CN103253718A - Preparation method of potassium chloroplatinite - Google Patents
Preparation method of potassium chloroplatinite Download PDFInfo
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- CN103253718A CN103253718A CN2013101996299A CN201310199629A CN103253718A CN 103253718 A CN103253718 A CN 103253718A CN 2013101996299 A CN2013101996299 A CN 2013101996299A CN 201310199629 A CN201310199629 A CN 201310199629A CN 103253718 A CN103253718 A CN 103253718A
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Abstract
The invention relates to a preparation method of potassium chloroplatinite. The preparation method mainly comprises the following steps of: dissolving platinum with aqua regia; removing nitre and acid; adding potassium chloride; filtering to obtain potassium chloroplatinate precipitate; adding reductant solution; jointly processing by utilizing 200mW/cm<2> cosine ultrasonic wave under 20 to 25kHz and 200mW/cm<2> variable frequency ultrasonic wave under 35 to 40kHz, and continuously stirring at the same time, thus obtaining potassium chloroplatinite solution. According to the preparation method of the potassium chloroplatinite, the specific ultrasonic cavitation effect is utilized to promote the reaction process of reducing potassium chloroplatinate through potassium formate, thus the reaction time is shortened, the reaction is complete, and the yield of potassium chloroplatinite is increased.
Description
Technical field
The invention belongs to the synthetic field of mineral compound, be specifically related to a kind of under the ultrasonic wave condition method of efficient production potassium chloroplatinite.
Background technology
Cancer is that current serious influences human health, threatens one of principal disease of human life; It constitutes the world today's three big causes of death with cardiovascular and cerebrovascular diseases and mishap.Therefore, each state all classifies capture cancer as a top priority as, and the research of cancer therapy drug becomes the focus of drug development.
Barnett Rosenberg chanced on cis-platinum in 1969 and has the inhibition cel l proliferation, thereby had excited the concern of people to metal complexes antitumor action and mechanism.Nowadays, platinum series antineoplastic medicament is widely used in the clinical treatment of tumour, and evident in efficacy to kinds of tumors, now progressively forms the market medication system based on first-generation cis-platinum, s-generation carboplatin and third generation oxaliplatin.The action target spot of above-mentioned platinum series antineoplastic medicament mainly is DNA, can destroy copying of DNA and suppress the growth that cell fission waits to suppress tumour cell by crosslinked in the formation DNA chain, interchain linkage, DNA-protein cross, plays antineoplastic action.
Potassium chloroplatinite is the important intermediate of platinum compound medicines such as preparation above-mentioned cis-platinum, carboplatin and oxaliplatin, along with the making earnest efforts the research platinum compound of people in recent years, also feasible research to potassium chloroplatinite becomes focus, on the other hand, potassium chloroplatinite is owing to the platinum source that also is used as the platinum catalyst preparation is paid close attention to widely.
The preparation method who openly prepares at present potassium chloroplatinite is as follows:
Chinese patent CN102774894A discloses a kind of preparation method of potassium chloroplatinite, the route of employing: the conventional preparation of spongy platinum Platinic chloride---the oxalic acid reduction generates chloro-platinous acid---adds Repone K and generates potassium chloroplatinite.
Chinese patent CN101279772B discloses a kind of preparation method of potassium chloroplatinite, is that metal platinum adopts conventional path of preparing Platinic chloride---add Repone K and prepare potassium platinichloride---, and the hydrazine hydrochloride reduction obtains potassium chloroplatinite.
Chinese patent CN102390874A discloses the combined preparation process of a kind of potassium chloroplatinite and potassium platinichloride, and its route is: the conventional path of preparing Platinic chloride of metal platinum, and------adding potassium oxalate reduction (partial reduction chloro-platinous acid)---obtaining potassium chloroplatinite---adds hydrogen peroxide and obtains potassium platinichloride in the mother liquor in the potassium hydroxide and Platinic chloride.
But in above-mentioned 3 kinds of methods that prepare potassium chloroplatinite, the reaction times of reductive agent reduction Platinic chloride generation chloro-platinous acid is consuming time longer among CN102774894A and the CN102390874A, there is the inadequate problem of reaction, though the reductive agent relative response is rapid among the CN101279772B, but there is severe toxicity in reductive agent itself, therefore be badly in need of finding a kind of weak point consuming time, can react fully and finish, and the method for reductive agent safety non-toxic.
Summary of the invention
Technical problem to be solved by this invention is that reduction Platinic chloride reaction time consumption is long when preparing potassium chloroplatinite in the prior art, react insufficient, and the problem of reductive agent toxicity, thereby provide a kind of employing nontoxic reductive agent, utilize ultrasonic cavitation to promote the potassium platinichloride reduction, and then shorten the reaction times, make reaction prepare the method for potassium chloroplatinite more fully.
For solving the problems of the technologies described above, the present invention is achieved by the following technical solutions:
A kind of preparation method of potassium chloroplatinite is characterized in that, comprises the steps:
S01 is dissolved in spongy platinum in the chloroazotic acid, obtains platinum acid chloride solution after catching up with nitre, catching up with sour step;
S02 adds Klorvess Liquid in the platinum acid chloride solution that obtains to described step S01, and being stirred to the throw out of separating out no longer increases, and filters to obtain the potassium platinichloride precipitation, adds water, obtains the potassium platinichloride suspension liquid;
S03 under the ultrasonic oscillation condition, adds reductant solution in the potassium platinichloride precipitation suspension liquid that obtains among the described step S02, and stirring obtains the solution of scarlet, no longer deepens until solution colour;
S04 adds concentrated hydrochloric acid in the scarlet solution that obtains in the described step S03, precipitates unreacted potassium platinichloride, and the filtering post precipitation obtains the chloro-platinous acid potassium solution;
S05, the potassium chloroplatinite solution concentration with described step S04 obtains adds with volume ethanol or glycerine, cools off half an hour in 0 ℃ of mixture of ice and water, and potassium chloroplatinite crystallization is wherein separated out, and filters and obtains the potassium chloroplatinite crystal; With ethanol or glycerine washing crystal, after the vacuum-drying, namely get product.
Among the described step S02, described ultrasonic concussion mode is that cosine attitude ultrasonic wave and frequency conversion ultrasonic wave are handled jointly.
Described cosine attitude frequency of ultrasonic is 20-25kHz, and power is 200mW/cm
2Can select for use cosine ultrasonic instrument conventional in the prior art to handle.
Described frequency conversion ultrasonic frequency is 35-40kHz, and power is 200mW/cm
2Can select for use frequency conversion ultrasonic instrument conventional in the prior art to handle.
The transmission that can adopt the medium known in the prior art to shake in the above-mentioned ultrasound procedure of the present invention for example can adopt the simplest water medium transmission to realize.
Among the described step S03, described reductant solution preferable formic acid potassium; Those skilled in the art also can select other suitable nontoxicity reductive agents as required.
The mass ratio of described spongy platinum and described reductive agent is 1:0.42-0.5.
The mass ratio of described spongy platinum and described Repone K is 1:0.8-1.
Among the described step S02, described Klorvess Liquid is 10% Klorvess Liquid, and the temperature of reaction of described step S02 is 60 ℃.
The temperature of reaction of described step S03 is 50 ℃.
The micro-bubble (cavitation nucleus) that ultrasonic cavitation refers to be present in the liquid is activated under the effect of ultrasonic field, shows as a series of dynamic processes such as vibration, growth, contraction and even collapse of complex.Extreme conditions such as the formed thundering high temperature of ultrasonic cavitation, high pressure have obtained using widely in scientific research and industrial production for the chemical reaction that difficult realization under general condition maybe can not realize provides a kind of new very special physicochemical environment.When strong ultrasonic field is propagated, can produce series of effects, as mechanical effect, heat effect, chemical effect, photoeffect etc. in media.Stirring, dispersion, degasification, mist formation, cohesion, impact grinding and fatigue damage effect are arranged in mechanical effect; The integral body heating that in heat effect, has acoustic energy to be absorbed and cause, the local heating of boundary; Can promotes oxidn in chemical effect, reduction, promote the polymerization of polymer substance or unzipping etc.In addition, the physical influence that ultrasonic cavitation causes has a very important role in the chemical industry mass transfer process, can cause solid-liquid reaction system in the mass transfer process, reactive liquid solution system, produce turbulence effect, perturbation effect, interfacial effect, cavity effect, the comprehensive action of these effects is accelerated diffusion reinforcement in the mass transfer process, solid surface activation, mass transfer area increase, speed of response, improves mass-transfer efficiency, promotion effect of mass transmitting.
Technique scheme of the present invention has the following advantages compared to existing technology:
(1) preparation method of a kind of potassium chloroplatinite of the present invention utilizes ultrasonic cavitation to promote potassium platinichloride to be reduced into the reaction process of potassium chloroplatinite, has shortened the reaction times, makes reaction more abundant, has improved the productive rate of potassium chloroplatinite.
(2) preparation method of a kind of potassium chloroplatinite of the present invention adopts 20-25kHz, 200mW/cm
2Ultrasonic and the 35-40kHz of cosine attitude, 200mW/cm
2The frequency conversion ultrasonic wave is handled jointly, and composite ultraphonic can increase vibration amplitude, and it is long-pending to increase mass transfer surfaces; And can reduce the dead angle that standing wave causes, improve productive rate; And the bubble of composite ultraphonic maximum empty produces stronger collapse greater than the maximum empty bubble of combined ultrasonic, has synergy.
(3) adopt potassium formiate to reduce Platinic chloride as reductive agent; Formate is a kind of stronger reductive agent of reductibility commonly used, often is used to the reduction of noble metal catalyst, also is used for drilling fluid or Snow Agent, cheaply be easy to get, and nontoxic.
(4) preparation method of a kind of potassium chloroplatinite of the present invention, in described step S04, adopt to increase the mode of chlorion in the reaction solution, the solubleness of potassium platinichloride in reaction solution that is not reduced is reduced and separate out with precipitation, thereby improved the purity of potassium chloroplatinite.
Description of drawings
Content of the present invention is easier clearly to be understood in order to make, and below in conjunction with accompanying drawing, the present invention is further detailed explanation, wherein:
Fig. 1 is the structural representation of ultrasonic reactor of the present invention;
Reference numeral is expressed as among the figure: 1-water, and the 2-glass reactor, 3-cosine frequency conversion ultrasound probe, 4-cosine frequency conversion ultrasonic generator, the frequency conversion of 5-slot type is ultrasonic, 6-water inlet, 7-water port, 8-temperature controller, 9-thermometer, 10-heating rod.
Embodiment
The method for preparing potassium chloroplatinite of the present invention can adopt and can adopt the attainable mode of knowing in the prior art to carry out in the prior art.As shown in Figure 1 a kind of available mode, can adopt the combination of described ultrasonic reactor to carry out the control of reaction conditions among the following embodiment 1-11, ultrasonic concussion is carried out in reaction.This reactor with glass reactor 2 as reaction compartment, shake transmission with WATER AS FLOW MEDIUM 1 as ultrasonic medium, carry out common ultrasound procedure with slot type frequency conversion ultrasonic 5 and cosine frequency conversion ultrasonic generator 4, described cosine frequency conversion ultrasonic generator 4 utilizes cosine frequency conversion ultrasound probe 3 to stretch in the described glass reactor 2 to shake control, and described slot type frequency conversion ultrasonic 5 is provided with water inlet 6 and water port 7 for medium flowing.Also be provided with thermometer 9 with the monitoring reaction temperature in ultrasonic 5 reactive tanks of described slot type frequency conversion, and carry out temperature controlling by temperature controller 8 control heating rods 10.In the process of preparation potassium chloroplatinite, the potassium platinichloride suspension liquid is placed glass reactor 2, under the common ultrasonication of slot type frequency conversion ultrasonic 5 and cosine frequency conversion ultrasound probe 3, promote reductive agent that the potassium platinichloride reduction is generated potassium chloroplatinite.
Embodiment 1
The described method for preparing potassium chloroplatinite of present embodiment comprises the steps:
S01 is dissolved in the 10g spongy platinum in the chloroazotic acid, and through catching up with nitre, catching up with acid, to the molasse shape, diluting soln obtains platinum acid chloride solution to 100mL then with solution concentration;
S02 adds the 100mL10% Klorvess Liquid in the platinum acid chloride solution that obtains to described step S01, being stirred to the throw out of separating out in 60 ℃ no longer increases, and filters and obtains the potassium platinichloride precipitation, adds water 100mL in the precipitation, obtains the potassium platinichloride suspension liquid;
S03, at 20-25kHz, 200mW/cm
2Ultrasonic and the 35-40kHz of cosine attitude, 200mW/cm
2Under the condition of the common concussion of frequency conversion ultrasonic wave, the potassium formiate solution of 435mL1% is joined in the potassium platinichloride suspension liquid that obtains among the described step S02, stirring in 50 ℃ obtains the solution of scarlet, no longer deepens until solution colour; Solution concentration can be added pure water in case of necessity to 250mL;
S04 adds with the volume concentrated hydrochloric acid in the scarlet solution that obtains in the described step S03, precipitates unreacted potassium platinichloride, and the filtering post precipitation obtains the chloro-platinous acid potassium solution;
S05 adds with volume ethanol or glycerine in the chloro-platinous acid potassium solution that obtains to described step S04,0 ℃ of cooling half an hour, potassium chloroplatinite crystallization is wherein separated out, and filters and obtains the potassium chloroplatinite crystal; With ethanol or glycerine washing crystal, after the vacuum-drying, namely.
The described method for preparing potassium chloroplatinite of present embodiment comprises the steps:
S01 is dissolved in the 10g spongy platinum in the chloroazotic acid, and through catching up with nitre, catching up with acid, to the molasse shape, diluting soln obtains platinum acid chloride solution to 100mL then with solution concentration;
S02 adds the 80mL10% Klorvess Liquid in the platinum acid chloride solution that obtains to described step S01, being stirred to the throw out of separating out in 60 ℃ no longer increases, and filters and obtains the potassium platinichloride precipitation, adds water 100mL in the precipitation, obtains the potassium platinichloride suspension liquid;
S03, at 20-25kHz, 200mW/cm
2Ultrasonic and the 35-40kHz of cosine attitude, 200mW/cm
2Under the condition of the common concussion of frequency conversion ultrasonic wave, the potassium formiate solution of 435mL1% is joined in the potassium platinichloride suspension liquid that obtains among the described step S02, stirring in 50 ℃ obtains the solution of scarlet, no longer deepens until solution colour; Concentrated solution can be added pure water in case of necessity to 250mL;
S04 adds with the volume concentrated hydrochloric acid in the scarlet solution that obtains in the described step S03, precipitates unreacted potassium platinichloride, and the filtering post precipitation obtains the chloro-platinous acid potassium solution;
S05 adds ethanol or glycerine in the chloro-platinous acid potassium solution that obtains to described step S04, be cooled to 0 ℃ potassium chloroplatinite crystallization is wherein separated out, and filters and obtains the potassium chloroplatinite crystal; With ethanol or glycerine washing crystal, after the vacuum-drying, namely.
The described method for preparing potassium chloroplatinite of present embodiment comprises the steps:
S01 is dissolved in the 10g spongy platinum in the chloroazotic acid, and through catching up with nitre, catching up with acid, to the molasse shape, diluting soln obtains platinum acid chloride solution to 100mL then with solution concentration;
S02 adds the 38mL20% Klorvess Liquid in the platinum acid chloride solution that obtains to described step S01, being stirred to the throw out of separating out in 65 ℃ no longer increases, and filters and obtains the potassium platinichloride precipitation, adds water 100mL in the precipitation, obtains the potassium platinichloride suspension liquid;
S03, at 20-25kHz, 200mW/cm
2Ultrasonic and the 35-40kHz of cosine attitude, 200mW/cm
2Under the condition of the common concussion of frequency conversion ultrasonic wave, the potassium formiate solution of 500mL1% is joined in the potassium platinichloride suspension liquid that obtains among the described step S02, stirring in 70 ℃ obtains the solution of scarlet, no longer deepens until solution colour; Concentrated solution can be added pure water in case of necessity to 250mL;
S04 adds with the volume concentrated hydrochloric acid in the scarlet solution that obtains in the described step S03, precipitates unreacted potassium platinichloride, and the filtering post precipitation obtains the chloro-platinous acid potassium solution;
S05 adds ethanol or glycerine in the chloro-platinous acid potassium solution that obtains to described step S04, cooling is separated out potassium chloroplatinite crystallization wherein, 0 ℃ of cooling half an hour, filters and obtains the potassium chloroplatinite crystal; With ethanol or glycerine washing crystal, after the vacuum-drying, namely.
The described method for preparing potassium chloroplatinite of present embodiment comprises the steps:
S01 is dissolved in the 10g spongy platinum in the chloroazotic acid, and through catching up with nitre, catching up with acid, to the molasse shape, diluting soln obtains platinum acid chloride solution to 100mL then with solution concentration;
S02 adds the 80mL10% Klorvess Liquid in the platinum acid chloride solution that obtains to described step S01, being stirred to the throw out of separating out in 55 ℃ no longer increases, and filters and obtains the potassium platinichloride precipitation, adds water 100mL in the precipitation, obtains the potassium platinichloride suspension liquid;
S03, at 20-25kHz, 200mW/cm
2Ultrasonic and the 35-40kHz of cosine attitude, 200mW/cm
2Under the condition of the common concussion of frequency conversion ultrasonic wave, the potassium formiate solution of 500mL1% is joined in the potassium platinichloride suspension liquid that obtains among the described step S02, stirring in 60 ℃ obtains the solution of scarlet, no longer deepens until solution colour; Concentrated solution can be added pure water in case of necessity to 250mL;
S04 adds with the volume concentrated hydrochloric acid in the scarlet solution that obtains in the described step S03, precipitates unreacted potassium platinichloride, and the filtering post precipitation obtains the chloro-platinous acid potassium solution;
S05 adds with volume ethanol or glycerine in the chloro-platinous acid potassium solution that obtains to described step S04,0 ℃ of cooling half an hour potassium chloroplatinite crystallization is wherein separated out, and filters and obtains the potassium chloroplatinite crystal; With ethanol or glycerine washing crystal, after the vacuum-drying, namely.
Embodiment 5
The described method for preparing potassium chloroplatinite of present embodiment comprises the steps:
S01 is dissolved in the 10g spongy platinum in the chloroazotic acid, and through catching up with nitre, catching up with sour step solution concentration to the molasse shape, diluting soln obtains platinum acid chloride solution to 100mL then;
S02 adds the 80mL10% Klorvess Liquid in the platinum acid chloride solution that obtains to described step S01, being stirred to the throw out of separating out in 60 ℃ no longer increases, and filters and obtains the potassium platinichloride precipitation, adds water 100mL in the precipitation, obtains the potassium platinichloride suspension liquid;
S03, at 20-25kHz, 200mW/cm
2Ultrasonic and the 45-50kHz of cosine attitude, 200mW/cm
2Under the condition of the common concussion of frequency conversion ultrasonic wave, the potassium formiate solution of 430mL1% is joined in the potassium platinichloride suspension liquid that obtains among the described step S02, stirring in 50 ℃ obtains the solution of scarlet, no longer deepens until solution colour; Concentrated solution can be added pure water in case of necessity to 250mL;
S04 adds with the volume concentrated hydrochloric acid in the scarlet solution that obtains in the described step S03, precipitates unreacted potassium platinichloride, and the filtering post precipitation obtains the chloro-platinous acid potassium solution;
S05 adds with volume ethanol or glycerine in the chloro-platinous acid potassium solution that obtains to described step S04, and 0 ℃ of cooling is separated out the half an hour of potassium chloroplatinite crystallization wherein, filters and obtains the potassium chloroplatinite crystal; With ethanol or glycerine washing crystal, after the vacuum-drying, namely.
Embodiment 6
The described method for preparing potassium chloroplatinite of present embodiment comprises the steps:
S01 is dissolved in the 10g spongy platinum in the chloroazotic acid, and through catching up with nitre, catching up with acid, to the molasse shape, diluting soln obtains platinum acid chloride solution to 100mL then with solution concentration;
S02 adds the 80mL10% Klorvess Liquid in the platinum acid chloride solution that obtains to described step S01, being stirred to the throw out of separating out in 60 ℃ no longer increases, and filters and obtains the potassium platinichloride precipitation, adds water 100mL in the precipitation, obtains the potassium platinichloride suspension liquid;
S03, at 10-15kHz, 200mW/cm
2Ultrasonic and the 20-25kHz of cosine attitude, 100mW/cm
2Under the condition of the common concussion of frequency conversion ultrasonic wave, the potassium formiate solution of 470mL1% is joined in the potassium platinichloride suspension liquid that obtains among the described step S02, stirring in 50 ℃ obtains the solution of scarlet, no longer deepens until solution colour; Concentrated solution can be added pure water in case of necessity to 250mL;
S04 adds with the volume concentrated hydrochloric acid in the scarlet solution that obtains in the described step S03, precipitates unreacted potassium platinichloride, and the filtering post precipitation obtains the chloro-platinous acid potassium solution;
S05 adds with volume ethanol or glycerine in the chloro-platinous acid potassium solution that obtains to described step S04,0 ℃ of cooling half an hour potassium chloroplatinite crystallization is wherein separated out, and filters and obtains the potassium chloroplatinite crystal; With ethanol or glycerine washing crystal, after the vacuum-drying, namely.
Embodiment 7
The described method for preparing potassium chloroplatinite of present embodiment comprises the steps:
S01 is dissolved in the 10g spongy platinum in the chloroazotic acid, and through catching up with nitre, catching up with acid, to the molasse shape, diluting soln obtains platinum acid chloride solution to 100mL then with solution concentration;
S02 adds the 76mL10% Klorvess Liquid in the platinum acid chloride solution that obtains to described step S01, being stirred to the throw out of separating out in 60 ℃ no longer increases, and filters and obtains the potassium platinichloride precipitation, adds water 100mL in the precipitation, obtains the potassium platinichloride suspension liquid;
S03, at 20-25kHz, 200mW/cm
2Under the condition of cosine attitude ultrasonic oscillation, the potassium formiate solution of 450mL1% is joined in the potassium platinichloride suspension liquid that obtains among the described step S02, stirring in 50 ℃ obtains the solution of scarlet, no longer deepens until solution colour; Concentrated solution can be added pure water in case of necessity to 250mL;
S04 adds with the volume concentrated hydrochloric acid in the scarlet solution that obtains in the described step S03, precipitates unreacted potassium platinichloride, and the filtering post precipitation obtains the chloro-platinous acid potassium solution;
S05 adds ethanol or glycerine in the chloro-platinous acid potassium solution that obtains to described step S04,0 ℃ of cooling separates out potassium chloroplatinite crystallization wherein half an hour, filters and obtains the potassium chloroplatinite crystal; With ethanol or glycerine washing crystal, after the vacuum-drying, namely.
The described method for preparing potassium chloroplatinite of present embodiment comprises the steps:
S01 is dissolved in the 10g spongy platinum in the chloroazotic acid, and through catching up with nitre, catching up with acid, to the molasse shape, diluting soln obtains platinum acid chloride solution to 100mL then with solution concentration;
S02 adds the 78mL10% Klorvess Liquid in the platinum acid chloride solution that obtains to described step S01, being stirred to the throw out of separating out in 60 ℃ no longer increases, and filters and obtains the potassium platinichloride precipitation, adds water 100mL in the precipitation, obtains the potassium platinichloride suspension liquid;
S03, at 35-40kHz, 200mW/cm
2Under the condition of frequency conversion ultrasonic oscillation, the potassium formiate solution of 430mL1% is joined in the potassium platinichloride suspension liquid that obtains among the described step S02, stirring in 50 ℃ obtains the solution of scarlet, no longer deepens until solution colour; Concentrated solution can be added pure water in case of necessity to 250mL;
S04 adds with the volume concentrated hydrochloric acid in the scarlet solution that obtains in the described step S03, precipitates unreacted potassium platinichloride, and the filtering post precipitation obtains the chloro-platinous acid potassium solution;
S05 adds with volume ethanol or glycerine in the chloro-platinous acid potassium solution that obtains to described step S04, and 0 ℃ of cooling separates out potassium chloroplatinite crystallization wherein half an hour, filters and obtains the potassium chloroplatinite crystal; With ethanol or glycerine washing crystal, after the vacuum-drying, namely.
Embodiment 9
The described method for preparing potassium chloroplatinite of present embodiment comprises the steps:
S01 is dissolved in the 10g spongy platinum in the chloroazotic acid, and through catching up with nitre, catching up with acid, to the molasse shape, diluting soln obtains platinum acid chloride solution to 100mL then with solution concentration;
S02 adds the 80mL10% Klorvess Liquid in the platinum acid chloride solution that obtains to described step S01, being stirred to the throw out of separating out in 60 ℃ no longer increases, and filters and obtains the potassium platinichloride precipitation, adds water 100mL in the precipitation, obtains the potassium platinichloride suspension liquid;
S03, at 20kHz, 200mW/cm
2Under the condition of sinusoidal attitude ultrasonic oscillation, the potassium formiate solution of 490mL1% is joined in the potassium platinichloride suspension liquid that obtains among the described step S02, stirring in 50 ℃ obtains the solution of scarlet, no longer deepens until solution colour; Concentrated solution can be added pure water in case of necessity to 250mL;
S04 adds with the volume concentrated hydrochloric acid in the scarlet solution that obtains in the described step S03, precipitates unreacted potassium platinichloride, and the filtering post precipitation obtains the chloro-platinous acid potassium solution;
S05 adds ethanol or glycerine in the chloro-platinous acid potassium solution that obtains to described step S04,0 ℃ of cooling separates out potassium chloroplatinite crystallization wherein half an hour, filters and obtains the potassium chloroplatinite crystal; With ethanol or glycerine washing crystal, after the vacuum-drying, namely.
The described method for preparing potassium chloroplatinite of present embodiment comprises the steps:
S01 is dissolved in the 10g spongy platinum in the chloroazotic acid, and through catching up with nitre, catching up with acid, to the molasse shape, diluting soln obtains platinum acid chloride solution to 100mL then with solution concentration;
S02 adds the 80mL10% Klorvess Liquid in the platinum acid chloride solution that obtains to described step S01, being stirred to the throw out of separating out in 60 ℃ no longer increases, and filters and obtains the potassium platinichloride precipitation, adds water 100mL in the precipitation, obtains the potassium platinichloride suspension liquid;
S03, at 35kHz, 200mW/cm
2Under the condition of single-frequency ultrasonic oscillation, the potassium formiate solution of 470mL1% is joined in the potassium platinichloride suspension liquid that obtains among the described step S02, stirring in 50 ℃ obtains the solution of scarlet, no longer deepens until solution colour; Concentrated solution can be added pure water in case of necessity to 250mL;
S04 adds with the volume concentrated hydrochloric acid in the scarlet solution that obtains in the described step S03, precipitates unreacted potassium platinichloride, and the filtering post precipitation obtains the chloro-platinous acid potassium solution;
S05 adds with volume ethanol or glycerine in the chloro-platinous acid potassium solution that obtains to described step S04, and 0 ℃ of cooling separates out potassium chloroplatinite crystallization wherein half an hour, filters and obtains the potassium chloroplatinite crystal; With ethanol or glycerine washing crystal, after the vacuum-drying, namely.
Embodiment 11
The described method for preparing potassium chloroplatinite of present embodiment comprises the steps:
S01 is dissolved in the 10g spongy platinum in the chloroazotic acid, and through catching up with nitre, catching up with acid, to the molasse shape, diluting soln obtains platinum acid chloride solution to 100mL then with solution concentration;
S02 adds the 80mL10% Klorvess Liquid in the platinum acid chloride solution that obtains to described step S01, being stirred to the throw out of separating out in 60 ℃ no longer increases, and filters and obtains the potassium platinichloride precipitation, adds water 100mL in the precipitation, obtains the potassium platinichloride suspension liquid;
S03 joins the potassium formiate solution of 470mL1% in the potassium platinichloride suspension liquid that obtains among the described step S02, and stirring in 50 ℃ obtains the solution of scarlet, no longer deepens until solution colour; Concentrated solution can be added pure water in case of necessity to 250mL;
S04 adds with the volume concentrated hydrochloric acid in the scarlet solution that obtains in the described step S03, precipitates unreacted potassium platinichloride, and the filtering post precipitation obtains the chloro-platinous acid potassium solution;
S05 adds ethanol or glycerine in the chloro-platinous acid potassium solution that obtains to described step S04,0 ℃ of cooling separates out potassium chloroplatinite crystallization wherein half an hour, filters and obtains the potassium chloroplatinite crystal; With ethanol or tempt washing crystal, after the vacuum-drying, namely.
Collection also detects the yield of products obtained therefrom among above-described embodiment 1-11 and the purity index of products obtained therefrom, shown in seeing the following form:
According to last table data, we adopt the sonic oscillation mode to control the reaction times that can effectively shorten entire reaction, and also can realize higher productive rate within a short period of time as can be seen.Use independent frequency conversion ultrasonic power or use independent cosine ultrasonic power all to help lend some impetus to reaction and carry out faster, and improve product yield; And adopt the ultrasonic mode of frequency conversion and the ultrasonic acting in conjunction of cosine more further to promote the yield of reaction, and realized reaction fully completely in the shorter time; When at 20-25kHz, 200mW/cm
2Ultrasonic and the 35-40kHz of cosine attitude, 200mW/cm
2Under the condition of the common concussion of frequency conversion ultrasonic wave, the reaction times of potassium formiate reduction potassium platinichloride foreshortens to about 1/3, and the productive rate of products therefrom reaches the highest and near the saturation type reaction, not only obviously be better than other reaction conditionss, and effect is very remarkable simultaneously.
Obviously, above-described embodiment only is for example clearly is described, and is not the restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here need not also can't give all embodiments exhaustive.And the apparent variation of being extended out thus or change still are among the protection domain of the invention.
Claims (10)
1. the preparation method of a potassium chloroplatinite is characterized in that, comprises the steps:
S01 is dissolved in spongy platinum in the chloroazotic acid, obtains platinum acid chloride solution after catching up with nitre, catching up with sour step;
S02 adds Klorvess Liquid in the platinum acid chloride solution that obtains to described step S01, and being stirred to the throw out of separating out no longer increases, and filters to obtain the potassium platinichloride precipitation, adds water in precipitation, obtains the potassium platinichloride suspension liquid;
S03 under ultrasonic concussion, joins reductant solution in the potassium platinichloride precipitation suspension liquid that obtains among the described step S02, stirs, and reaction obtains the solution of scarlet, after solution colour is no longer deepened, and stopped reaction;
S04 adds concentrated hydrochloric acid in the scarlet solution that obtains in the described step S03, precipitates unreacted potassium platinichloride, and the filtering post precipitation obtains the chloro-platinous acid potassium solution;
S05 adds ethanol or glycerine in the chloro-platinous acid potassium solution that obtains to described step S04, cooling is separated out potassium chloroplatinite crystallization wherein, filters to obtain the potassium chloroplatinite crystal; With ethanol or glycerine washing crystal, after the vacuum-drying, namely.
2. the preparation method of potassium chloroplatinite according to claim 1, it is characterized in that: among the described step S02, described ultrasonic concussion mode is that cosine attitude ultrasonic wave and frequency conversion ultrasonic wave are handled jointly.
3. the preparation method of potassium chloroplatinite according to claim 2, it is characterized in that: described cosine attitude frequency of ultrasonic is 20-25kHz, and power is 200mW/cm
2
4. according to the preparation method of claim 2 or 3 described potassium chloroplatinites, it is characterized in that: described frequency conversion ultrasonic frequency is 35-40kHz, and power is 200mW/cm
2
5. according to the preparation method of the arbitrary described potassium chloroplatinite of claim 1-4, it is characterized in that: among the described step S03, described reductant solution is potassium formiate.
6. the preparation method of potassium chloroplatinite according to claim 5, it is characterized in that: the mass ratio of described spongy platinum and described reductive agent is 1:0.42-0.5.
7. the preparation method of potassium chloroplatinite according to claim 6, it is characterized in that: the mass ratio of described spongy platinum and described Repone K is 1:0.8-1.
8. the preparation method of potassium chloroplatinite according to claim 7, it is characterized in that: among the described step S02, described Klorvess Liquid is 10% Klorvess Liquid.
9. according to the preparation method of the arbitrary described potassium chloroplatinite of claim 1-8, it is characterized in that: the temperature of reaction of described step S02 is 60 ℃.
10. according to the preparation method of the arbitrary described potassium chloroplatinite of claim 1-8, it is characterized in that: the temperature of reaction of described step S03 is 50 ℃.
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| CN103880889A (en) * | 2014-03-18 | 2014-06-25 | 昆明贵研催化剂有限责任公司 | Precursor for preparing platinized catalyst and synthesis method thereof |
| CN105294728A (en) * | 2015-10-19 | 2016-02-03 | 江阴职业技术学院 | Method for extracting artemisinin through ultrasonic technology |
| CN109761290A (en) * | 2019-03-15 | 2019-05-17 | 西安凯立新材料股份有限公司 | A kind of preparation method of potassium chloroplatinite |
| CN114315912A (en) * | 2021-12-28 | 2022-04-12 | 江西贝特利新材料有限公司 | Preparation method of cis-dichlorobis (diethyl sulfide) platinum (II) |
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| CN114315912A (en) * | 2021-12-28 | 2022-04-12 | 江西贝特利新材料有限公司 | Preparation method of cis-dichlorobis (diethyl sulfide) platinum (II) |
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