CN102909078B - 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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- CN102909078B CN102909078B CN201210411408.9A CN201210411408A CN102909078B CN 102909078 B CN102909078 B CN 102909078B CN 201210411408 A CN201210411408 A CN 201210411408A CN 102909078 B CN102909078 B CN 102909078B
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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 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 ABS plastic material in producing.Owing to thering is larger application future and market, be 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.Current existing palladium catalyst is active general, conventionally the palladium metal content in palladium catalyst working solution need to be brought up to 50～100ppm and just can guarantee that palladium catalyst working solution can work continually and steadily, otherwise can have an immense impact on to subsequent chemistry nickel operation; And palladium catalyst is directly configured to working solution conventionally at present, when being configured to concentrate, easily occurs unstable, and in process of production, there will be palladium bichloride to separate out and cause waste, palladium bichloride cost accounts for the overwhelming majority of whole cost simultaneously, has therefore improved the cost of catalyst.
Utility model content
For the defect existing in 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:
As improvement, this palladium catalyst concentrate also comprises the malic acid of 1～5g/L.
Another object of the present invention is to provide a kind of preparation method of high-activity palladium concentrated catalyst solution of above-mentioned chemical plating of non-metal material, comprises the following steps:
A, get load weighted hydrochloric acid and be dissolved in and in deionized water, obtain hydrochloric acid solution, and this hydrochloric acid solution is divided into two parts;
B, a copy of it hydrochloric acid solution is heated to 40～50 degrees Celsius, and slowly progressively adds palladium bichloride powder, stir, obtain palladium chloride solution;
C, stannous chloride is dissolved in another part of hydrochloric acid solution, then adds successively sodium stannate, ascorbic acid and cinnamic acid, and completely dissolve and obtain stannous chloride solution;
D, under stirring, palladium chloride solution is slowly joined to the mixed liquor that forms palladium bichloride and stannous chloride in stannous chloride solution, and is heated to 105 ℃～110 ℃ boilings, and be incubated 5h at 40～60 ℃ more than, complete.
As preferably, in steps d, the mixed liquor of palladium bichloride and stannous chloride is heated to boiling operation, adopt step heating method, this step heating method is for first by temperature increase to 45～55 ℃ and be incubated 0.5h～1h, then continue to rise to 80 ℃～90 ℃ and be incubated 0.5h～1h, finally by temperature increase to 105 ℃～110 ℃ until boiling, and stop heating.By distributed heating, insulation at 50～70 ℃, 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 being directly 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.Appropriate 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 and dissolves, and be divided into two parts, and a copy of it is heated to 50 ℃, slowly adds 8g palladium bichloride under strong agitation, completely dissolves and obtains palladium chloride solution; The stannous chloride that adds 300g in another part of chlorinated solution, once adds 25g sodium stannate, 1g cinnamic acid and 2g ascorbic acid until completely dissolved, fully stirs until completely dissolve and obtain stannous chloride solution.Then under stirring state, palladium chloride solution is slowly poured in stannous chloride solution, and be heated to 60 ℃ of insulation 1h, continue to be warmed up to about 90 ℃ insulation 1h; Finally be heated to about 110 ℃ boilings, stop immediately heating, and be incubated 8h at 50～80 ℃ more than.The palladium catalyst concentrate that above method obtains is dark-brown clear liquid, and liquid bottom does not have residue, and the utilization rate of palladium bichloride is high.How many common palladium catalyst concentrates there will be residue in process of production, and this residue contains higher Metal Palladium, and in the concentrate that makes to prepare, palladium content reduces, and causes 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.By through the ABS plastic parts of alligatoring at 25 ℃, immerse 30s in palladium catalyst work, then after dispergation, putting into chemical nickel observes, through observation shows that: immerse about 3s left and right in chemical nickel plating solution and start to occur nickel deposition, during 8s left and right, whole plating piece is coated with evenly continuous grizzly chemical nickel coating completely, that is to say that concentration by the preparation of this palladium catalyst concentrate is only for the ABS workpiece of the palladium catalyst working solution of 20ppm left and right start-up time in chemical nickel is 8s.So repetition test is 10 times, and chemical nickel is about 8s start-up time.And common palladium catalyst working solution all needs that the concentration of palladium ion is brought up to 40～50ppm and just can make chemical nickel reach 10s left and right start-up time.
Palladium catalyst working solution, after standing 3 days, is carried out to colorimetric observation, have no color and change.In addition, get and the above-mentioned ABS plastic parts with batch alligatoring, and again immerse in palladium catalyst working solution after 30s, through dispergation, put into chemical nickel, be 12s the start-up time of chemical nickel deposition.Hence one can see that, and palladium catalyst is after standing 3 days, and activity is substantially constant, and there is no variable color, has high stability.
Claims (5)
1. a high-activity palladium concentrated catalyst solution for chemical plating of non-metal material, is characterized in that comprising following component:
2. the high-activity palladium concentrated catalyst solution of chemical plating of non-metal material according to claim 1, is characterized in that: the malic acid that also comprises 1～5g/L.
3. a preparation method for the high-activity palladium concentrated catalyst solution of chemical plating of non-metal material described in claim 1, is characterized in that comprising the following steps:
A, get load weighted hydrochloric acid and be dissolved in and in deionized water, obtain hydrochloric acid solution, and this hydrochloric acid solution is divided into two parts;
B, a copy of it hydrochloric acid solution is heated to 40～50 degrees Celsius, and slowly progressively adds palladium bichloride powder, stir, obtain palladium chloride solution;
C, stannous chloride is dissolved in another part of hydrochloric acid solution, then adds successively sodium stannate, ascorbic acid and cinnamic acid, and completely dissolve and obtain stannous chloride solution;
D, under stirring, palladium chloride solution is slowly joined to the mixed liquor that forms palladium bichloride and stannous chloride in stannous chloride solution, and is heated to 105 ℃～110 ℃ boilings, and be incubated 5h at 40～60 ℃ more than, complete.
4. the preparation method of the high-activity palladium concentrated catalyst solution of chemical plating of non-metal material according to claim 3, it is characterized in that: in steps d, the mixed liquor of palladium bichloride and stannous chloride is heated to boiling operation, adopt step heating method, this step heating method is for first by temperature increase to 45～55 ℃ and be incubated 0.5h～1h, then continue to rise to 80 ℃～90 ℃ and be incubated 0.5h～1h, finally by temperature increase to 105 ℃～110 ℃ until boiling, and stop heating.
5. the preparation method of the high-activity palladium concentrated catalyst solution of 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 true CN102909078B (en) | 2014-09-24 |
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| 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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| 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 |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| US6797312B2 (en) * | 2003-01-21 | 2004-09-28 | Mattson Technology, Inc. | Electroless plating solution and process |
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| 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 |
| 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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