CN102285693A - Preparation method of dinitroso diammineplatinum - Google Patents
Preparation method of dinitroso diammineplatinum Download PDFInfo
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- CN102285693A CN102285693A CN2011101576202A CN201110157620A CN102285693A CN 102285693 A CN102285693 A CN 102285693A CN 2011101576202 A CN2011101576202 A CN 2011101576202A CN 201110157620 A CN201110157620 A CN 201110157620A CN 102285693 A CN102285693 A CN 102285693A
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Abstract
The invention discloses a preparation method of a noble metal compound dinitroso diammineplatinum [Pt(NH3)2(NO2)2] which is used in the platinum plating process with a cyanogen-free electroplating method. The preparation method comprises the following steps: reacting metal platinum used as a raw material with aqua regia to prepare chloroplatinic acid; reducing chloroplatinic acid into chloroplatinous acid with hydrazine hydrochloride as a reducer; and preparing dichlorotetraammineplatinum by utilizing a one-pot method, and subsequently reacting dichlorotetraammineplatinum with excess sodium nitrite so as to obtain dinitroso diammineplatinum. According to the preparation method disclosed by the invention, chloroplatinic acid is precisely reduced into chloroplatinous acid, and dichlorotetraammineplatinum is prepared by using the one-pot method and then further reacts with sodium nitrite so as to prepare P salt (dinitroso diammineplatinum), thereby effectively solving the problem that the content of potassium ion in the P salt is too large in the traditional preparation method. According to the invention, the element analysis result of the P salt prepared by using the preparation method is basically in conformity with a theoretical value; and the P salt dose not contain the potassium ion, and the contents of sodium ion and chlorine ion in the P salt are less than 50PPM.
Description
Technical field:
The present invention relates to the preparation method of the precious metal chemical complex dinitroso diammonia platinum [Pt (NH3) 2 (NO2) 2] that uses in a kind of cyanideless electro-plating platinum plating process.
Background technology:
Dinitroso diammonia platinum [Pt (NH3) 2 (NO2) 2] is commonly called as P salt, mainly is used in the platinum plating in the cyanideless electro-plating, and gained coating hardness height, resistance are little, can weld; Electronic devices and components surface platinum plating.Common preparation method is: the metal platinum aqua regia dissolution prepares Platinic chloride, Platinic chloride and Repone K are made into 10% solution respectively, with the platinum acid chloride solution heating, under agitation add Klorvess Liquid then, generate the potassium platinichloride precipitation this moment, potassium platinichloride water furnishing pasty state, in sand bath, heat, add the solution of 40% Sodium Nitrite, when temperature reaches 90 ℃, begin to separate out nitrogen peroxide, temperature is controlled at 105 ℃ until reacting completely, and obtains yellow-green soln.Cooling back adding ammoniacal liquor (25%) bottling also shakes up the bottleneck jam-pack, places spend the night back suction filtration and wash crystallization several, uses the boiling water recrystallize then, promptly gets P salt after draining.The P salt that this method makes, potassium content is bigger, and can't remove by the method for washing and hot water recrystallization, and under the situation that galvanization coating is had relatively high expectations, to the stress influence maximum of coating, electroplating effect is undesirable.
Summary of the invention:
The present invention is directed to the deficiency that prior art exists, propose a kind of preparation method of dinitroso diammonia platinum of simple no potassium ion.
The present invention includes following steps: the employing metal platinum is a raw material, with chloroazotic acid prepared in reaction Platinic chloride, with the hydrazine hydrochloride is that reductive agent reduction Platinic chloride is a chloro-platinous acid, the method that utilization is treated different things alike prepares dichloro four ammino platinum, and then dichloro four ammino platinum react with excessive Sodium Nitrite and obtain dinitroso diammonia platinum.
The preparation process of described platinum acid chloride solution is with metal platinum and chloroazotic acid reaction, and reaction stops back adding concentrated hydrochloric acid and catches up with nitre to system not have brown gas generation, changes Rotary Evaporators then over to and is concentrated into anhydrous steaming, and adds suitable quantity of water and makes that Platinic chloride concentration is 200-300g/L.
The preparation process of described chloro-platinous acid is to be that the hydrazine hydrochloride drips of solution of 30%-40% is added in the platinum acid chloride solution with concentration, and add-on adds in the ratio of Platinic chloride and hydrazine hydrochloride mol ratio 1.5-2.5, filters not tolerant.
The preparation process of described dichloro four ammino platinum is that chloro-platinous acid solution is heated to boiling, doubly measures the ebullient strong aqua to wherein adding 5-10, and it is colourless that final solution is, and concentration and evaporation is separated out dichloro four ammino platinum white crystals.
The add-on of described Sodium Nitrite adds the Sodium Nitrite saturated solution in the ratio that 1g dichloro four ammino platinum add the 0.5-2g Sodium Nitrite.
The concentration of described hydrazine hydrochloride is preferred 35%, and the mol ratio of Platinic chloride and hydrazine hydrochloride is preferably 2.0.
The best adding of described ammoniacal liquor and chloro-platinous acid mol ratio is 10.
The optimal addn of described Sodium Nitrite adds in the ratio that 1g dichloro four ammino platinum add the 0.6g Sodium Nitrite.
The present invention accurately is reduced to chloro-platinous acid with Platinic chloride, and the method for the treatment of different things alike is prepared dichloro four ammonia platinum then, further with Sodium Nitrite prepared in reaction P salt, efficiently solves the excessive problem of P salt potassium content in the traditional preparation process method.Adopt the ultimate analysis of P salt and the theoretical value basically identical of the present invention's preparation, do not contain potassium ion, and sodium ion and chloride ion content all are lower than 50PPM.
Adopt the dinitroso diammonia platinum (P salt) [Pt (NH3) 2 (NO2) 2] of the present invention's preparation to test through ICP, platinum content is 59.7 ± 0.2%, and sodium ion is 15ppm, and potassium ion does not detect, chlorion is 10ppm, and the total content of other metal ions is no more than 50ppm.
Embodiment:
A) preparation of Platinic chloride: take by weighing a certain amount of metal platinum, put into beaker after cleaning, add an amount of chloroazotic acid, suitably heating starting reaction, reaction is advisable with the even bubbling of solution.Reaction stops to add hydrochloric acid and catches up with nitre, emerges to no longer including brown gas, changes Rotary Evaporators over to, is concentrated into anhydrous steaming, and transfers to add suitable quantity of water in the beaker to be mixed with concentration be the 200-300g/L platinum acid chloride solution.
B) chloro-platinous acid is synthetic: hydrazine hydrochloride is that reductive agent reduction Platinic chloride prepares chloro-platinous acid, its process is to be that the hydrazine hydrochloride drips of solution of 30%-40% is added in the platinum acid chloride solution with concentration, add-on adds in the ratio of Platinic chloride and hydrazine hydrochloride mol ratio 1.5-2.5, filter not tolerantly, obtain scarlet chloro-platinous acid solution.
C) preparation of dichloro four ammino platinum: chloro-platinous acid solution is heated to boiling, and to wherein adding excessive ebullient strong aqua, it is colourless that final solution is, and evaporation concentration is separated out dichloro four ammino platinum white crystals.
D) take by weighing a certain amount of dichloro four ammino platinum, the ratio that adds the 0.5-2g Sodium Nitrite in 1g dichloro four ammino platinum adds the Sodium Nitrite saturated solution, and mixture is heated to the aureus precipitation and changes into colourlessly in water-bath, and cooling crystallization filters the hot water recrystallization.Sample thief carries out icp analysis.
The concentration of hydrazine hydrochloride of the present invention is preferred 35%, and the mol ratio of Platinic chloride and hydrazine hydrochloride is preferably 2.0.
The best adding of ammoniacal liquor of the present invention and chloro-platinous acid mol ratio is 10.
The optimal addn of Sodium Nitrite of the present invention adds in the ratio that 1g dichloro four ammino platinum add the 0.6g Sodium Nitrite.
Embodiment 1: takes by weighing the 195g metal platinum, puts into beaker after cleaning, add an amount of chloroazotic acid, and suitably heating starting reaction, reaction is advisable with the even bubbling of solution.Reaction stops to add hydrochloric acid and catches up with nitre, emerges to no longer including brown gas, changes Rotary Evaporators over to, is concentrated into anhydrous steaming, and transfers to add suitable quantity of water in the beaker to be mixed with concentration be the 200g/L platinum acid chloride solution.
Take by weighing the 52.5g hydrazine hydrochloride, be mixed with 35% deionized water solution, be added drop-wise in the above-mentioned platinum acid chloride solution, obtain the chloro-platinous acid solution of scarlet.
Chloro-platinous acid solution is heated to the ammoniacal liquor that the boiling back adds 10 times of molar weights of ebullient, is heated to final solution and is colourless, evaporation concentration is separated out white dichloro four ammino platinum 345.2g.
The deionized water 3L that adds heat then adds the saturated solution that contains the 204g Sodium Nitrite, and mixture is heated to yellow mercury oxide and is converted into colourlessly in water-bath, and cooling crystallization filters the hot water recrystallization, P salt 256g, yield 80.1%.
Embodiment 2: takes by weighing the 390g metal platinum, puts into beaker after cleaning, add an amount of chloroazotic acid, and suitably heating starting reaction, reaction is advisable with the even bubbling of solution.Reaction stops to add hydrochloric acid and catches up with nitre, emerges to no longer including brown gas, changes Rotary Evaporators over to, is concentrated into anhydrous steaming, and transfers to add suitable quantity of water in the beaker to be mixed with concentration be the 200g/L platinum acid chloride solution.
Take by weighing the 105g hydrazine hydrochloride, be mixed with 35% deionized water solution, be added drop-wise in the above-mentioned platinum acid chloride solution, obtain the chloro-platinous acid solution of scarlet.
Chloro-platinous acid solution is heated to the ammoniacal liquor that boiling adds 10 times of molar weights of ebullient, is heated to final solution and is colourless, evaporation concentration is separated out white dichloro four ammino platinum 685.3g
The deionized water 3L that adds heat then adds the saturated solution that contains the 204g Sodium Nitrite, and mixture is heated to yellow mercury oxide and is converted into colourlessly in water-bath, and cooling crystallization filters the hot water recrystallization, P salt 521.6g, yield 83.4%.
Claims (8)
1. the preparation method of the precious metal chemical complex dinitroso diammonia platinum that uses in the cyanideless electro-plating platinum plating process, it is characterized in that it is raw material that described method comprises the steps: to adopt metal platinum, with chloroazotic acid prepared in reaction Platinic chloride, with the hydrazine hydrochloride is that reductive agent reduction Platinic chloride is a chloro-platinous acid, the method that utilization is treated different things alike prepares dichloro four ammino platinum, and then dichloro four ammino platinum react with excessive Sodium Nitrite and obtain dinitroso diammonia platinum.
2. the preparation method of dinitroso diammonia platinum according to claim 1, it is characterized in that: the preparation process of described platinum acid chloride solution is with metal platinum and chloroazotic acid reaction, reaction stops back adding concentrated hydrochloric acid and catches up with nitre to system not have brown gas generation, change Rotary Evaporators then over to and be concentrated into anhydrous steaming, add suitable quantity of water and make that Platinic chloride concentration is 200-300g/L.
3. the preparation method of dinitroso diammonia platinum according to claim 1, it is characterized in that: the preparation process of described chloro-platinous acid is to be that the hydrazine hydrochloride drips of solution of 30%-40% is added in the platinum acid chloride solution with concentration, add-on adds in the ratio of Platinic chloride and hydrazine hydrochloride mol ratio 1.5-2.5, filters not tolerant.
4. the preparation method of dinitroso diammonia platinum according to claim 1, it is characterized in that: the preparation process of described dichloro four ammino platinum is that chloro-platinous acid solution is heated to boiling, doubly measure the ebullient strong aqua to wherein adding 5-10, it is colourless that final solution is, concentration and evaporation is separated out dichloro four ammino platinum white crystals.
5. the preparation method of dinitroso diammonia platinum according to claim 1 is characterized in that: the add-on of described Sodium Nitrite adds the Sodium Nitrite saturated solution in the ratio that 1g dichloro four ammino platinum add the 0.5-2g Sodium Nitrite.
6. the preparation method of dinitroso diammonia platinum according to claim 3 is characterized in that: the concentration of described hydrazine hydrochloride is preferred 35%, and the mol ratio of Platinic chloride and hydrazine hydrochloride is preferably 2.0.
7. the preparation method of dinitroso diammonia platinum according to claim 4 is characterized in that: described ammoniacal liquor and chloro-platinous acid be best, and to add mol ratio be 10.
8. the preparation method of dinitroso diammonia platinum according to claim 5 is characterized in that: the optimal addn of described Sodium Nitrite adds in the ratio that 1g dichloro four ammino platinum add the 0.6g Sodium Nitrite.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583589A (en) * | 2012-04-07 | 2012-07-18 | 昆明贵研药业有限公司 | New method for synthesizing dinitroso diammineplatinum (II) |
| CN102766169A (en) * | 2012-08-01 | 2012-11-07 | 昆明贵研药业有限公司 | New method for synthesizing anti-tumor drug miboplatin |
| CN113979490A (en) * | 2021-11-17 | 2022-01-28 | 西安科技大学 | Method for hydrothermal preparation of dinitroso diammineplatinum with cubic structure and application |
| CN114057242A (en) * | 2021-11-17 | 2022-02-18 | 西安科技大学 | Method for preparing spherical dinitroso diammine platinum by hydrothermal method and application |
| CN114436348A (en) * | 2021-12-31 | 2022-05-06 | 励福(江门)环保科技股份有限公司 | Synthetic method of platinum salt electroplated dinitroso diammine platinum |
| CN114456214A (en) * | 2021-11-18 | 2022-05-10 | 浙江微通催化新材料有限公司 | Preparation method of cis-bis (benzonitrile) platinum dichloride |
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| JPH01308836A (en) * | 1988-06-08 | 1989-12-13 | Tanaka Kikinzoku Kogyo Kk | Production of tetrammineplatinum(ii) chloride |
| CN101279772A (en) * | 2008-05-15 | 2008-10-08 | 金川集团有限公司 | Preparation of potassium platinochloride |
| CN101367557A (en) * | 2008-09-25 | 2009-02-18 | 昆明贵金属研究所 | Novel method for synthesis of tetrammine platinum hydrogen nitrate (II) |
| CN101987748A (en) * | 2009-08-04 | 2011-03-23 | 天津市化学试剂研究所 | Preparation method of analytically pure chloroplatinic acid |
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2011
- 2011-06-13 CN CN2011101576202A patent/CN102285693A/en active Pending
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| US4831009A (en) * | 1987-03-30 | 1989-05-16 | W. R. Grace & Co.-Conn. | Method of applying a catalyst to a support |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583589A (en) * | 2012-04-07 | 2012-07-18 | 昆明贵研药业有限公司 | New method for synthesizing dinitroso diammineplatinum (II) |
| CN102583589B (en) * | 2012-04-07 | 2014-01-15 | 昆明贵研药业有限公司 | New method for synthesizing dinitroso diammineplatinum (II) |
| CN102766169A (en) * | 2012-08-01 | 2012-11-07 | 昆明贵研药业有限公司 | New method for synthesizing anti-tumor drug miboplatin |
| CN102766169B (en) * | 2012-08-01 | 2015-04-22 | 昆明贵研药业有限公司 | New method for synthesizing anti-tumor drug miboplatin |
| CN113979490A (en) * | 2021-11-17 | 2022-01-28 | 西安科技大学 | Method for hydrothermal preparation of dinitroso diammineplatinum with cubic structure and application |
| CN114057242A (en) * | 2021-11-17 | 2022-02-18 | 西安科技大学 | Method for preparing spherical dinitroso diammine platinum by hydrothermal method and application |
| CN114456214A (en) * | 2021-11-18 | 2022-05-10 | 浙江微通催化新材料有限公司 | Preparation method of cis-bis (benzonitrile) platinum dichloride |
| CN114436348A (en) * | 2021-12-31 | 2022-05-06 | 励福(江门)环保科技股份有限公司 | Synthetic method of platinum salt electroplated dinitroso diammine platinum |
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Application publication date: 20111221 |