JP2986248B2 - Method for producing tetraammineplatinum dichloride solution - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention relates to a tetraammineplatinum (I
I) The present invention relates to a method for producing dichloride (hereinafter referred to as “TAPtDC”).

[0002]

2. Description of the Related Art Conventionally, as a method for producing TAPtDC, hydrazine hydrochloride is added to a chloroplatinic (IV) acid solution to reduce platinum bivalently, and then the solution is divided into two equal parts, and ammonia is added to one side. After adding water and heating to effect ammination, the mixture was heated to remove excess ammonia, and the remaining solution divided into two equal portions was added thereto to form a precipitate of Magnus salt, which was then separated by filtration. This is a method for preparing a tetraammineplatinum (II) dichloride solution by adding hydrochloric acid and aqueous ammonia and dissolving the mixture, followed by heating.

[0003]

SUMMARY OF THE INVENTION The present invention has been made to solve the above-mentioned drawbacks of the conventional method.
It is an object of the present invention to provide a method capable of producing APtDC.

[0004]

DISCLOSURE OF THE INVENTION The present invention provides platinum (IV) chloride.
After reducing the acid solution with hydrazine, add ammonia water and heat under pressure to react, then add water to the reacted solution, heat and filter any precipitate, if any, and heat the filtrate. A method for producing a tetraammineplatinum dichloride solution, characterized by removing excess ammonia.

Hereinafter, the present invention will be described in detail. The concentration of the chloroplatinic (IV) acid solution is not particularly limited, but from the viewpoint of workability, the platinum concentration is 50 to 150 g / l.
And a solution containing a small excess of hydrochloric acid. When a hydrazine dihydrochloride solution (prepared to a concentration of about 200 g / l) is added little by little to the chloroplatinic (IV) acid solution while stirring the equivalent amount of the reaction while stirring, the red-brown color of the solution changes to red-black. . Hydrazine dihydrochloride is used as hydrazine because impurities do not remain in the target TAPtDC solution.

Then, ammonia water is added and the reaction is carried out under pressure to carry out an amminating reaction. For example, the pressure is 1 to 2.5 kg / cm ² and the heating temperature is 1 in an autoclave.
The reaction is carried out at about 20 ° C. for about 15 hours. At this time, the ammonia water to be added is about 28% and the reaction equivalent of 1.5%
It is better to add up to 2.5 times.

After reacting under pressure, about 95
The precipitate was separated by filtration by heating at a temperature of 70 ° C. and a precipitate was separated by filtration, and a resin (Mitsubishi Kasei Kogyo: Styrene-
A small amount of divinylbenzene (HP20) is added thereto, and the mixture is stirred and treated, and then filtered to separate the resin.
Heat at 00 ° C. with stirring to remove excess ammonia. Completion of the ammonia removal may be performed when the pH of the solution becomes about 7.

[0008] A TAPtDC solution can be obtained by the method described above, but it is sufficient to remove excess ammonia and then filter if a precipitate exists in the solution. Hereinafter, examples of the present invention will be described, but the examples do not limit the present invention.

[0009]

EXAMPLE A chloroplatinic acid solution (100 g / Pt)
250 ml containing 0.1 g / l of excess hydrochloric acid)
A solution obtained by dissolving 6.72 g of hydrazine dihydrochloride in 30 ml of pure water was added little by little to reduce platinum to divalent.
Heating was performed on a hot water bath at 0 ° C. until foaming disappeared. Next, the solution was filtered, the filtrate was placed in an autoclave, 126 ml of aqueous ammonia (29%) was added, and the mixture was heated with stirring to a pressure of 1 to 2.5 kg / cm ^{2 and} a heating temperature of 12 kg / cm ^2.
The reaction was carried out at about 0 ° C. for 17 hours. Next, the reacted solution was taken out, 100 ml of pure water was added, the mixture was heated at 95 ° C. in a hot water bath, and then filtered.
20 g of P20) was added, and the mixture was stirred for 10 minutes, allowed to stand for about 1 hour, and then filtered. The filtrate was heated at 95 ° C. for 3 hours on a hot water bath to reach pH 7, and the heating was stopped. A yellow solution was obtained. Analysis of the solution revealed that the desired T
It was confirmed that this was an APtDC solution. It took two days to produce a TAPtDC solution by this production method.

[0010]

Conventional example: Chloroplatinic (IV) acid solution (100 g / Pt /
250 ml containing 0.1 g / l of excess hydrochloric acid)
Then, a solution obtained by dissolving 6.72 g of hydrazine dihydrochloride in 30 ml of pure water was added little by little, and platinum was reduced to divalent. Then, the solution was divided into two equal parts, and ammonia water (28%) was added to one of them.
Was added when the color of the solution became colorless and transparent, and the remaining two solutions were added to form a precipitate of Magnus salt, and the precipitate was separated by filtration.
and 900 ml of aqueous ammonia (28%) were added, and the mixture was heated to 95 ° C. on a hot water bath with stirring and maintained for 1 hour, and TAP was added.
A tDC solution was prepared. It took 14 days to perform this operation.

[0011]

As is clear from the above description, according to the method of the present invention, the time required for manufacturing can be reduced to 1/7 of the conventional method by an extremely simple method.
The fact that the TAPtDC solution using expensive platinum as a raw material can be produced in a short time can be said to be economically effective.

Claims (1)

(57) [Claims] After reducing a chloroplatinic (IV) acid solution with hydrazine, ammonia water is added thereto, and the mixture is heated and reacted under pressure. Then, water is added to the reacted solution and heated to remove precipitates. A method for producing a tetraammineplatinum dichloride solution, which comprises filtering the filtrate and heating the filtrate to remove excess ammonia.