CN102583589B - New method for synthesizing dinitroso diammineplatinum (II) - Google Patents
New method for synthesizing dinitroso diammineplatinum (II) Download PDFInfo
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- CN102583589B CN102583589B CN201210099447.XA CN201210099447A CN102583589B CN 102583589 B CN102583589 B CN 102583589B CN 201210099447 A CN201210099447 A CN 201210099447A CN 102583589 B CN102583589 B CN 102583589B
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- dinitroso
- ammino platinum
- platinum
- diiodo
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Abstract
The invention discloses a new method for synthesizing dinitroso diammineplatinum (II). Cis-diiododiammineplatinum (II) is used as the original raw material. The new method comprises the following steps of: adding a certain quantity of purified water into the cis-diiododiammineplatinum to uniformly stir, then, reacting with mercurous nitrate to obtain a hydrating solution, and enabling the obtained hydrating solution to react with a sodium nitrite solution to prepare the dinitroso diammineplatinum (II). The method is simple in operation, short in production period and capable of effectively solving the problem of overhigh content of free inorganic salt.
Description
Technical field
The present invention relates to compound dinitroso two ammino platinum (II) [Pt (NH that use in a kind of cyanideless electro-plating platinum plating process
3)
2(NO
2)
2] synthetic method.
Background technology
Dinitroso two ammino platinum (II) [Pt (NH
3)
2(NO
2)
2], be commonly called as P salt, be mainly used in the platinum plating in cyanideless electro-plating, gained coating hardness is high, resistance is little, can weld; Electronic devices and components surface platinum plating.Main synthetic method be by metal platinum with making Platinic chloride after aqua regia dissolution, generate potassium platinichloride precipitation reacting with Klorvess Liquid.Potassium platinichloride is precipitated to water and stir into pasty state, be placed in sand bath and heat.Sodium nitrite solution is joined in the mashed prod of potassium platinichloride, continue to be heated to 105 ℃, obtain yellow-green soln.Cooling, filter.Filtrate packs in vial, adds ammoniacal liquor, will after the sedimentation and filtration recrystallization of generation, obtain product.The main problem of the method is containing more inorganic salt, even if also more difficult removing of recrystallization affects the quality of product.
Patent (application number: method 201110157620.2) is that employing metal platinum is raw material, react and prepare Platinic chloride with chloroazotic acid, hydrazine hydrochloride is that reductive agent reduction Platinic chloride is potassium chloroplatinite, the method that utilization is treated different things alike is prepared dichloro four ammonia platinum (II), follows with excessive Sodium Nitrite and reacts and obtain dinitroso two ammino platinum (II).The method can reduce the inorganic salt content in product effectively, but will under the condition of boiling, add excess of ammonia water in the process of synthetic dichloro four ammonia platinum, larger on the impact of human body and environment.
Summary of the invention
The object of the invention is to provide dinitroso two ammino platinum (II) preparation methods that a kind of product yield is high, with short production cycle, be applicable to scale operation and the free inorganic salt of effective control.
Dinitroso two ammino platinum (II) preparation methods of the present invention, the cis-diiodo--bis-ammino platinum (II) of take is starting raw material.Added a certain amount of purified water to stir and be heated to approximately 50～60 ℃ after with Mercury protonitrate by amount of substance ratio, be 1: 0.98～1, liquor capacity is 1mol cis-diiodo--bis-ammino platinum (II): 300～600ml purified water, react 3～7 hours, after filtering precipitation, obtain pale yellow solution.By sodium nitrite solution, by cis-diiodo--bis-ammino platinum (II), be 1: 2～4 with the ratio of the amount of substance of Sodium Nitrite, temperature of reaction is room temperature, reaction times is to react with hydrating solution for 2～7 hours, and the solid filtering obtaining is dried and obtained dinitroso two ammino platinum (II) solids.
Reaction scheme of the present invention is as follows:
Embodiment
Reagent and material that invention adopts:
Cis-diiodo--bis-ammino platinum (II) (NH
3)
2ptI
2molecular weight 483, adopts K
2ptCl
4be dissolved in suitable quantity of water, add excessive analytical pure KI, after 30min, add proper ammonia, after 2 hours, filter the yellow mercury oxide settling out, difference water, washing with alcohol, 70 ℃ are dry, obtain (NH
3)
2ptI
2product, purity>=98%.All the other reagent are domestic analytical pure.
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 4.83 grams of cis-diiodo--bis-ammino platinum (II), add a small amount of purified water to stir, adding 5.60 grams of Mercury protonitrate solution, supplement purified water to 400 milliliter, in the time of approximately 50 ℃, lucifuge reaction is 5 hours, filters and obtains light yellow clear solution 1.
Take 1.52 grams of Sodium Nitrites, after dissolving, under room temperature lucifuge agitation condition, be added drop-wise in light yellow clear solution 1 by purified water, react after 6 hours the sedimentation and filtration obtaining, water, dehydrated alcohol are respectively washed 3 times and are dryly afterwards obtained 2.6 grams of light yellow solids.
In compound, the content of platinum is 60.5% after testing, and ammonia solvent experiment is qualified, and Hg ion content is less than 5ppm.
Embodiment 2:
Take 4.83 grams of cis-diiodo--bis-ammino platinum (II), add a small amount of purified water to stir, adding 5.60 grams of Mercury protonitrate solution, supplement purified water to 450 milliliter, in the time of approximately 60 ℃, lucifuge reaction is 6 hours, filters and obtains light yellow clear solution 1.
Take 1.66 grams of Sodium Nitrites, after dissolving, under room temperature lucifuge agitation condition, be added drop-wise in light yellow clear solution 1 by purified water, react after 6 hours the sedimentation and filtration obtaining, water, dehydrated alcohol are respectively washed 3 times and are dryly afterwards obtained 2.7 grams of light yellow solids.
In compound, the content of platinum is 60.41% after testing, and ammonia solvent experiment is qualified, and Hg ion content is less than 5ppm.
Embodiment 3:
Take 4.83 grams of cis-diiodo--bis-ammino platinum (II), add a small amount of purified water to stir, adding 5.60 grams of Mercury protonitrate solution, supplement purified water to 350 milliliter, in the time of approximately 60 ℃, lucifuge reaction is 5 hours, filters and obtains light yellow clear solution 1.
Take 2.1 grams of Sodium Nitrites, after dissolving, under room temperature lucifuge agitation condition, be added drop-wise in light yellow clear solution 1 by purified water, react after 6 hours the sedimentation and filtration obtaining, water, dehydrated alcohol are respectively washed 3 times and are dryly afterwards obtained 2.7 grams of light yellow solids.
In compound, the content of platinum is 60.5% after testing, and ammonia solvent experiment is qualified, and Hg ion content is less than 5ppm.
Claims (2)
1. a preparation method for dinitroso two ammino platinum (II), is characterized in that comprising the steps:
Adopting cis-diiodo--bis-ammino platinum (II) is starting raw material, with after Mercury protonitrate hydrolysis, hydrating solution is reacted with Sodium Nitrite and obtain dinitroso two ammino platinum (II), cis-diiodo--bis-ammino platinum (II) is 1:0.98 ~ 1 with the ratio of the amount of substance of Mercury protonitrate, temperature of reaction is between 50 ~ 60 ℃, liquor capacity is 1mol cis-diiodo--bis-ammino platinum (II): 300 ~ 600ml purified water, reaction times is 3 ~ 7 hours, cis-diiodo--bis-ammino platinum (II) is 1:2 ~ 4 with the ratio of the amount of substance of Sodium Nitrite, temperature of reaction is room temperature, reaction times is 2 ~ 7 hours.
2. the preparation method of dinitroso two ammino platinum (II) according to claim 1, is characterized in that: reaction process is all carried out under lucifuge condition.
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| CN201210099447.XA CN102583589B (en) | 2012-04-07 | 2012-04-07 | New method for synthesizing dinitroso diammineplatinum (II) |
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| CN115650321A (en) * | 2022-09-19 | 2023-01-31 | 山东有研国晶辉新材料有限公司 | Preparation method of cis-dinitrosoplatinum |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101234788A (en) * | 2008-02-05 | 2008-08-06 | 昆明贵研药业有限公司 | Method for synthesizing antineoplastic medicine cisplatin |
| CN102285693A (en) * | 2011-06-13 | 2011-12-21 | 陕西瑞科新材料股份有限公司 | Preparation method of dinitroso diammineplatinum |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101234788A (en) * | 2008-02-05 | 2008-08-06 | 昆明贵研药业有限公司 | Method for synthesizing antineoplastic medicine cisplatin |
| CN102285693A (en) * | 2011-06-13 | 2011-12-21 | 陕西瑞科新材料股份有限公司 | Preparation method of dinitroso diammineplatinum |
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