CN107176625A - A kind of production method of the ammonia palladium of sulfuric acid four - Google Patents
A kind of production method of the ammonia palladium of sulfuric acid four Download PDFInfo
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- CN107176625A CN107176625A CN201710258691.9A CN201710258691A CN107176625A CN 107176625 A CN107176625 A CN 107176625A CN 201710258691 A CN201710258691 A CN 201710258691A CN 107176625 A CN107176625 A CN 107176625A
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- sulfuric acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
- C01G55/002—Compounds containing, besides ruthenium, rhodium, palladium, osmium, iridium, or platinum, two or more other elements, with the exception of oxygen or hydrogen
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
- C01G55/001—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/50—Electroplating: Baths therefor from solutions of platinum group metals
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of production method of the ammonia palladium of sulfuric acid four, it includes the steps such as ammoniacal liquor complexing, ion exchange, sulfuric acid neutralization, recrystallization purification, the synthetic method of the present invention production ammonia palladium of sulfuric acid four, technique is simple, byproduct is few, product purity is high, high conversion rate, and the present invention adds baking step in ammoniacal liquor complexing, it thus is avoided that the ammoniacal liquor of surface of solids residual participates in the reactions steps of next step, influence the purity of the ammonia palladium of sulfuric acid four so that the purity of the ammonia palladium of sulfuric acid four has further raising.
Description
Technical field
The present invention relates to chemical field, more particularly to a kind of production method of the ammonia palladium of sulfuric acid four.
Background technology
The ammonia palladium of sulfuric acid four is a kind of novel electroplating product, plates palladium for electronics industry, is mainly used in coating computer master
Plate and network plug, manufacture automobile cat cracker etc..Because its electroplating efficiency is high, and without halogens, wiper ring
Protect, traditional halogen electroplate liquid can be replaced.At present, domestic open source information there is no the ammonia palladium synthesis technique introduction of sulfuric acid four, beautiful
State's patent [US 6346222B1] report drives the nitric acid in palladium nitrate solution using sulfuric acid, obtains palladium sulfate solution, then use ammonia
Water complexing obtains the ammonia palladium of sulfuric acid four.During need largely to use sulfuric acid to drive away nitric acid, excess sulfuric acid is more, accessory substance increase,
And in complexation process, substantial amounts of ammonium sulfate is produced, mixed with the ammonia palladium of sulfuric acid four, it is necessary to which additionally increase product separates work
Sequence, technological process is long, and the yield and quality of product are all more difficult to control.
The content of the invention
It is produced by the invention instant invention overcomes the deficiencies in the prior art there is provided a kind of production method of the ammonia palladium of sulfuric acid four
The ammonia palladium product purity of sulfuric acid four is very high, high conversion rate, the need for disclosure satisfy that existing industrialized production.
A kind of production method of the ammonia palladium of sulfuric acid four, step is as follows：
(1) ammoniacal liquor is complexed：25-35 parts of ammoniacal liquor are heated with stirring to 45-50 DEG C, 8-12 parts of palladium chlorides is then added, stirs
Dissolving is mixed, undissolved particle is then filtered out, obtains settled solution；Then proceed to be warming up to 80-90 DEG C, stirring is concentrated into crystal
Separate out, then stop heating, be cooled to room temperature, separate out a large amount of solid crystals；Solid crystal drying is removed into ammonia, drying temperature is
100-105℃；
(2) ion exchange：The crystalline solid that step (1) is obtained is dissolved in 500-800 parts of water, then uses anion exchange
Resin carry out ion exchange, with silver nitrate solution inspection exchange tail washings in whether remaining Cl- ions, exchange repeatedly, until detect
Cl- ions are not gone out；
(3) sulfuric acid is neutralized：Sulfuric acid is added in solution into step (2) Jing Guo ion exchange, stirs, that is, obtains sulphur
Sour four ammonia palladium solution；
(4) recrystallization purification：The ammonia palladium solution of sulfuric acid four is transferred in evaporator, is evaporated under reduced pressure, is crystallized in solution
Solution can be removed and be cooled to 0 DEG C by thing, a large amount of yellow needles occur, and filtering takes solid to recrystallize 2 times, obtains light
The solid oven drying of yellow, drying temperature is 60-80 DEG C, dries 8-10h, obtained faint yellow needle-like solid is final
The ammonia palladium of product sulfuric acid four；
It is referred to above to number be all parts by weight.
Further, described resin anion (R.A.) be 201 × 2,201 × 4,201 × 7, D290, D296, D371, D382
One or more of mixtures in resin.
Further, described sulfuric acid is 30-40 parts of the sulfuric acid solution that volumetric concentration is 50%, and the number is parts by weight
Number.
Further, the pressure being evaporated under reduced pressure in described step (4) is 0.03MPa, and evaporating temperature is 45-50 DEG C.
Compared with prior art, the beneficial effects of the invention are as follows：The synthetic method of the present invention production ammonia palladium of sulfuric acid four, technique
Simply, byproduct is few, product purity is high, high conversion rate, and the present invention adds baking step in step (1), thus is avoided that
The ammoniacal liquor of surface of solids residual participates in the reactions steps of next step, influences the purity of the ammonia palladium of sulfuric acid four so that the ammonia palladium of sulfuric acid four
Purity have further raising.
Embodiment
With reference to embodiment, the present invention is further illustrated.Embodiments of the present invention are including but not limited to following
Embodiment.
[embodiment 1]
A kind of production method of the ammonia palladium of sulfuric acid four, step is as follows：
(1) ammoniacal liquor is complexed：25kg ammoniacal liquor is heated with stirring to 45 DEG C, then addition 8kg palladium chlorides, stirring and dissolving, so
After filter out undissolved particle, obtain settled solution；Then proceed to be warming up to 80 DEG C, stirring is concentrated into crystal precipitation, Ran Houting
Only heat, be cooled to room temperature, separate out a large amount of solid crystals；Solid crystal drying is removed into ammonia, drying temperature is 100 DEG C, during drying
Between be 5h；
(2) ion exchange：The crystalline solid that step (1) is obtained is dissolved in 500kg water, then uses D371 anion exchanges
Resin carry out ion exchange, with silver nitrate solution inspection exchange tail washings in whether remaining Cl- ions, exchange repeatedly, until detect
Cl- ions are not gone out；
(3) sulfuric acid is neutralized：Volumetric concentration is added in solution into step (2) Jing Guo ion exchange molten for 50% sulfuric acid
Liquid 30kg sulfuric acid, stirs, that is, obtains the ammonia palladium solution of sulfuric acid four；
(4) recrystallization purification：The ammonia palladium solution of sulfuric acid four is transferred in evaporator, is evaporated under reduced pressure, the pressure of reduction vaporization
For 0.03MPa, evaporating temperature is to occur crystal in 45-50 DEG C, solution to remove solution and be cooled to 0 DEG C, is occurred greatly
Yellow needles are measured, filtering takes solid to recrystallize 2 times, obtains flaxen solid oven drying, drying temperature is 60
DEG C, 8h is dried, obtained faint yellow needle-like solid is the final ammonia palladium of product sulfuric acid four.
[embodiment 2]
A kind of production method of the ammonia palladium of sulfuric acid four, step is as follows：
(1) ammoniacal liquor is complexed：35kg ammoniacal liquor is heated with stirring to 50 DEG C, then addition 12kg palladium chlorides, stirring and dissolving, so
After filter out undissolved particle, obtain settled solution；Then proceed to be warming up to 80-90 DEG C, stirring is concentrated into crystal precipitation, then
Stop heating, be cooled to room temperature, separate out a large amount of solid crystals；Solid crystal drying is removed into ammonia, drying temperature is 105 DEG C；
(2) ion exchange：The crystalline solid that step (1) is obtained is dissolved in 800kg water, then uses D382 anion exchanges
Resin carry out ion exchange, with silver nitrate solution inspection exchange tail washings in whether remaining Cl- ions, exchange repeatedly, until detect
Cl- ions are not gone out；
(3) sulfuric acid is neutralized：Volumetric concentration is added in solution into step (2) Jing Guo ion exchange molten for 50% sulfuric acid
Liquid 40kg, stirs, that is, obtains the ammonia palladium solution of sulfuric acid four；
(4) recrystallization purification：Solution is transferred in evaporator, is evaporated under reduced pressure, the pressure of reduction vaporization is 0.03MPa,
Evaporating temperature is 45-50 DEG C, and occurring crystal in solution can remove solution and be cooled to 0 DEG C, a large amount of yellow needles of appearance
Crystallization, filtering takes solid to recrystallize 2 times, obtains flaxen solid oven drying, and drying temperature is 80 DEG C, dries 10h,
Obtained faint yellow needle-like solid is the final ammonia palladium of product sulfuric acid four；
[embodiment 3]
A kind of production method of the ammonia palladium of sulfuric acid four, step is as follows：
(1) ammoniacal liquor is complexed：30kg ammoniacal liquor is heated with stirring to 47.5 DEG C, then addition 10kg palladium chlorides, stirring and dissolving,
Then undissolved particle is filtered out, settled solution is obtained；Then proceed to be warming up to 85 DEG C, stirring is concentrated into crystal precipitation, then
Stop heating, be cooled to room temperature, separate out a large amount of solid crystals；Solid crystal drying is removed into ammonia, drying temperature is 102.5 DEG C；
(2) ion exchange：The crystalline solid that step (1) is obtained is dissolved in 650kg water, then uses anion exchange resin
Carry out ion exchange, with silver nitrate solution inspection exchange tail washings in whether remaining Cl- ions, exchange repeatedly, until examine do not measure
Cl- ions；
(3) sulfuric acid is neutralized：Volumetric concentration is added in solution into step (2) Jing Guo ion exchange molten for 50% sulfuric acid
Liquid 35kg, stirs, that is, obtains the ammonia palladium solution of sulfuric acid four；
(4) recrystallization purification：Solution is transferred in evaporator, is evaporated under reduced pressure, occurring crystal in solution can will be molten
Liquid removes and is cooled to 0 DEG C, a large amount of yellow needles occurs, and filtering takes solid to recrystallize 2 times, obtains flaxen solid
With oven drying, drying temperature is 70 DEG C, dries 9h, obtained faint yellow needle-like solid is the final ammonia of product sulfuric acid four
Palladium
[embodiment 4]
A kind of production method of the ammonia palladium of sulfuric acid four, step is as follows：
(1) ammoniacal liquor is complexed：26kg ammoniacal liquor is heated with stirring to 46 DEG C, then addition 9kg palladium chlorides, stirring and dissolving, so
After filter out undissolved particle, obtain settled solution；Then proceed to be warming up to 81 DEG C, stirring is concentrated into crystal precipitation, Ran Houting
Only heat, be cooled to room temperature, separate out a large amount of solid crystals；Solid crystal drying is removed into ammonia, drying temperature is 101 DEG C；
(2) ion exchange：The crystalline solid that step (1) is obtained is dissolved in 510kg water, then uses anion exchange resin
Carry out ion exchange, with silver nitrate solution inspection exchange tail washings in whether remaining Cl- ions, exchange repeatedly, until examine do not measure
Cl- ions；
(3) sulfuric acid is neutralized：Volumetric concentration is added in solution into step (2) Jing Guo ion exchange molten for 50% sulfuric acid
Liquid 31kg, stirs, that is, obtains the ammonia palladium solution of sulfuric acid four；
(4) recrystallization purification：Solution is transferred in evaporator, is evaporated under reduced pressure, occurring crystal in solution can will be molten
Liquid removes and is cooled to 0 DEG C, a large amount of yellow needles occurs, and filtering takes solid to recrystallize 2 times, obtains flaxen solid
With oven drying, drying temperature is 61 DEG C, dries 8.1h, obtained faint yellow needle-like solid is the final ammonia of product sulfuric acid four
Palladium.
[embodiment 5]
A kind of production method of the ammonia palladium of sulfuric acid four, step is as follows：
(1) ammoniacal liquor is complexed：34kg ammoniacal liquor is heated with stirring to 49 DEG C, then addition 11kg palladium chlorides, stirring and dissolving, so
After filter out undissolved particle, obtain settled solution；Then proceed to be warming up to 90 DEG C, stirring is concentrated into crystal precipitation, Ran Houting
Only heat, be cooled to room temperature, separate out a large amount of solid crystals；Solid crystal drying is removed into ammonia, drying temperature is 104 DEG C；
(2) ion exchange：The crystalline solid that step (1) is obtained is dissolved in 790kg water, then uses anion exchange resin
Carry out ion exchange, with silver nitrate solution inspection exchange tail washings in whether remaining Cl- ions, exchange repeatedly, until examine do not measure
Cl- ions；
(3) sulfuric acid is neutralized：Volumetric concentration is added in solution into step (2) Jing Guo ion exchange molten for 50% sulfuric acid
Liquid 34kg, stirs, that is, obtains the ammonia palladium solution of sulfuric acid four；
(4) recrystallization purification：Solution is transferred in evaporator, is evaporated under reduced pressure, occurring crystal in solution can will be molten
Liquid removes and is cooled to 0 DEG C, a large amount of yellow needles occurs, and filtering takes solid to recrystallize 2 times, obtains flaxen solid
With oven drying, drying temperature is 79 DEG C, dries 9.9h, obtained faint yellow needle-like solid is the final ammonia of product sulfuric acid four
Palladium.
It is embodiments of the invention as described above.The present invention is not limited to the above-described embodiments, anyone should learn that
The structure change made under the enlightenment of the present invention, the technical schemes that are same or similar to the present invention each fall within this
Within the protection domain of invention.
Claims (4)
1. a kind of production method of the ammonia palladium of sulfuric acid four, it is characterised in that step is as follows：
(1) ammoniacal liquor is complexed：25-35 parts of ammoniacal liquor are heated with stirring to 45-50 DEG C, 8-12 parts of palladium chlorides are then added, stirred molten
Solution, then filters out undissolved particle, obtains settled solution；Then proceed to be warming up to 80-90 DEG C, stirring is concentrated into crystal analysis
Go out, then stop heating, be cooled to room temperature, separate out a large amount of solid crystals；Solid crystal drying is removed into ammonia, drying temperature is 100-
105℃；
(2) ion exchange：The crystalline solid that step (1) is obtained is dissolved in 500-800 parts of water, then uses anion exchange resin
Carry out ion exchange, with silver nitrate solution inspection exchange tail washings in whether remaining Cl- ions, exchange repeatedly, until examine do not measure
Cl- ions；
(3) sulfuric acid is neutralized：Sulfuric acid is added in solution into step (2) Jing Guo ion exchange, stirs, that is, obtains sulfuric acid four
Ammonia palladium solution；
(4) recrystallization purification：The ammonia palladium solution of sulfuric acid four is transferred in evaporator, is evaporated under reduced pressure, crystal occurs i.e. in solution
Solution can be removed and be cooled to 0 DEG C, a large amount of yellow needles occur, filtering takes solid to recrystallize 2 times, obtains faint yellow
Solid oven drying, drying temperature be 60-80 DEG C, dry 8-10h, obtained faint yellow needle-like solid is final production
The ammonia palladium of thing sulfuric acid four；
It is referred to above to number be all parts by weight.
2. a kind of production method of the ammonia palladium of sulfuric acid four according to claim 1, it is characterised in that：Described resin anion (R.A.)
For one or more of mixtures in 201 × 2,201 × 4,201 × 7, D290, D296, D371, D382 resin.
3. a kind of production method of the ammonia palladium of sulfuric acid four according to claim 1, it is characterised in that：Described sulfuric acid is volume
Concentration is 50% 30-40 parts of sulfuric acid solution, and the number is parts by weight.
4. a kind of production method of the ammonia palladium of sulfuric acid four according to claim 1, it is characterised in that：In described step (4)
The pressure of reduction vaporization is 0.03MPa, and evaporating temperature is 45-50 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108864200A (en) * | 2018-08-06 | 2018-11-23 | 金川集团股份有限公司 | Plating one one step preparation method of ethylenediamine sulfate palladium |
| CN108946829A (en) * | 2018-08-06 | 2018-12-07 | 金川集团股份有限公司 | A kind of electrodialysis preparation method of four ammonia palladium of sulfuric acid |
| CN112429785A (en) * | 2020-12-07 | 2021-03-02 | 辽宁石油化工大学 | Preparation method of analytically pure platinum tetrachloride |
| CN112897600A (en) * | 2021-03-15 | 2021-06-04 | 徐州浩通新材料科技股份有限公司 | Preparation method of tetraamminepalladium sulfate (II) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6346222B1 (en) * | 1999-06-01 | 2002-02-12 | Agere Systems Guardian Corp. | Process for synthesizing a palladium replenisher for electroplating baths |
| CN101838830A (en) * | 2010-05-07 | 2010-09-22 | 厦门大学 | Electrolyte of electroplating palladium-nickel alloy |
| CN102786100A (en) * | 2012-08-30 | 2012-11-21 | 贵研资源（易门）有限公司 | Synthetic method of palladium tetra-ammino sulfate |
-
2017
- 2017-04-19 CN CN201710258691.9A patent/CN107176625A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6346222B1 (en) * | 1999-06-01 | 2002-02-12 | Agere Systems Guardian Corp. | Process for synthesizing a palladium replenisher for electroplating baths |
| CN101838830A (en) * | 2010-05-07 | 2010-09-22 | 厦门大学 | Electrolyte of electroplating palladium-nickel alloy |
| CN102786100A (en) * | 2012-08-30 | 2012-11-21 | 贵研资源（易门）有限公司 | Synthetic method of palladium tetra-ammino sulfate |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108864200A (en) * | 2018-08-06 | 2018-11-23 | 金川集团股份有限公司 | Plating one one step preparation method of ethylenediamine sulfate palladium |
| CN108946829A (en) * | 2018-08-06 | 2018-12-07 | 金川集团股份有限公司 | A kind of electrodialysis preparation method of four ammonia palladium of sulfuric acid |
| CN108864200B (en) * | 2018-08-06 | 2020-12-11 | 金川集团股份有限公司 | One-step preparation method of ethylenediamine palladium sulfate for electroplating |
| CN112429785A (en) * | 2020-12-07 | 2021-03-02 | 辽宁石油化工大学 | Preparation method of analytically pure platinum tetrachloride |
| CN112897600A (en) * | 2021-03-15 | 2021-06-04 | 徐州浩通新材料科技股份有限公司 | Preparation method of tetraamminepalladium sulfate (II) |
| CN112897600B (en) * | 2021-03-15 | 2021-11-19 | 徐州浩通新材料科技股份有限公司 | Preparation method of tetraamminepalladium sulfate (II) |
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