CN1151972C - Palladium chloride producing process - Google Patents
Palladium chloride producing process Download PDFInfo
- Publication number
- CN1151972C CN1151972C CNB021572259A CN02157225A CN1151972C CN 1151972 C CN1151972 C CN 1151972C CN B021572259 A CNB021572259 A CN B021572259A CN 02157225 A CN02157225 A CN 02157225A CN 1151972 C CN1151972 C CN 1151972C
- Authority
- CN
- China
- Prior art keywords
- dissolving liquid
- palladium sponge
- palladium
- weight
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Manufacture And Refinement Of Metals (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention discloses a palladium chloride producing method. Palladium sponge powder with the purity larger than 99.95% is put into a beaker of 5 liters; then, analysis pure and concentrated hydrochloric acid with weight of 3 to 4 times of the weight of the palladium sponge powder is added to the beaker, and the temperature of dissolving liquid is heated to be from 60 to 70 DEG C; analysis pure hydrogen peroxide with weight of 1 to 2 times of the weight of the palladium sponge powder is slowly added to the dissolving liquid in batches, and the mixture is continuously stirred; after the dissolving liquid is filtered and concentrated, the dissolving liquid is evaporated to be in a thick state, and the thick dissolving liquid is put into a drying oven to be dried; the dissolving liquid is taken out to be ground into powder. Thus, a palladium chloride product is obtained. When the palladium sponge powder is dissolved, hydrogen peroxide replaces nitric acid to be used as an oxidizing agent to cause the dissolving liquid to contain no nitrate. Consequently, the detection of nitrate indexes can be omitted during product inspection. Simultaneously, when the dissolving liquid is concentrated and evaporated, redundant nitric acid can not be exhausted, and production period is shortened. No oxynitride gas is generated during the production course, no pollution exists, and yield is high.
Description
Technical field
The present invention relates to a kind of method of producing fine chemical product, the production method of especially producing Palladous chloride.
Background technology
Palladous chloride is mainly used in the surfactant that preparation extraordinary catalyzer, molecular sieve and preparation non-conductive material coating uses etc., traditional production method is mainly the aqua regia dissolution method, this method needs repeatedly to add concentrated hydrochloric acid to catch up with nitric acid unnecessary in the most lysate in the lysate evaporative process in batches, thereby cause a large amount of toxic gas oxynitrides gaseous volatilizations, and easily cause the loss of overflowing of palladium liquid.Nitrate content requires to be not more than 0.05% in the product palladium.
Summary of the invention
The objective of the invention is to provide a kind of with short production cycle, easy and simple to handle, yield rate is high, do not produce the Palladous chloride production method of oxynitrides toxic gas.
The object of the present invention is achieved like this: the palladium sponge powder of purity＞99.95% is put into 5 liters of beakers, add palladium sponge grain weight amount 3-4 analytical pure concentrated hydrochloric acid doubly then, lysate is heated to 60-70 ℃, and the slow palladium sponge grain weight amount 1-2 analytical pure hydrogen peroxide doubly that in batches adds, constantly stir, then lysate filtering and concentrating post-heating is evaporated to thick shape, put into drying in oven, taking-up grinds to form powdery, promptly gets the Palladous chloride product.
The drying baker temperature remains on below 150 ℃ during oven dry, and is interrupted and stirs.
Before taking out, baking oven needs whether also have the hydrogen chloride gas volatilization with the ammoniacal liquor check.
Advantage of the present invention: use hydrogen peroxide to replace nitric acid as oxidant during the dissolving of palladium sponge powder, make and do not contain nitrate in the lysate, therefore the detection that can omit the nitrate index during examination and test of products need not be caught up with unnecessary to the greatest extent nitric acid during the lysate concentration and evaporation simultaneously, has shortened the production cycle; No oxynitrides gas produces in the production process, and is pollution-free and yield is high.
Embodiment
Get the palladium sponge powder of 500 gram purity＞99.95%, put into 5 liters of beakers, add the analytical pure concentrated hydrochloric acid of 1500 grams, lysate is heated to 65 ℃ on electricradiator, slowly add the analytical pure hydrogen peroxide of 750 grams then in batches, add fashionable continuous stirring and dissolving liquid, then lysate filtering and concentrating post-heating is evaporated to thick shape, the baking oven of putting into 100 ℃ stirred once in 1 hour, up to oven dry, taking-up grinds to form powdery, promptly gets the Palladous chloride product.But before in baking oven, taking out, need whether also have the hydrogen chloride gas volatilization with the ammoniacal liquor check.The result is as follows:
| Lot number | Palladium sponge powder input amount | The Palladous chloride product | Yield rate (%) |
| 1 | 500 grams | 831.82 | 99.81 |
| 2 | 500 grams | 831.53 | 99.78 |
| 3 | 500 grams | 830.01 | 99.60 |
The Palladous chloride product is a brown ceramic powder, is dissolved in hydrochloric acid, ethanol, acetone and Hydrogen bromide.Analytical results is as follows:
1. constituent content (%) Pd59.85 in the product; Pt0.005; Au0.005; Rh0.005; Fe0.005; Ir0.005; Ni0.003; Pb＜0.0001; As≤50ppb.
2. the diluted hydrochloric acid dissolution test meets the GB8185-87 index.
3. nitrate detects: do not have.
Claims (3)
1. Palladous chloride production method, it is characterized in that the palladium sponge powder of purity＞99.95% is put into 5 liters of beakers, add palladium sponge grain weight amount 3-4 analytical pure concentrated hydrochloric acid doubly then, lysate is heated to 60-70 ℃, and slowly adds palladium sponge grain weight amount 1-2 analytical pure hydrogen peroxide doubly in batches, constantly stirs, then lysate filtering and concentrating post-heating is evaporated to thick shape, put into drying in oven, take out and grind to form powdery, promptly get the Palladous chloride product.
2. Palladous chloride production method according to claim 1, the drying baker temperature remains on below 150 ℃ when it is characterized in that drying, and is interrupted and stirs.
3. Palladous chloride production method according to claim 1 is characterized in that needing whether also have the hydrogen chloride gas volatilization with the ammoniacal liquor check before baking oven takes out.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021572259A CN1151972C (en) | 2002-12-19 | 2002-12-19 | Palladium chloride producing process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021572259A CN1151972C (en) | 2002-12-19 | 2002-12-19 | Palladium chloride producing process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1421395A CN1421395A (en) | 2003-06-04 |
| CN1151972C true CN1151972C (en) | 2004-06-02 |
Family
ID=4752890
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021572259A Expired - Fee Related CN1151972C (en) | 2002-12-19 | 2002-12-19 | Palladium chloride producing process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1151972C (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102311147A (en) * | 2010-07-07 | 2012-01-11 | 中国石油化工股份有限公司 | Method for preparing palladium nitrate |
| CN102838469B (en) * | 2011-06-23 | 2015-02-25 | 中国石油化工股份有限公司 | Preparation method for palladium acetylacetonate |
| CN102390875A (en) * | 2011-08-06 | 2012-03-28 | 河南兴发精细化工有限公司 | Method for preparing palladium chloride solution in process of producing sodium gluconate by using multielement metal catalytic oxidation method |
| CN102557156A (en) * | 2011-12-15 | 2012-07-11 | 无锡威孚环保催化剂有限公司 | Method for preparing palladium nitrate solution |
| EP2987571B1 (en) * | 2014-08-19 | 2018-08-15 | Heraeus Deutschland GmbH & Co. KG | Method for the production of active palladium (0) powder, active palladium (0) powder and its use in making a palladium salt |
| CN104773765A (en) * | 2015-05-05 | 2015-07-15 | 昆明正江工贸有限责任公司 | Preparing method of analytically-pure palladium chloride |
| CN106430333B (en) * | 2016-08-30 | 2018-03-20 | 昆明铂磊科技有限公司 | A kind of production technology of palladium bichloride |
| CN109384266A (en) * | 2018-10-30 | 2019-02-26 | 金川集团股份有限公司 | A method of preparing palladium chloride |
| CN110194493A (en) * | 2019-05-28 | 2019-09-03 | 苏州美源达环保科技股份有限公司 | A kind of palladium chloride green synthesis method |
| CN115707658A (en) * | 2022-12-20 | 2023-02-21 | 沈阳中色稀贵金属新材料有限公司 | Method for efficiently preparing ammonium tetrachloropalladate |
-
2002
- 2002-12-19 CN CNB021572259A patent/CN1151972C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1421395A (en) | 2003-06-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1151972C (en) | Palladium chloride producing process | |
| CN103554510B (en) | A kind of Amino End Group modified-cellulose and its preparation method and application | |
| CN109745984A (en) | A kind of preparation method of the monatomic doped carbon nanometer pipe of metal | |
| CN104368316B (en) | A kind of hydrosulfide group cellulose class stalk adsorbent and preparation method and the recovery to noble silver | |
| CN106000333B (en) | The preparation method of the material of Adsorption of Lead | |
| CN105174859A (en) | Diatomite micropowder-based interior wall paint capable of removing formaldehyde and peculiar smell in indoor air and preparation method thereof | |
| CN105148917A (en) | Method for improving catalysis efficiency of formaldehyde catalyst, and formaldehyde catalyst thereof | |
| CN102614836A (en) | Method for adsorbing and recovering precious metal palladium by persimmon tannin-containing metal adsorbent | |
| CN110734063A (en) | method for preparing rice hull based nitrogen-doped active carbon | |
| CN101691225A (en) | Method for coproducing nano silicon dioxide and active carbon from rice hull ash | |
| CN1663986A (en) | Technology for producing yellow humic acid by using coal | |
| CN102847554A (en) | Preparation method and application of cotton stalk bast fiber loaded nano gold catalyst | |
| CN106276895B (en) | A kind of preparation method of amberlite aliphatic radical carbon material | |
| CN111945420B (en) | Environment-friendly silver fiber fabric and preparation method thereof | |
| CN106390930B (en) | A kind of method that glycine prepares active carbon loading silver with silver nitrate complexing | |
| CN112718014A (en) | Treatment method of catalyst carrier, catalyst for preparing methanol by carbon dioxide hydrogenation, preparation method and application thereof | |
| CN109775760B (en) | Ultra-low potassium ammonium molybdate solution, ammonium molybdate solution derivative product and preparation method thereof | |
| CN110484269A (en) | A kind of heavy-metal contaminated soil renovation agent and its preparation and application method | |
| CN114517262B (en) | Recovery process of lead in waste lead storage battery | |
| Yuantao et al. | Platinum loss from alloy catalyst gauzes in nitric acid plants | |
| CN113929090A (en) | Preparation method of graphene | |
| CN112266292A (en) | Slow-release compound fertilizer and preparation method thereof | |
| CN113428913B (en) | Preparation process of palladium nitrate solution | |
| CN111203207A (en) | Catalyst for reducing p-nitrophenol and preparation method and application thereof | |
| CN116621647B (en) | Method for preparing humic acid slow-release trace element fertilizer by efficiently activating lignite through MOF derivative |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |