CN112429785B - Preparation method of analytically pure platinum tetrachloride - Google Patents
Preparation method of analytically pure platinum tetrachloride Download PDFInfo
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- CN112429785B CN112429785B CN202011417786.9A CN202011417786A CN112429785B CN 112429785 B CN112429785 B CN 112429785B CN 202011417786 A CN202011417786 A CN 202011417786A CN 112429785 B CN112429785 B CN 112429785B
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- C01—INORGANIC CHEMISTRY
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- C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
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Abstract
The invention relates to a preparation method of analytically pure platinum tetrachloride, which comprises the following steps of firstly dissolving metal platinum by aqua regia to obtain a metal platinum solution; nitrate radicals in the metal platinum solution are removed by using hydrochloric acid, and then the metal platinum solution is reacted with hydrogen peroxide to prepare chloroplatinic acid solution; and then adding the chloroplatinic acid solution into a vacuum-rotary evaporator, and removing hydrochloric acid in the solution by vacuum rotary evaporation to obtain analytically pure platinum tetrachloride. The invention has advanced process technology, high production efficiency and large yield; chlorine gas does not need to be introduced, and the environmental pollution is small; the produced platinum tetrachloride product has high purity and low impurity content, and the market competitiveness is improved.
Description
Technical Field
The invention relates to the field of inorganic compound preparation methods, and particularly relates to a preparation method of analytically pure platinum tetrachloride.
Background
Platinum tetrachloride is widely applied to the fields of electroplating, catalysts and the like. The existing preparation method of platinum tetrachloride mainly uses metal platinum as a raw material, the metal platinum is heated and reacted with a mixed solution of hydrochloric acid and nitric acid, after the reaction is completed, the solution is filtered and subjected to nitrate removal, the solution is evaporated until crystals are separated out, then the crystals are transferred to a porcelain boat, the temperature is slowly raised to completely volatilize water, the temperature needs to be continuously raised to 275-300 ℃ within 2 hours, the temperature is kept for half an hour, then the temperature is lowered to 150 ℃, the product is taken out and rapidly crushed, then the product is placed in the boat again, the temperature is kept for half an hour after the product is heated to 250 ℃ in chlorine airflow, and the product is put into a sealed bottle while the product is hot to obtain the platinum tetrachloride.
The process for preparing the platinum tetrachloride has the advantages of complex steps, high cost and serious environmental pollution, and the produced platinum tetrachloride has low purity and high impurity content.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provide a preparation method of analytically pure platinum tetrachloride with high purity and low impurity content.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
the invention provides a preparation method of analytically pure platinum tetrachloride, which comprises the following steps: firstly, dissolving metal platinum by aqua regia to obtain a metal platinum solution; nitrate is removed by hydrochloric acid to remove nitrate in the metal platinum solution, and then the metal platinum solution reacts with hydrogen peroxide to prepare chloroplatinic acid solution; and then adding the chloroplatinic acid solution into a vacuum-rotary evaporator, and removing hydrochloric acid in the solution by vacuum rotary evaporation to obtain analytically pure platinum tetrachloride.
Further, the method of the invention comprises the following specific steps:
a) putting metal platinum into the aqua regia, heating to 190-220 ℃, and obtaining a metal platinum solution after the metal platinum is completely dissolved;
b) heating and concentrating the metal platinum solution obtained in the step (a), controlling the temperature of the metal platinum solution to be 150-190 ℃, adding hydrochloric acid to drive nitrate, stirring until no yellow gas is generated, repeating the step for 3 times, and adding hydrogen peroxide to obtain a chloroplatinic acid solution;
c) pouring a chloroplatinic acid solution into a rotary evaporator, starting a vacuum pump to 55-70 KPa, adjusting the rotating speed of the rotary evaporator to 80-120 r/min, firstly adjusting the temperature to 130-170 ℃, keeping the temperature constant for 1-2.5 h, then heating to 200-240 ℃, keeping the temperature constant for 1.5-2.5 h, finally heating to 260-300 ℃, keeping the temperature constant for 0.5-1.5 h, stopping heating, cooling to room temperature, taking out and grinding to obtain analytically pure platinum tetrachloride.
Further, the hydrochloric acid in the step b) is a hydrochloric acid aqueous solution with the mass fraction of 30%, and the addition amount of the nitric acid aqueous solution per kilogram of metal platinum is 300-500 ml per time.
Further, the hydrogen peroxide in the step b) is aqueous hydrogen peroxide with the mass fraction of 30%, and the addition amount of each kilogram of the aqueous hydrogen peroxide containing metal platinum is 30-50 ml.
Further, the metal platinum in the step a) is a reagent with analytical purity and above.
The invention provides a preparation method of analytically pure platinum tetrachloride, which comprises the steps of dissolving metal platinum by aqua regia, removing nitrate by hydrochloric acid solution after complete dissolution until nitrate radical is completely removed to obtain chloroplatinic acid solution, then pouring the chloroplatinic acid solution into a vacuum-rotary evaporator, heating in three stages, carrying out vacuum rotary evaporation until the hydrochloric acid solution is completely removed, and obtaining the analytically pure platinum tetrachloride. Compared with the prior art, the platinum tetrachloride produced by the method has high purity and low impurity content, and through full-element analysis and chemical analysis, the platinum content is 57.8 +/-0.2 percent, the total impurity content is not more than 0.03 percent, the method has advanced process technology, high production efficiency and high yield; chlorine gas does not need to be introduced, and the environmental pollution is small; the produced platinum tetrachloride product has high purity and low impurity content, and the market competitiveness is improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
a) Putting 500g of spongy platinum into a glass beaker, adding a mixed solution of 700ml of concentrated nitric acid (mass fraction of 69%) and 2100ml of concentrated hydrochloric acid (mass fraction of 38%), heating to 190 ℃, and waiting for platinum powder to be completely dissolved;
b) continuously heating and concentrating the volume, slowly adding 200ml of hydrochloric acid aqueous solution (the mass fraction is 30%) into the solution when the temperature of the solution is 170 ℃, stirring until no yellow gas is generated, repeating the steps for 3 times, and adding 20ml of hydrogen peroxide (the mass fraction is 30%) to finally obtain a chloroplatinic acid solution;
c) pouring the chloroplatinic acid solution into a rotary evaporator, starting a vacuum pump, adjusting the pressure of the vacuum pump to 60Kpa, adjusting the rotating speed of the rotary evaporator to 85r/min, adjusting the temperature to 150 ℃, keeping the temperature for 1.5h, then heating to 220 ℃, keeping the temperature for 2h, finally heating to 280 ℃, keeping the temperature for 1h, stopping heating, cooling to room temperature, taking out, and quickly grinding into powder to obtain analytically pure platinum tetrachloride.
The product prepared by the embodiment is a brownish red crystal, is easy to dissolve in water, is clear after dissolution, has no insoluble substances visible to naked eyes, and has the product yield of 99.5 percent. The crystal is sampled for full element analysis and chemical analysis, the platinum content is 57.8 percent, and the total impurity content is less than 0.03 percent.
Example 2
a) Putting 1000g of sponge platinum into a glass beaker, adding a mixed solution of 1400ml of concentrated nitric acid (mass fraction of 69%) and 4200ml of concentrated hydrochloric acid (mass fraction of 38%), heating to 195 ℃, and waiting for platinum powder to be completely dissolved;
b) continuing to heat and concentrate the volume, slowly adding 300ml of hydrochloric acid aqueous solution (the mass fraction is 30%) to the solution when the temperature of the solution is 160 ℃, stirring until no yellow gas is generated, repeating the steps for 3 times, and adding 38ml of hydrogen peroxide (the mass fraction is 30%) to obtain a chloroplatinic acid solution;
c) pouring the chloroplatinic acid solution into a rotary evaporator, starting a vacuum pump, adjusting the pressure of the vacuum pump to be 55Kpa, and adjusting the rotating speed of the rotary evaporator to be 95 r/min. Regulating the temperature to 160 ℃, keeping the temperature constant for 80min, then heating to 200 ℃, keeping the temperature constant for 2.5h, finally heating to 260 ℃, keeping the temperature constant for 80min, stopping heating, cooling to room temperature, taking out, and quickly grinding into powder to obtain analytically pure platinum tetrachloride.
The product prepared by the embodiment is a brownish red crystal, is easy to dissolve in water, is clear after dissolution, and has the product yield of 99.6 percent. The crystal is sampled for full element analysis and chemical analysis, and compounds except platinum tetrachloride are not detected, the platinum content in the product is 57.7 percent, and the total impurity content is less than 0.03 percent.
Example 3
a) Putting 1500g of sponge platinum into a glass beaker, adding a mixed solution of 2100ml of concentrated nitric acid (mass fraction of 69%) and 6300ml of concentrated hydrochloric acid (mass fraction of 38%), heating to 195 ℃, and waiting for platinum powder to be completely dissolved;
b) continuing to heat and concentrate the volume, slowly adding 600ml of 30 mass percent hydrochloric acid aqueous solution (30 mass percent) into the solution when the temperature of the solution is 180 ℃, stirring until no yellow gas is generated, repeating the steps for 3 times, and adding 60ml of hydrogen peroxide (30 mass percent) to obtain chloroplatinic acid solution;
c) pouring the chloroplatinic acid solution into a rotary evaporator, starting a vacuum pump, adjusting the pressure of the vacuum pump to 65Kpa, adjusting the rotating speed of the rotary evaporator to 105r/min, keeping the temperature constant for 1h when the temperature is adjusted to 170 ℃, then heating to 230 ℃ and keeping the temperature constant for 130min, finally heating to 290 ℃ and keeping the temperature constant for 65min, stopping heating, cooling to room temperature, taking out, and quickly grinding into powder to obtain analytically pure platinum tetrachloride.
The product prepared by the embodiment is a brownish red crystal, is easy to dissolve in water, is clear after dissolution, and has the product yield of 99.7 percent. The crystal is sampled for full element analysis and chemical analysis, and compounds except platinum tetrachloride are not detected, the platinum content in the product is 57.7 percent, and the total impurity content is less than 0.03 percent.
The technical idea of the present invention is described in the above technical solutions, and the protection scope of the present invention is not limited thereto, and any changes and modifications made to the above technical solutions according to the technical essence of the present invention belong to the protection scope of the technical solutions of the present invention.
Claims (4)
1. A preparation method of analytically pure platinum tetrachloride is characterized by comprising the following steps: firstly, dissolving metal platinum by aqua regia to obtain a metal platinum solution; nitrate is removed by hydrochloric acid to remove nitrate in the metal platinum solution, and then the metal platinum solution reacts with hydrogen peroxide to prepare chloroplatinic acid solution; then adding the chloroplatinic acid solution into a vacuum-rotary evaporator, and removing hydrochloric acid in the solution by vacuum rotary evaporation to obtain analytically pure platinum tetrachloride; the method comprises the following specific steps:
a) putting metal platinum into aqua regia, heating to 190-220 ℃, and obtaining a metal platinum solution after the metal platinum is completely dissolved;
b) heating and concentrating the metal platinum solution obtained in the step (a), controlling the temperature of the metal platinum solution to be 150-190 ℃, adding hydrochloric acid to drive nitrate, stirring until no yellow gas is generated, repeating the step for 3 times, and adding hydrogen peroxide to obtain a chloroplatinic acid solution;
c) pouring a chloroplatinic acid solution into a rotary evaporator, starting a vacuum pump to 55-70 KPa, adjusting the rotating speed of the rotary evaporator to 80-120 r/min, firstly adjusting the temperature to 130-170 ℃, keeping the temperature constant for 1-2.5 h, then heating to 200-240 ℃, keeping the temperature constant for 1.5-2.5 h, finally heating to 260-300 ℃, keeping the temperature constant for 0.5-1.5 h, stopping heating, cooling to room temperature, taking out and grinding to obtain analytically pure platinum tetrachloride; the platinum tetrachloride content is 57.8 +/-0.2%, and the total impurity content is not more than 0.03%.
2. The method as claimed in claim 1, wherein the hydrochloric acid in step b) is 30% aqueous hydrochloric acid, and the amount of the aqueous hydrochloric acid solution added per kilogram of metal platinum is 300-500 ml.
3. The method according to claim 1, wherein the hydrogen peroxide in step b) is 30% by weight aqueous hydrogen peroxide, and the amount of the hydrogen peroxide added is 30-50 ml per kg of the aqueous metal platinum hydrogen peroxide.
4. The method of claim 1, wherein the platinum metal in step a) is an analytically pure or higher purity reagent.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH0559076A (en) * | 1991-09-04 | 1993-03-09 | Tanaka Kikinzoku Kogyo Kk | Production of platinum compound |
| 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 |
| CN102030378A (en) * | 2009-09-28 | 2011-04-27 | 天津市化学试剂研究所 | Method for preparing pure light spectrum platinum tetrachloride |
| DE102013203743A1 (en) * | 2013-03-05 | 2014-09-11 | Heraeus Precious Metals Gmbh & Co. Kg | Process for the preparation of high purity platinum powder and platinum powder obtainable by this process and use |
| CN107176625A (en) * | 2017-04-19 | 2017-09-19 | 乐山东承新材料有限公司 | A kind of production method of the ammonia palladium of sulfuric acid four |
| TWI667202B (en) * | 2018-12-07 | 2019-08-01 | 鑫鼎奈米科技股份有限公司 | Method of making inorganic platinum compound |
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