platinichlorides such as hydrazine hydrochloride, two hydrazine hydrochloride (CN101279772, JN03131529A) or hydrazine hydrate, hydrazonium sulfate, sulfurous gas.
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 in the process of synthesis platinum complex normal produce waste material (Yu Jianmin. precious metal chemical complex and title complex synthesis handbook [M]. Beijing: Chemical Industry Press, 2009:158-159.), the method of general 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 reclaiming simple substance platinum, produce a large amount of waste gas, waste water, not only cause environmental pollution, and platinum loss in removal process is comparatively large, thus cause production cost higher.
Summary of the invention
The object of this invention is to provide a kind of method preparing potassium chloroplatinite, the method closes Tetrachloroplatinum for raw material is to prepare potassium chloroplatinite to synthesize the platinum waste material tetramino platinum produced in the process of platinum complex, improve platinum utilization, be conducive to reducing production cost, reduce environmental pollution.
Technical scheme of the present invention is as follows: a kind of preparation method of potassium chloroplatinite, is characterized in that, tetramino platinum closes Tetrachloroplatinum [Pt (NH
3)
4] [PtCl
4] heating reflux reaction in concentrated hydrochloric acid, the filtrate obtained after filtration and Repone K react and generate potassium chloroplatinite.Synthetic route is as follows:
Specifically comprise the following steps: get tetramino platinum and close Tetrachloroplatinum, add the concentrated hydrochloric acid that concentration is 36 ~ 38%, reflux (i.e. concentrated hydrochloric acid boiling) reaction 5 ~ 15 hours; After cooling down to room temperature, filter the yellow insolubles of filtering, collect filtrate; Potassium chloride joins after adding purified water stirring and dissolving in above-mentioned filtrate, and at room temperature after stirring reaction 30-60min, under ventilation condition, concentration of reaction solution produces to there being dark brown solid, and potassium chloroplatinite crystal is separated out in cooling, filters, dry potassium chloroplatinite.
Close the use gauge of Tetrachloroplatinum with tetramino platinum, 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) existing chloro-platinous acid process for synthesis of potassium is compared, the method closes Tetrachloroplatinum for raw material with waste material tetramino platinum, save cost, reactions steps of the present invention is simple simultaneously, and do not use chloroazotic acid (corrodibility is extremely strong, high to the requirement of equipment) and reductive agent hydrazine hydrochloride (poisonous, contaminate environment) etc., therefore, the carrying out of suitability for industrialized production is more suitable for.
(2) compare existing tetramino platinum and close Tetrachloroplatinum recoverying and utilizing method, the present invention directly produces potassium chloroplatinite with this waste material, eliminate tetramino platinum and close the reaction process that Tetrachloroplatinum reduction generates simple substance platinum, significantly saved cost, improve platinum utilization.Avoid in the process reclaiming simple substance platinum simultaneously and produce large quantity of exhaust gas, useless water problem, reduce environmental pollution.
(3) to sum up, the present invention closes Tetrachloroplatinum for raw material is to prepare potassium chloroplatinite to synthesize the platinum waste material tetramino platinum produced in platinum complex process, improve platinum utilization, enormously simplify the production technique of potassium chloroplatinite, considerably reduce production cost, decrease environmental pollution, be more suitable for the carrying out of industrialization reaction.
Embodiment
The reagent that the present invention adopts and material: tetramino platinum closes Tetrachloroplatinum [Pt (NH
3)
4] [PtCl4] be trichlorine ammonia potassium platinate produce in produce platinum waste material (Yu Jianmin. precious metal chemical complex and title complex synthesis handbook [M]. Beijing: Chemical Industry Press, 2009:158-159.), hydrochloric acid is the concentrated hydrochloric acid of 36 ~ 38%.Other reagent are domestic analytical pure, and water used is purified water.
The present invention is further illustrated below by example.Example of the present invention is only used for the present invention being described and providing, and is not limitation of the present invention.So, under method prerequisite of the present invention, all protection scope of the present invention is belonged to simple modifications of the present invention.
Embodiment 1:
Take tetramino platinum and close Tetrachloroplatinum 20 grams, add 600ml concentrated hydrochloric acid, heating reflux reaction 8 hours, after cooling down, filter the yellow insolubles of filtering, collect filtrate.Taking after 8 grams of Repone K add purified water stirring and dissolving joins in above-mentioned filtrate, at room temperature after stirring reaction 40min, under ventilation condition, boil concentrated (temperature 98-102 DEG C) reaction solution produce to there being dark brown solid, be down to room temperature, separate out potassium chloroplatinite crystal, filter, dry potassium chloroplatinite 11.7 grams of (platinum contents 46.75%, 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 Tetrachloroplatinum 35 grams, add 1000ml concentrated hydrochloric acid, heating reflux reaction 10 hours, after cooling down, filter the yellow insolubles of filtering, collect filtrate.Taking after 12 grams of Repone K add purified water stirring and dissolving joins in above-mentioned filtrate, at room temperature after stirring reaction 50min, under ventilation condition, boil concentrated (temperature 98-102 DEG C) reaction solution produce to there being dark brown solid, be cooled to room temperature, separate out potassium chloroplatinite crystal, filter, dry potassium chloroplatinite 20 grams of (platinum contents 46.85%, 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 Tetrachloroplatinum 80 grams, add 2000ml concentrated hydrochloric acid, heating reflux reaction 15 hours, after cooling down, filter the yellow insolubles of filtering, collect filtrate.Taking after 26 grams of Repone K add purified water stirring and dissolving joins in above-mentioned filtrate, at room temperature after stirring reaction 40min, under ventilation condition, boil concentrated (temperature 98-102 DEG C) reaction solution produce to there being dark brown solid, be cooled to room temperature and separate out potassium chloroplatinite crystal, filter, dry potassium chloroplatinite 54.3 grams (platinum content 46.7%, weight loss on drying 0.22%), productive rate 89%, the effective rate of utilization 49.1% of platinum.
Claims (1)
1. a preparation method for potassium chloroplatinite, is characterized in that, gets tetramino platinum and closes Tetrachloroplatinum, add the concentrated hydrochloric acid that concentration is 36 ~ 38%, heating reflux reaction 5 ~ 15 hours; After cooling down to room temperature, filter the yellow insolubles of filtering, collect filtrate; Potassium chloride joins after adding purified water stirring and dissolving in above-mentioned filtrate, and at room temperature after stirring reaction 30-60min, concentration of reaction solution produces to there being dark brown solid, and potassium chloroplatinite crystal is separated out in cooling, filters, dry potassium chloroplatinite; Close the use gauge of Tetrachloroplatinum with tetramino platinum, the add-on of described concentrated hydrochloric acid is 10 ~ 50ml/g, and the add-on of described Repone K is 0.3 ~ 0.5 g/g.
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| CN104140131B true CN104140131B (en) | 2015-09-16 |
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Families Citing this family (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 |
| 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 |
| CN113173607B (en) * | 2021-05-07 | 2023-01-31 | 内江洛伯尔材料科技有限公司 | Synthesis method of trichloro ammine potassium platinate |
| 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 |
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 |
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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 |
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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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