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Preparation method of palladium(II) tetrammine chloride

A technology of dichlorotetraammine palladium and chloropalladium acid is applied in chemical instruments and methods, ruthenium/rhodium/palladium/osmium/iridium/platinum compounds, inorganic chemistry, etc., and can solve the problem of long reaction time and difficulty in product separation and purification and other problems to achieve the effect of increasing the probability of contact and collision, increasing instability, and speeding up the generation

Active Publication Date: 2015-09-23
陕西煤业化工技术开发中心有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The present invention solves the problems of long reaction time and difficult product separation and purification in the preparation method of dichlorotetraammine palladium in the prior art, and then provides a separation and purification process that can effectively shorten the reaction time and simplify the product, The preparation method of dichloro tetraammine palladium that improves reaction yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The preparation method of dichloro tetraammine palladium described in the present embodiment, comprises the steps:

[0030] Add 17.73g of palladium chloride powder into 200ml, 1mol / L hydrochloric acid solution in batches, and stir for 30min until the palladium chloride powder is completely dissolved to obtain a chloropalladium acid solution;

[0031] The above-mentioned chloropalladium acid solution is transferred in the good reactor tube of translucency, and the deionized water of 500ml is added wherein, then this reactor tube is placed in the ultraviolet photochemical reactor, turn on the ultraviolet lamp (the wavelength of ultraviolet light Set as 280nm, the ratio of its intensity to the mass of palladium is 60000cd / g), and ultraviolet light is vertically incident into the reactor tube; Ammonia gas was introduced into the bottom of the aqueous solution for 32.6 minutes; the reaction solution was heated and concentrated until a layer of crystal film appeared on the li...

Embodiment 2

[0035] The preparation method of dichloro tetraammine palladium described in the present embodiment, comprises the steps:

[0036] Add 17.73g of palladium chloride powder into 200ml, 1mol / L hydrochloric acid solution in batches, and stir for 45min until the palladium chloride powder is completely dissolved to obtain the chloropalladium acid solution;

[0037]The above-mentioned chloropalladium acid solution is transferred in the good reactor tube of translucency, and the deionized water of 750ml is added wherein, this reactor tube is placed in the ultraviolet photochemical reactor, turn on the ultraviolet lamp (the wavelength of ultraviolet light is set Determined as 380nm, the ratio of its intensity to the mass of palladium is 30000cd / g), and the ultraviolet light is vertically incident into the reactor tube; use a mass flowmeter and flow to the aqueous solution of chloropalladium acid with a flow rate of 4ml / s through the gas distributor Inject ammonia gas at the bottom for ...

Embodiment 3

[0041] The preparation method of dichloro tetraammine palladium described in the present embodiment, comprises the steps:

[0042] Add 17.73g of palladium chloride powder into 200ml, 1mol / L hydrochloric acid solution in batches, and stir for 30min until the palladium chloride powder is completely dissolved to obtain a chloropalladium acid solution;

[0043] The above-mentioned chloropalladium acid solution is transferred in the good reactor tube of translucency, and the deionized water of 500ml is added wherein, then this reactor tube is placed in the ultraviolet photochemical reactor, open ultraviolet lamp, (ultraviolet light The wavelength is set at 320nm, the ratio of its intensity to the mass of palladium is 600cd / g), and the ultraviolet light is vertically incident into the reactor tube; use a mass flowmeter and pass through the gas distributor to the bottom of the solution at a flow rate of 10ml / s Enter ammonia gas for 16.3 minutes, then keep reacting for 13.7 minutes; h...

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Abstract

The invention provides a preparation method of palladium(II) tetrammine chloride. The method comprises the step that chloropalladic acid reacts with ammonia under irradiation of ultraviolet light of 280-380 nm to generate the palladium(II) tetrammine chloride. The reaction system by irradiating through the ultraviolet light of 280-380 nm is adopted in the preparation process of the palladium(II) tetrammine chloride for the first time, dissociation of (PdCl4)2- in the chloropalladic acid is effectively accelerated, the reaction rate is improved conveniently, and generation of the palladium(II) tetrammine chloride is accelerated. The preparation method can increase the reaction rate of the chloropalladic acid and the ammonia to be converted into the palladium(II) tetrammine chloride, greatly shorten the reaction time and also reduce the loss of palladium, thereby facilitating improvement of product yield. The yield of the preparation method is above 98%.

Description

technical field [0001] The invention relates to a preparation method of dichlorotetraammine palladium, which belongs to the field of inorganic compounds. technical background [0002] Tetraammine palladium (II) compounds ([Pd(NH 3 ) 4 ]X 2 , X=Cl, Br, NO 2 , NO 3 , AcO, SO 4 、C 2 o 4 etc.) is an important class of palladium compounds, widely used in chemical catalysis and electroplating industries. Among them, dichlorotetraamminepalladium is the most readily available tetraamminepalladium product, and it is also a necessary intermediate or precursor for the preparation of other tetraamminepalladium compounds. Therefore, optimizing the preparation process of palladium dichlorotetraammine, so that its preparation raw materials are easier to obtain, the reaction time is shorter, and the product purity is higher, has positive practical significance and broad application prospects. [0003] At present, the preparation method of dichlorotetraammine palladium can be divide...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G55/00
Inventor 张蕾宋双田王振宇白文校祁敏鲁思达杨凯宁
Owner 陕西煤业化工技术开发中心有限责任公司
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