CN102909078A - Non-metallic material chemical plating high-activity palladium catalyst concentrated solution and preparation method thereof - Google Patents
Non-metallic material chemical plating high-activity palladium catalyst concentrated solution and preparation method thereof Download PDFInfo
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- CN102909078A CN102909078A CN2012104114089A CN201210411408A CN102909078A CN 102909078 A CN102909078 A CN 102909078A CN 2012104114089 A CN2012104114089 A CN 2012104114089A CN 201210411408 A CN201210411408 A CN 201210411408A CN 102909078 A CN102909078 A CN 102909078A
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Abstract
The invention discloses a non-metallic material chemical plating high-activity palladium catalyst concentrated solution and a preparation method thereof. The non-metallic material chemical plating high-activity palladium catalyst concentrated solution comprises the following components: 1-10g/L of palladium chloride, 200-400ml/L of muriatic acid, 200-400g/L of stannous chloride, 10-50g/L of sodium stannate, 1-5g/L of ascorbic acid, 0.5-2g/L of cinnamyl aldehyde and the balance of deionized water. The non-metallic material chemical plating high-activity palladium catalyst concentrated solution has high catalytic activity and the preparation method of the non-metallic material chemical plating high-activity palladium catalyst concentrated solution is high in utilization rate of palladium chloride.
Description
Technical field
The invention belongs to the inorganic functional material field, relate in particular to the palladium catalyst of using for the chemical plating pre-treatment of nonmetallic materials especially ABS.
Background technology
Electroplating industry is carried out metallized research at non-metal material surface, especially the ABS plastic material in producing.Owing to have larger application future and market has been subjected to increasing attention.In the metallized process of nonmetallic materials, the performance of palladium catalyst is to be related to one of metallized key factor of nonmetallic materials.At present existing palladium catalyst is active general, usually the palladium metal content in the palladium catalyst working solution need to be brought up to 50～100ppm and can guarantee that just the palladium catalyst working solution can work continually and steadily, otherwise can have an immense impact on to subsequent chemistry nickel operation; And palladium catalyst directly is configured to working solution usually at present, when being configured to concentrate, occurs easily unstable, and in process of production, palladium bichloride can occur and separate out and cause waste, the palladium bichloride cost accounts for the overwhelming majority of whole cost simultaneously, has therefore improved the cost of catalyst.
Summary of the invention
For the defective that exists in the prior art and technical problem, the invention provides a kind of.
For solving the problems of the technologies described above, the present invention by the following technical solutions: a kind of high-activity palladium concentrated catalyst solution of chemical plating of non-metal material comprises following component:
Palladium bichloride 1～10g/L;
Hydrochloric acid 200～400ml/L;
Stannous chloride 200～400g/L;
Sodium stannate 10～50g/L;
Ascorbic acid 1～5g/L;
Cinnamic acid 0.5～2g/L, and the deionized water of surplus.
As improvement, this palladium catalyst concentrate also comprises the malic acid of 1～5g/L.
Another purpose of the present invention provides a kind of preparation method of high-activity palladium concentrated catalyst solution of above-mentioned chemical plating of non-metal material, may further comprise the steps:
A, get load weighted hydrochloric acid and be dissolved in and obtain hydrochloric acid solution in the deionized water, and this hydrochloric acid solution is divided into two parts;
B, a copy of it hydrochloric acid solution is heated to 40～50 degrees centigrade, and slowly progressively adds the palladium bichloride powder, stir, obtain palladium chloride solution;
C, stannous chloride is dissolved in another part hydrochloric acid solution, then adds successively sodium stannate, ascorbic acid and cinnamic acid, and dissolving obtains stannous chloride solution fully;
D, under stirring, palladium chloride solution is slowly joined in the stannous chloride solution mixed liquor that forms palladium bichloride and stannous chloride, and is heated to 105 ℃～110 ℃ boilings, and more than 40～60 ℃ of lower insulation 5h, finish.
As preferably, in the steps d, the mixed liquor of palladium bichloride and stannous chloride is heated to the boiling operation, adopt step heating method, this step heating method is at first with temperature increase to 45～55 ℃ and be incubated 0.5h～1h, then continue to rise to 80 ℃～90 ℃ and be incubated 0.5h～1h, at last with temperature increase to 105 ℃～110 ℃ until boiling, and stopped heating.By distributed heating, 50～70 ℃ of lower insulations, Metal Palladium ion and divalent tin ion form active force and are fully wrapped up by divalent tin ion, and then a large amount of chlorions of collection of crowding around outside, thereby form the palladium ion active particle of preliminarily stabilised.With respect to directly being heated to boiling, distributed heating means more can improve the stability of palladium ion active particle.
Further, the malic acid that adds 1～5g/L in the stannous chloride solution that step c obtains.An amount of malic acid can participate in the complexing of palladium ion, is conducive to the stability of palladium catalyst concentrate.
Beneficial effect: with respect to prior art, the present invention has the following advantages: palladium catalyst concentrate of the present invention has high catalytic activity, and its preparation method is high to the utilization rate of palladium bichloride.
The specific embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
The hydrochloric acid that adds 300ml in the deionized water of 1000ml stirs fully dissolving, and is divided into two parts, and a copy of it is heated to 50 ℃, slowly adds the 8g palladium bichloride under strong agitation, and dissolving obtains palladium chloride solution fully; Add the stannous chloride of 300g in another part chlorinated solution, once add until completely dissolved 25g sodium stannate, 1g cinnamic acid and 2g ascorbic acid, fully stir until fully dissolving obtain stannous chloride solution.Then under stirring state, palladium chloride solution is slowly poured in the stannous chloride solution, and be heated to 60 ℃ of insulation 1h, continue to be warmed up to about 90 ℃ and be incubated 1h; Be heated at last about 110 ℃ boiling, stopped heating immediately, and more than 50～80 ℃ of lower insulation 8h.The palladium catalyst concentrate that above method obtains is the dark-brown clear liquid, and liquid bottom does not have residue, and the utilization rate of palladium bichloride is high.What residue can occur to common palladium catalyst concentrate in process of production, and this residue contains higher Metal Palladium, so that palladium content in the concentrate of preparation, and cause waste.
Press proportioning: the hydrochloric acid of 4ml/L palladium catalyst concentrate, 100ml/L and 150g/L sodium chloride, thereby configuration palladium catalyst working solution.Will be through the ABS plastic parts of alligatoring under 25 ℃, immerse 30s in the palladium catalyst work, then putting into chemical nickel behind dispergation observes, through observation shows that: namely begin to occur the nickel deposition about about 3s in the immersion chemical nickel plating bath, whole plating piece is coated with evenly continuous grizzly chemical nickel coating fully during the 8s left and right sides, that is to say that the concentration by the preparation of this palladium catalyst concentrate is 8s for the start-up time of ABS workpiece in chemical nickel of the palladium catalyst working solution about 20ppm only.So repetition test is 10 times, and chemical nickel is about 8s start-up time.And common palladium catalyst working solution all needs the concentration of palladium ion is brought up to 40～50ppm ability so that chemical nickel reaches about 10s start-up time.
After the palladium catalyst working solution left standstill 3 days, carry out colorimetric and observe, have no color and change.In addition, get and above-mentioned ABS plastic parts with batch alligatoring, and again immerse in the palladium catalyst working solution behind the 30s, put into chemical nickel through dispergation, be 12s the start-up time of chemical nickel deposition.Hence one can see that, and palladium catalyst is after leaving standstill 3 days, and activity is substantially constant, and does not have variable color, has high stability.
Claims (5)
1. the high-activity palladium concentrated catalyst solution of a chemical plating of non-metal material is characterized in that comprising following component:
Palladium bichloride 1～10g/L;
Hydrochloric acid 200～400ml/L;
Stannous chloride 200～400g/L;
Sodium stannate 10～50g/L;
Ascorbic acid 1～5g/L;
Cinnamic acid 0.5～2g/L, and the deionized water of surplus.
2. the high-activity palladium concentrated catalyst solution of described chemical plating of non-metal material according to claim 1 is characterized in that: the malic acid that also comprises 1～5g/L.
3. the preparation method of the high-activity palladium concentrated catalyst solution of the described chemical plating of non-metal material of claim 1 is characterized in that may further comprise the steps:
A, get load weighted hydrochloric acid and be dissolved in and obtain hydrochloric acid solution in the deionized water, and this hydrochloric acid solution is divided into two parts;
B, a copy of it hydrochloric acid solution is heated to 40～50 degrees centigrade, and slowly progressively adds the palladium bichloride powder, stir, obtain palladium chloride solution;
C, stannous chloride is dissolved in another part hydrochloric acid solution, then adds successively sodium stannate, ascorbic acid and cinnamic acid, and dissolving obtains stannous chloride solution fully;
D, under stirring, palladium chloride solution is slowly joined in the stannous chloride solution mixed liquor that forms palladium bichloride and stannous chloride, and is heated to 105 ℃～110 ℃ boilings, and more than 40～60 ℃ of lower insulation 5h, finish.
4. the preparation method of the high-activity palladium concentrated catalyst solution of described chemical plating of non-metal material according to claim 4, it is characterized in that: in the steps d, the mixed liquor of palladium bichloride and stannous chloride is heated to the boiling operation, adopt step heating method, this step heating method is at first with temperature increase to 45～55 ℃ and be incubated 0.5h～1h, then continue to rise to 80 ℃～90 ℃ and be incubated 0.5h～1h, at last with temperature increase to 105 ℃～110 ℃ until boiling, and stopped heating.
5. the preparation method of the high-activity palladium concentrated catalyst solution of described chemical plating of non-metal material according to claim 4 is characterized in that: the malic acid that adds 1～5g/L in the stannous chloride solution that step c obtains.
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| CN201210411408.9A CN102909078B (en) | 2012-10-25 | 2012-10-25 | Non-metallic material chemical plating high-activity palladium catalyst concentrated solution and preparation method thereof |
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| CN201210411408.9A CN102909078B (en) | 2012-10-25 | 2012-10-25 | Non-metallic material chemical plating high-activity palladium catalyst concentrated solution and preparation method thereof |
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| CN102909078B CN102909078B (en) | 2014-09-24 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110318043A (en) * | 2018-03-28 | 2019-10-11 | 东莞市斯坦得电子材料有限公司 | A kind of high stability, the colloid palladium manufacture craft of high activity |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1334358A (en) * | 2001-08-09 | 2002-02-06 | 华南师范大学 | Process for preparing concentrated liquid specially adapted for chemical spray coating of Ni and its application method |
| US20040142114A1 (en) * | 2003-01-21 | 2004-07-22 | Mattson Technology, Inc. | Electroless plating solution and process |
| CN1947845A (en) * | 2005-10-14 | 2007-04-18 | 中国电子科技集团公司第十八研究所 | Carried catalyst chemical plating method for hydrolyzing hydroborates to produce hydrogen |
| CN101928937A (en) * | 2009-06-22 | 2010-12-29 | 比亚迪股份有限公司 | Colloid palladium activation solution, preparation method thereof and non-metal surface activation method |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1334358A (en) * | 2001-08-09 | 2002-02-06 | 华南师范大学 | Process for preparing concentrated liquid specially adapted for chemical spray coating of Ni and its application method |
| US20040142114A1 (en) * | 2003-01-21 | 2004-07-22 | Mattson Technology, Inc. | Electroless plating solution and process |
| CN1947845A (en) * | 2005-10-14 | 2007-04-18 | 中国电子科技集团公司第十八研究所 | Carried catalyst chemical plating method for hydrolyzing hydroborates to produce hydrogen |
| CN101928937A (en) * | 2009-06-22 | 2010-12-29 | 比亚迪股份有限公司 | Colloid palladium activation solution, preparation method thereof and non-metal surface activation method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110318043A (en) * | 2018-03-28 | 2019-10-11 | 东莞市斯坦得电子材料有限公司 | A kind of high stability, the colloid palladium manufacture craft of high activity |
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