CN104925872B - Preparation method of palladium(II) tetrammine chloride - Google Patents
Preparation method of palladium(II) tetrammine chloride Download PDFInfo
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- CN104925872B CN104925872B CN201510337197.2A CN201510337197A CN104925872B CN 104925872 B CN104925872 B CN 104925872B CN 201510337197 A CN201510337197 A CN 201510337197A CN 104925872 B CN104925872 B CN 104925872B
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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
The present invention relates to a kind of preparation method of the ammino palladium of dichloro four, belongs to inorganic compound field.
Technical background
Four ammino palladium (II) class compound ([Pd (NH3)4]X2, X=Cl, Br, NO2、NO3、AcO、SO4、C2O4Deng) it is a class
Important palladium compound, is widely used in chemical catalysis and electroplating industry.Wherein, the ammino palladium of dichloro four is four amminos being most easy to get
Palladium class product, be also prepare other four ammino palladium class compounds must Jing intermediates or presoma.Therefore, to the ammino palladium of dichloro four
Preparation technology be optimized so that its preparing raw material is more easy to get, the reaction time is shorter, product purity is higher, with positive
Realistic meaning and wide application prospect.
At present, the preparation method of the ammino palladium of dichloro four can be divided into four big class by initiation material：
The first kind is with palladium bichloride (PdCl2) it is initiation material, palladium bichloride is dissolved in watery hydrochloric acid and obtains chlorine palladium acid solution,
Enough ammoniacal liquor is added dropwise again, and the ammino palladium of dichloro four is obtained；
Equations of The Second Kind is with chlorine palladium acid compounds (X2PdCl4, X=H, Na, NH4Deng) it is initiation material, by chlorine palladium acids
Compound is soluble in water to obtain solution, then enough ammoniacal liquor is added dropwise the ammino palladium of dichloro four is obtained；
3rd class is to close palladium four ammino palladium (Pd (NH of acid with tetrachloro3)4·PdCl4) it is initiation material, it is dissolved in enough
The ammino palladium of dichloro four can be prepared in ammoniacal liquor；
4th class is with the ammino palladium (Pd (NH of dichloro two3)2Cl2) it is initiation material, the ammino palladium of dichloro two is dissolved in enough
The ammino palladium of dichloro four is obtained in ammoniacal liquor.
As described above, the first kind and Equations of The Second Kind method are currently to prepare the ammino palladium most common method of dichloro four, for example, by
Mcgraw-hill, inc of the U.S. publishes, the Inorganic Syntheses volumes eight of Henry F.Holtzclaw chief editors；It is Central-South
The chief editors' such as university press's publication, Du Xinling《Precious metals metallurgy technology》；Chemical Industry Press's publication, thorough method etc. are edited
's《Noble metal deep processing project》；Chemical Industry Press publishes, in building the chief editors' such as the people《Precious metal chemical complex and complex are closed
Into handbook》；And Wang Dawei etc. is published in《Noble metal》The article of the S1 phases of volume 35 employs above-mentioned Equations of The Second Kind method system
The standby ammino palladium of dichloro four.The flow process of the process is simple, easily operated, but the reaction time is longer, and needs to add excessively
Ammoniacal liquor can just make (PdCl4)2-It is fully converted to Pd (NH3)4 2+Furthermore, the excessive ammonia added in course of reaction is to follow-up
Separate and purification brings larger workload, be highly detrimental to the purification process of product.And for above-mentioned 3rd class and the 4th class
The preparation method of the ammino palladium of dichloro four, at present only Chemical Industry Press publish, in building the chief editors' such as the people《Precious metal chemical complex
And complex synthesis handbook》In refer to.Because the initiation material of both synthesis techniques is difficult to obtain, thus in actual production
In seldom adopt.
In consideration of it, how the preparation method of the ammino palladium of dichloro four is optimized and be improved, with effectively shorten the reaction time,
Simplify the separating-purifying operation of product, be this area technical barrier urgently to be resolved hurrily.
The content of the invention
The present invention solve be the ammino palladium of dichloro of the prior art four preparation method existing for reaction time length, produce
The difficult problem of product separating-purifying, and then provide and a kind of can effectively shorten the reaction time, simplify the separating-purifying operation of product, carry
The preparation method of the ammino palladium of dichloro four of high reaction yield.
The present invention solve the technical scheme that adopts of above-mentioned technical problem for：
A kind of preparation method of the ammino palladium of dichloro four, at least comprises the steps：
Under the ultraviolet light of 280-380nm, the acid of chlorine palladium reacts with ammonia, generates the ammino palladium of dichloro four.
The intensity of the ultraviolet light is 600-60000cd/g with the mass ratio of palladium in chlorine palladium acid.
In reaction system of the ultraviolet light vertical incidence to the acid of chlorine palladium with ammonia.
Reactor tube be arranged in parallel with multiple ultraviolet lamp tubes, and the ultraviolet lamp tube surrounds the reactor tube equidistant intervals
Arrange, and the reactor tube is equal with the distance between ultraviolet lamp tube each described.
The content of palladium is less than 60g/L in reaction system of the chlorine palladium acid with ammonia.
The purity of the ammonia is 99.99%-99.999%.
The ammonia Jing gas distributors are entered in the reaction system of the acid of chlorine palladium and ammonia.
The ammonia is 4: 1 with the mol ratio of chlorine palladium acid.
After the completion of question response, reaction system is filtered, plus hot filtrate to liquid level occurs stopping heating during epitaxial, cooling analysis
Crystalline substance, collects and drying crystallization, obtains final product the ammino palladium of the dichloro four.
The preparation method of the ammino palladium of dichloro of the present invention four, first using 280-380nm's in its preparation process
Ultraviolet light irradiating reaction system, to play a part of to activate the Pd-Cl coordinate bonds in the acid of chlorine palladium so that the bonding of the coordinate bond
Electronics on track is transitted on antibonding orbital to obtaining enough energy, so as to substantially increase the acid of chlorine palladium in
(PdCl4)2-Unstability, effectively accelerate (PdCl4)2-Dissociation, and then increase the amino molecule in ammonia and center from
Sub- Pd2+The probability for coming in contact and colliding, is conducive to improving reaction rate, accelerates the generation of the ammino palladium of dichloro four, the present invention
Preparation method can at short notice make chlorine palladium acid be almost completely converted to the ammino palladium of dichloro four, substantially reduce the reaction time,
Also avoid using substantial amounts of ammonia simultaneously, be conducive to separation and the purifying of product.The present invention limits the intensity of ultraviolet light and the acid of chlorine palladium
The mass ratio of middle palladium is 600-60000cd/g, and further limits ultraviolet light vertical incidence to the acid of chlorine palladium and the reaction of ammonia
In system, UV energy as high as possible can be obtained with the chlorine palladium acid in guarantor unit's volumetric reaction system, contribute to increasing
(PdCl in big chlorine palladium acid4)2-Unstability, so as to improve the acid of chlorine palladium and the reaction rate of ammonia.Preferably, in the present invention
Reactor tube be arranged in parallel with multiple ultraviolet lamp tubes, the ultraviolet lamp tube is equidistantly spaced around the reactor tube,
And the reactor tube is equal with the distance between ultraviolet lamp tube each described, with the unit volume for guaranteeing to be located in reactor tube
The UV energy that reaction system is received is identical, and then is conducive to improving reaction rate, shortens the reaction time.
Compared with the preparation method of the ammino palladium of dichloro of the prior art four, the system of the ammino palladium of dichloro of the present invention four
Preparation Method has the advantage that：
(1) preparation method of the ammino palladium of dichloro of the present invention four, adopts first 280-380nm in its preparation process
Ultraviolet light irradiating reaction system, can effectively accelerate the (PdCl in the acid of chlorine palladium4)2-Dissociation, be conducive to improve reaction rate
To accelerate the generation of the ammino palladium of dichloro four, compared with the method that prior art prepares the ammino palladium of dichloro four, the preparation side of the present invention
Method can at short notice make chlorine palladium acid be fully converted to the ammino palladium of dichloro four, substantially reduce the reaction time, reduce palladium
Loss, so as to be conducive to improving product yield so that the yield of preparation method of the present invention may be up to more than 98%.
(2) preparation method of the ammino palladium of dichloro of the present invention four, replaces the ammoniacal liquor in traditional handicraft to enter using ammonia
Row reaction, it is easier to control reaction process, also causes the preparation method of the present invention to be applicable to successional production technology.And
And, the actual amount of ammonia is only that at least excessive 1 times ammoniacal liquor phase is needed in its theoretical amount, with traditional handicraft in the present invention
Than the preparation method of the present invention effectively reduces the consumption of ammonia, the separation and purification of subsequent products is also allowed for, while contributing to carrying
The yield and purity of high product, dramatically saves on manpower and materials, reduce production cost.
(3) preparation method of the ammino palladium of dichloro of the present invention four is the reaction occurred under room temperature environment so that anti-
Answer mild condition, it is easier to operate.Also, according to being practically free of in the ammino palladium of dichloro four that obtains of preparation method of the present invention
Impurity ammonia, the content of palladium belongs to the ammino palladium product of highly purified dichloro four up to 43.3%.
Specific embodiment
The preparation method of the ammino palladium of dichloro four provided the present invention with reference to specific embodiment is described in detail.
Embodiment 1
The preparation method of the ammino palladium of dichloro four described in the present embodiment, comprises the steps：
The palladium bichloride powder of 17.73g is dividedly in some parts into the hydrochloric acid solution of 200ml, 1mol/L, 30min is to chlorine for stirring
Change palladium powder to be completely dissolved, that is, obtain chlorine palladium acid solution；
Above-mentioned chlorine palladium acid solution is transferred in the good reactor tube of translucency, and be added thereto to 500ml go from
Sub- water, then the reactor tube is placed in ultraviolet light chemical reactor, opening uviol lamp (wavelength of ultraviolet light is set as 280nm,
The mass ratio of its intensity and palladium is 60000cd/g), and make ultraviolet light vertical incidence to reactor tube；Use quality flow
Simultaneously Jing gas distributors are passed through ammonia 32.6min to meter with the flow of 5ml/s to chlorine palladium aqueous acid bottom；Reactant liquor is heated
It is concentrated into liquid level to occur stopping heating during a layer crystal film, natural cooling crystallization leaches crystal, and by the pale yellow crystals of gained
Vacuum is placed in be dried 24h in 40Kpa, 60 DEG C of vacuum drying oven, the ammino palladium 24.10g of dichloro four is obtained, yield is
98.09%.
Jing atomic emission spectrums are determined, and the content of palladium is 43.3% in product.
In the present embodiment, the ultraviolet light chemical reactor is provided with 3 ultraviolet lamp tubes, and 3 ultraviolet lamp tubes enclose
It is equidistantly spaced around the reactor tube, and parallel with the reactor tube, the reactor tube and each described purple
The distance between outer fluorescent tube is equal.
Embodiment 2
The preparation method of the ammino palladium of dichloro four described in the present embodiment, comprises the steps：
17.73g palladium bichloride powder is dividedly in some parts into the hydrochloric acid solution of 200ml, 1mol/L, 45min is to chlorination for stirring
Palladium powder is completely dissolved, and obtains final product chlorine palladium acid solution；
Above-mentioned chlorine palladium acid solution is transferred in the good reactor tube of translucency, and be added thereto to 750ml go from
Sub- water, the reactor tube is placed in ultraviolet light chemical reactor, opening uviol lamp (wavelength of ultraviolet light is set as 380nm, its
The mass ratio of intensity and palladium is 30000cd/g), and make ultraviolet light vertical incidence to reactor tube；Use quality flowmeter
And Jing gas distributors are passed through ammonia 40.8min with the flow of 4ml/s to chlorine palladium aqueous acid bottom；Reactant liquor is heated dense
It is reduced to liquid level to occur stopping heating during a layer crystal film, natural cooling crystallization leaches crystal, and gained pale yellow crystals are placed in
Vacuum is 60Kpa, 80 DEG C of vacuum drying oven is dried 24h, obtains the ammino palladium 24.13g of dichloro four, and yield is 98.20%.
Jing atomic emission spectrums are determined, and the content of palladium is 43.3% in product.
In the present embodiment, the ultraviolet light chemical reactor is provided with 4 ultraviolet lamp tubes, and 4 ultraviolet lamp tubes enclose
It is equidistantly spaced around the reactor tube, and parallel with the reactor tube, the reactor tube and each described purple
The distance between outer fluorescent tube is equal.
Embodiment 3
The preparation method of the ammino palladium of dichloro four described in the present embodiment, comprises the steps：
17.73g palladium bichloride powder is dividedly in some parts into the hydrochloric acid solution of 200ml, 1mol/L, 30min is to chlorination for stirring
Palladium powder is completely dissolved, that is, obtain chlorine palladium acid solution；
Above-mentioned chlorine palladium acid solution is transferred in the good reactor tube of translucency, and be added thereto to 500ml go from
Sub- water, then the reactor tube is placed in ultraviolet light chemical reactor, uviol lamp is opened, (wavelength of ultraviolet light is set as
320nm, the mass ratio of its intensity and palladium is 600cd/g), and make ultraviolet light vertical incidence to reactor tube；Use quality
Simultaneously Jing gas distributors are passed through ammonia 16.3min to flowmeter with the flow of 10ml/s to solution bottom, keep reaction again afterwards
13.7min；Reactant liquor heating is concentrated into when a layer crystal film occurs in liquid level and stops heating, natural cooling crystallization leaches crystal,
And gained pale yellow crystals are placed in into vacuum are dried 24h for 50Kpa, 70 DEG C of vacuum drying oven, obtain the ammino palladium of dichloro four
24.11g, yield is 98.13%.
Jing atomic emission spectrums are determined, and the palladium content in product is 43.3%.
In the present embodiment, the ultraviolet light chemical reactor is provided with 5 ultraviolet lamp tubes, and 5 ultraviolet lamp tubes enclose
It is equidistantly spaced around the reactor tube, and parallel with the reactor tube, the reactor tube and each described purple
The distance between outer fluorescent tube is equal.
Embodiment 4
The preparation method of the ammino palladium of dichloro four described in the present embodiment, comprises the steps：
17.73g palladium bichloride powder is dividedly in some parts into the hydrochloric acid solution of 200ml, 1mol/L, 45min is to chlorination for stirring
Palladium powder is completely dissolved, that is, obtain chlorine palladium acid solution；
Above-mentioned chlorine palladium acid solution is transferred in the good reactor tube of translucency, and be added thereto to 750ml go from
Sub- water, then the reactor tube is placed in ultraviolet light chemical reactor, opening uviol lamp (wavelength of ultraviolet light is set as 360nm,
The mass ratio of its intensity and palladium is 24000cd/g), and make ultraviolet light vertical incidence to reactor tube；Using mass flow
Simultaneously Jing gas distributors are passed through ammonia 23.3min to meter with the flow of 7ml/s to solution bottom, keep again reacting 20min afterwards；Will
Reactant liquor heating is concentrated into liquid level to be occurred stopping heating during a layer crystal film, and natural cooling crystallization leaches crystal, and gained is shallow
Yellow crystals are placed in vacuum and are dried 24h for 60Kpa, 60 DEG C of vacuum drying oven, obtain the ammino palladium 24.13g of dichloro four, and yield is
98.20%.
Jing atomic emission spectrums are determined, and the palladium content in product is 43.3%.
In the present embodiment, the ultraviolet light chemical reactor is provided with 6 ultraviolet lamp tubes, and 6 ultraviolet lamp tubes enclose
It is equidistantly spaced around the reactor tube, and parallel with the reactor tube, the reactor tube and each described purple
The distance between outer fluorescent tube is equal.
Comparative example 1
The preparation method of the ammino palladium of dichloro four described in this comparative example, comprises the steps：
The palladium bichloride powder of 17.73g is dividedly in some parts into the hydrochloric acid solution of 200ml, 1mol/L, 30min is to chlorine for stirring
Change palladium powder to be completely dissolved, that is, obtain chlorine palladium acid solution；
Above-mentioned chlorine palladium acid solution is transferred in the good reactor tube of translucency, and be added thereto to 500ml go from
Sub- water, then the reactor tube is placed in ultraviolet light chemical reactor, opening uviol lamp (wavelength of ultraviolet light is set as 280nm,
The mass ratio of its intensity and palladium is 60000cd/g), and make ultraviolet light vertical incidence to reactor tube；Within 32.6min
The ammoniacal liquor 35.85ml containing ammonia 25wt% is evenly added dropwise in chlorine palladium acid solution；Reactant liquor heating is concentrated into into liquid level and occurs one
Stop heating during layer crystal film, natural cooling crystallization leaches crystal, and the pale yellow crystals of gained are placed in into vacuum and is
24h is dried in 40Kpa, 60 DEG C of vacuum drying oven, the ammino palladium 21.21g of dichloro four is obtained, yield is 85.3%.
Jing atomic emission spectrums are determined, and the content of palladium is 42.8% in product.
In this comparative example, the ultraviolet light chemical reactor is provided with 3 ultraviolet lamp tubes, and 3 ultraviolet lamp tubes enclose
It is equidistantly spaced around the reactor tube, and parallel with the reactor tube, the reactor tube and each described purple
The distance between outer fluorescent tube is equal.
Comparative example 2
The preparation method of the ammino palladium of dichloro four described in this comparative example, comprises the steps：
The palladium bichloride powder of 17.73g is dividedly in some parts in the hydrochloric acid solution of 200ml, 1mol/L, 30min is to chlorination for stirring
Palladium powder is completely dissolved, that is, obtain chlorine palladium acid solution；
Add the deionized water of 500ml in above-mentioned chlorine palladium acid solution, use quality flowmeter and Jing gas distributors with
The flow of 5ml/s to chlorine palladium aqueous acid bottom is passed through ammonia 32.6min；Reactant liquor heating is concentrated into into liquid level and occurs one layer
Stop heating during epitaxial, natural cooling crystallization leaches crystal, and by the pale yellow crystals of gained be placed in vacuum for 40Kpa,
24h is dried in 60 DEG C of vacuum drying oven, the ammino palladium 20.12g of dichloro four is obtained, yield is 80.75%.
Jing atomic emission spectrums are determined, and the content of palladium is 42.7% in product.
Comparative example 3
The preparation method of the ammino palladium of dichloro four described in this comparative example, comprises the steps：
The palladium bichloride powder of 17.73g is dividedly in some parts in the hydrochloric acid solution of 200ml, 1mol/L, 30min is to chlorination for stirring
Palladium powder is completely dissolved, that is, obtain chlorine palladium acid solution；
Above-mentioned chlorine palladium acid solution is transferred in the good reactor tube of translucency, and be added thereto to 500ml go from
Sub- water, then the reactor tube is placed in ultraviolet light chemical reactor, opening uviol lamp (wavelength of ultraviolet light is set as 200nm,
The mass ratio of its intensity and palladium is 60000cd/g), and make ultraviolet light vertical incidence to reactor tube；Use quality flow
Simultaneously Jing gas distributors are passed through ammonia 32.6min to meter with the flow of 5ml/s to chlorine palladium aqueous acid bottom；Reactant liquor is heated
It is concentrated into liquid level to occur stopping heating during a layer crystal film, natural cooling crystallization leaches crystal, and by the pale yellow crystals of gained
Vacuum is placed in be dried 24h in 40Kpa, 60 DEG C of vacuum drying oven, the ammino palladium 21.50g of dichloro four is obtained, yield is
86.27%.
Jing atomic emission spectrums are determined, and the content of palladium is 42.7% in product.
In this comparative example, the ultraviolet light chemical reactor is provided with 3 ultraviolet lamp tubes, and 3 ultraviolet lamp tubes enclose
It is equidistantly spaced around the reactor tube, and parallel with the reactor tube, the reactor tube and each described purple
The distance between outer fluorescent tube is equal.
Obviously, above-described embodiment is only intended to clearly illustrate example, and not to the restriction of embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description other multi-forms change or
Change.There is no need to be exhaustive to all of embodiment.And the obvious change thus extended out or
Among changing still in the protection domain of the invention.
Claims (7)
1. the preparation method of the ammino palladium of a kind of dichloro four, it is characterised in that at least comprise the steps：
Under the ultraviolet light of 280-380nm, chlorine palladium acid solution reacts with ammonia, generates the ammino palladium of dichloro four；
The intensity of the ultraviolet light is 600~60000cd/g with the mass ratio of palladium in the chlorine palladium acid solution；The ultraviolet light
In the reaction system of vertical incidence to chlorine palladium acid solution and ammonia.
2. the preparation method of the ammino palladium of dichloro according to claim 1 four, it is characterised in that reactor tube is ultraviolet with multiple
Fluorescent tube be arranged in parallel, and the ultraviolet lamp tube is equidistantly spaced around the reactor tube, and the reactor tube and each
The distance between the ultraviolet lamp tube is equal.
3. the preparation method of the ammino palladium of dichloro according to claim 1 four, it is characterised in that in chlorine palladium acid solution and ammonia
Reaction system in palladium content be less than 60g/L.
4. the preparation method of the ammino palladium of dichloro according to claim 3 four, it is characterised in that the purity of the ammonia is
99.99%-99.999%.
5. the preparation method of the ammino palladium of dichloro four according to any one of claim 1-4, it is characterised in that the ammonia Jing
Gas distributor is entered in the reaction system of chlorine palladium acid solution and ammonia.
6. the preparation method of the ammino palladium of dichloro according to claim 5 four, it is characterised in that the ammonia and the chlorine palladium
The mol ratio of the chlorine palladium acid in acid solution is 4: 1.
7. the preparation method of the ammino palladium of dichloro four according to claim 1,2,3,4 or 6, it is characterised in that question response is complete
Cheng Hou, reaction system is filtered, plus hot filtrate to liquid level occurs stopping heating during epitaxial, and cooling crystallization is collected and drying crystalline
Thing, obtains final product the ammino palladium of the dichloro four.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102616869A (en) * | 2012-04-07 | 2012-08-01 | 昆明贵金属研究所 | Tetrammine palladium sulphate synthesis method |
| CN103846086A (en) * | 2014-03-05 | 2014-06-11 | 四川大学 | Catalyst for preparing nitric oxides through catalytic ammonia oxidation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| DE102007025358A1 (en) * | 2007-05-31 | 2009-01-08 | Süd-Chemie AG | Process for the preparation of a coated with Pd and / or Au shell catalyst |
| PL240163B1 (en) * | 2014-02-14 | 2022-02-28 | Univ Warszawski | Method for producing pure nanoparticles of noble metals with walls(100), nanoparticles obtained by this method and their application |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102616869A (en) * | 2012-04-07 | 2012-08-01 | 昆明贵金属研究所 | Tetrammine palladium sulphate synthesis method |
| CN103846086A (en) * | 2014-03-05 | 2014-06-11 | 四川大学 | Catalyst for preparing nitric oxides through catalytic ammonia oxidation |
Non-Patent Citations (2)
| Title |
|---|
| 制备高活性二氯四氨合钯(II)的工艺研究;王大维等;《贵金属》;20141130;第35卷(第S1期);第122-125页 * |
| 氯会巴酸铰的光反应研究;张素清等;《云南师范大学学报》;19920331;第12卷(第1期);第41-44页 * |
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