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Preparation method for potassium chloroplatinite

A technology of potassium chloroplatinite and chloroplatinic acid, applied in chemical instruments and methods, ruthenium/rhodium/palladium/osmium/iridium/platinum compounds, inorganic chemistry, etc., can solve the problem of incomplete reduction of platinum and repeatability of reduction process. Not good, incomplete restoration and other problems, to achieve the effect of enhancing the restoration ability

Active Publication Date: 2019-05-17
XIAN CATALYST NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In the above 4 kinds of methods for preparing potassium chloroplatinite, CN101279772A, CN102774894A and CN103253718B all have the problem of incomplete reduction in the reduction process, thereby affecting the product purity of potassium chloroplatinite. CN102390874A reduces chloroplatinic acid solution with oxalic acid, due to chlorine The acidity of the platinum acid solution is difficult to be strictly controlled, the reduction process is not repeatable, and the phenomenon of incomplete platinum reduction is prone to occur, which affects the purity of potassium chloroplatinite.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The present embodiment prepares the method for potassium chloroplatinite, comprises the following steps:

[0032] Step 1, dissolving 85g platinum sponge with aqua regia, filtering after concentrating and catching up with nitrate, diluting the filtrate obtained by filtering with water, obtaining a chloroplatinic acid solution with a mass content of platinum of 20%;

[0033] Step 2. Add the chloroplatinic acid solution described in step 1 dropwise to a potassium chloride solution containing 93.5g KCl with a mass concentration of 15%, react at 70°C for 2h and no longer precipitate, cool to room temperature and filter ;

[0034] Step 3. Wash the filtered precipitate in step 2 with a potassium chloride solution having a mass concentration of 2% until the filtrate is neutral, then rinse the washed precipitate with ethanol, and dry at 70° C. to obtain 207.8 g of potassium chloroplatinate;

[0035] Step 4. Mix 1 L of deionized water and 200 g of potassium chloroplatinate descr...

Embodiment 2

[0039] The present embodiment prepares the method for potassium chloroplatinite, comprises the following steps:

[0040] Step 1, dissolving 85g platinum sponge with aqua regia, filtering after concentrating and catching up with nitrate, diluting the filtrate obtained by filtering with water, obtaining a chloroplatinic acid solution with a mass content of platinum of 15%;

[0041] Step 2, adding the chloroplatinic acid solution described in step 1 dropwise to a potassium chloride solution containing 102 g of KCl at a mass concentration of 20%, reacting at 50° C. for 3 h and no precipitation of the precipitate, cooling and filtering;

[0042] Step 3. Wash the filtered precipitate in step 2 with a potassium chloride solution having a mass concentration of 3% until the filtrate is neutral, then rinse the washed precipitate with ethanol, and dry at 75° C. to obtain 209.3 g of potassium chloroplatinate;

[0043] Step 4. Mix 1.4L of deionized water and 200g of potassium chloroplatina...

Embodiment 3

[0047] The present embodiment prepares the method for potassium chloroplatinite, comprises the following steps:

[0048] Step 1, dissolving 85g platinum sponge with aqua regia, filtering after concentrating and catching up with nitrate, diluting the filtrate obtained by filtering with water, obtaining a chloroplatinic acid solution with a mass content of platinum of 25%;

[0049] Step 2. Add the chloroplatinic acid solution described in step 1 dropwise to a 10% potassium chloride solution containing 97.5g KCl in mass concentration, react at 65°C for 2.5h and the precipitate will no longer separate out. After cooling to room temperature filter;

[0050] Step 3. Wash the filtered precipitate in step 2 with a potassium chloride solution having a mass concentration of 1% until the filtrate is neutral, then rinse the washed precipitate with ethanol, and dry at 80° C. to obtain 207.1 g of potassium chloroplatinate;

[0051] Step 4. Mix 1.3L of deionized water and 200g of potassium ...

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Abstract

The invention discloses a preparation method for potassium chloroplatinite. The preparation method comprises the following steps: 1) dissolving spongy platinum in aqua regia for denitration, thereby acquiring a chloroplatinic acid solution; 2) dropwise adding the chloroplatinic acid solution into a potassium chloride solution and reacting; 3) washing the potassium chloride solution with ethyl alcohol, and then drying, thereby acquiring potassium chloroplatinate; 4) uniformly mixing deionized water and potassium chloroplatinate, thereby forming a turbid liquid; dropwise adding hydroxylamine hydrochloride solution and potassium hydroxide solution in turn; removing platinum black by filtering under a heat state after the ending of reaction, thereby acquiring the potassium chloroplatinite solution; 5) performing rotary evaporation on the potassium chloroplatinite solution, and then cooling and filtering, and vacuum-drying, thereby acquiring solid potassium chloroplatinite. According to theinvention, hydroxylamine hydrochloride is used as a reducing agent for reducing potassium chloroplatinate, potassium hydroxide is used for neutralizing excessive acid in the system, and potassium chloroplatinate is completely reduced to potassium chloroplatinite, so that high-purity potassium chloroplatinite is prepared. The quality purity of the prepared potassium chloroplatinite is more than orequal to 99.5%, potassium chloroplatinate residue is less than or equal to 0.04% and yield is above 92.2%.

Description

technical field [0001] The invention belongs to the technical field of preparation of pharmaceutical intermediates, and in particular relates to a preparation method of potassium chloroplatinite. Background technique [0002] Cancer is currently one of the major diseases that seriously affect human health and threaten human life, so the development of anticancer drugs has become a research hotspot. Since American scientist Rosenberg discovered that cisplatin has the ability to inhibit tumor cell growth in 1967, the research and clinical application of platinum-based drugs in tumor treatment has achieved rapid development. Cisplatin, carboplatin and oxaliplatin have become mature anti-tumor drugs, and the market demand is increasing year by year. The new generation of platinum-based anti-tumor drugs such as leplatin and cycloplatin will further expand the application of platinum-based compounds in anti-tumor treatment. application. [0003] Potassium chloroplatinite is an i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G55/00
Inventor 王昭文潘丽娟王慧闫江梅张磊翟康
Owner XIAN CATALYST NEW MATERIALS CO LTD
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