Palladium catalyst recycling technology 1. Wen-hai 2. Huangdeng Jiang (1. Liuzhou environmental monitoring detachment, Liuzhou 545001; 2.

Liuzhou environmental protection monitoring station, Liuzhou 545001) Abstract Palladium catalysts are widely used in chemical industry, and its inactivation to be significant, the recovery of palladium has a greater economic value. Describes the different types of palladium catalyst recycling waste carrier purification methods. Key words Pd; catalyst; recovery Key Words TQ426.83 Document code A Article ID 1003-2673 (2008) 11-20-02 1. Introduction palladium is a metal, hydrogen and oxygen on the adsorption capacity with a special, widely used in the catalyst industry. Many different types of palladium catalysts, most used in the petrochemical industry and catalytic hydrogenation and oxidation reactions, such as the preparation of acetaldehyde, pyridine derivatives, vinyl acetate and a variety of chemical reaction products [1]. Mass content of palladium in the catalyst is generally the very few to a few percent. Expensive and limited resources, palladium, palladium catalyst deactivation is mainly the growth of palladium to catalytic activity of the grain size decreases, the coverage and poisoning of impurities and other reasons. And palladium are good corrosion resistance, high temperature performance and stable electrical properties, the loss of palladium during the reaction was not great, the waste palladium catalyst Pd content compared with the difference between the fresh catalyst is not, therefore, spent catalysts Palladium for a more complete recovery to be possible. So far, palladium catalyst preparation methods are impregnation, vapor deposition of metal ions, solvated metal atom impregnation, ion exchange, sol - gel method. Palladium catalyst dispersed in suitable carrier to use, for different reactions, the largest carrier for the present study, activated carbon, aluminum oxide, zeolite and zeolite, ceramics, silicone and so on. Under the palladium catalyst preparation methods and

Lin Yimin et al [2] for related experiments. using the appropriate treatment process. Activated carbon supported palladium catalyst 2 Pd catalysts are widely used in pharmaceutical and chemical industries. technology is relatively simple. reduce resource waste. burning device design will become a research priority.) dissolved palladium. ****. characterized by using less chemicals. palladium recovery rate of increase. resulting in the loss of palladium. After a long use. but also by the corresponding method of recycling. titanium and other impurities. etc. Domestic Wuguan Min et al [3] palladium recovery incinerator designed system. the reduction of oxidized palladium into palladium metal. scrubbers. oxidizing agents (aqua regia. a waste catalyst. effectively . Usually by reducing agents such as combustion residues (hydrazine hydrate. Palladium in the form of ash left behind to be enriched. Dissolved with hydrochloric acid. blast equipment. chimney structure. roasting to purification. **** for example. the results show that the recovery rate of waste palladium carbon catalyst is the burning of the most important aspects of palladium in the solution. follow-up procedure is slightly different. acid hydrogenation reactions are used palladium / activated carbon catalyst. Palladium carbon catalyst to improve the recovery rate of waste.different carriers. filters. the palladium catalyst contaminated by impurities loss of activity. Palladium particles in the incineration process is easy with the burning of the gas out of the incinerator. according to the composition of ash. the process of reduction and purification loss is minimal. the burning furnace. **** diisocyanate synthesis and purification of caprolactam. but generally will be dissolved palladium complex with ammonia to form a precipitate drying. formic acid) reduction. after which iron. Will air at 800-1500 volatile coal combustion into CO2 removed. From spent Pd / activated carbon catalyst for the recovery of palladium is currently the most widely incineration. so incineration is the most important steps in the process of burning.

and the value of recycling of these catalysts is also relatively large. propylene hydrogenation of crude off the propargyl and pyrolysis gasoline hydrogenation. 3Al2O3 catalyst such palladium catalysts is mainly Al2O3 as the carrier.inhibited the loss of palladium. That of an alkali metal or alkaline earth metal carbonate as additive in the 700 ~ 800 . Al2O3 supported catalyst for recycling of the most widely used technology at home and abroad are roasting leaching method and sublimation. Palladium content of active component in the very few with a few per thousand.95%. hydrochloric acid dissolution method added oxidants. This process. the palladium recovery rate of 95% or more.1 The first roasting leaching palladium catalyst waste sometime in the high temperature baking to remove impurities and volatile organic compounds which. In addition to burning solution method but also have a soda leaching. and then separated by electrolysis Pd. sulfuric acid dissolving carrier and so on. Surface of the catalyst metal particles increases and the sintering hydrocarbons catalytic activity covered. and then leaching recovery. Leaching of the catalyst there are many ways Pd can be used aqua regia digestion method. including removal of crude acetylene. almost no loss of active components. mainly for the hydrogenation of ethylene. there are fire method (gas volatility). pressure acid leaching. 3. chloride (fluoride) volatilization. so that the catalytic activity greatly reduced the loss of catalytic activity. the waste incineration Pd-C catalyst for oxidation of carbon removal. so there is still recovery value. Pd recovery rate of up to one-way more than 97% purity of 99. Wuguan Min et al [3] from the failure of the recovery of Pd-C catalyst Pd way. fine residue obtained after refining with alkali metal acid sulphate react to produce soluble Pd salt . after filtering processing of the filtrate and the residue. commonly . respectively. adsorption and other recovery techniques.

the catalyst is dissolved oxidant and HCl. the reaction is: H2PdCl4 Na2S = PdS 2NaC1 2HC1. iron and other elements of content cannot be too high. iron cathode. electrolysis. Moreover. low cost. After roasting waste palladium catalyst. can be calcined at high temperatures into acid insoluble α-Al2O3. led to the recovery of palladium decreased. rapid response. The law and avoid the extensive use of aqua regia in a hurry the . sulfuric acid. Cathode in electrolytic deposition of palladium on the cathode materials used are mainly two: the carbon cathode. ion exchange law. because when adding sodium sulfide reacts with sulfur nitrate. NaOH NaCN. This process is suitable for processing materials with high content of palladium and aluminum materials. Zhang Zheng-Hong et al [4. iron and other ions in the ammonia complex will have a **** washing the hydroxide gel filtration and precipitation. a nitrate effect in time. ammonia complex purification palladium.used methods of extraction of palladium complex purification. without adding excess Na2S. through ion exchange. Pd sulfide precipitation has good selectivity. experimental results show that: Na2S small amount of precipitation that can achieve a high rate (almost 100%). the concentrated solution into an electrolytic cell in the electrolytic refining. and then electrolysis to extract palladium are more commonly used. without a single catch nitrate. easy to control conditions. reduced to elemental Pd and simple process. to increase the difficulty of separation. This method uses electrochemical principles. Good solvents NaCN. Pd precipitation with sodium sulfide and residual nitric acid will reduce the harm. When the Carrier by the γ-Al2O3. NH4C1 or NH4NO3 and HC1 oxidants (such as H2O2) and so on. and then impregnated with aqua regia acid solvent such as recycling. aqua regia. will be adsorbed palladium. Such technology has some limitations: aqua regia leaching solution is usually a large number of dissolved aluminum. aqua regia dissolution process.5] Treatment with aqua regia impregnation sodium sulfide.

replacement fluid discharge. PdCl2 trapping agent and the formation of complex salt. 99. KF and so on. the process is simple. At a certain temperature. This approach to a second leaching. but in the electrolytic cell to be complicated to operate. 3. Pd recovery rate of 99%. gasification agent concentration trapping agent to collect the reaction with palladium complexes [6]. the effect is better and high recovery rate. Control of acidity. and then were precipitated with **** palladium and palladium dichloride ammonia Purification Asian network.2 sublimation method under high temperature and pressure. NaC1. but the aqua regia corrosion. CaC12.3 Pretreatment of wet Fe Replacement: After crushing the spent catalyst with hydrochloric acid and sodium chlorate oxidation leaching.process of nitrate pollution of the environment. high temperature distillation of two-step method. gasification agent and chelating agent are basically highly toxic substances. NaF. Coarse palladium powder obtained for washing. SO2. 3. Low cost. NaC1 and so on. leaching with hydrochloric acid. equipment requirements and therefore high. commonly used chelating agent has NH4C1. take a . pollution of the environment. effective [7.95% purity palladium sponge. complex operation. Aqua regia leaching method is commonly used methods. also recovered acid and chlorine sub-carrier of aluminum powder Pd difficult to separate. This method is unique technology. filtering the full reaction of the secondary leaching residue. with the gasification agent treatment of waste catalyst.3%. In addition to chlorine as well outside the commonly used gasification agent CO.8]. Waste palladium catalyst Pd content is 0. German experts Allen's patented two-step method reported in the recovery of precious metals. it is not suitable for industrialization. the use of watersoluble capture agent after capturing PdCl2 recovery. the chlorine in the circular flow of waste by heating the palladium catalyst into the separation of volatile chlorides. Filtrate plus Fe replacement.

acid pretreatment. 4 multi-active components with palladium catalyst such catalysts generally contain the active component of other metals such as Pt. or electrochemical methods of purification. and then restore (or formaldehyde through hydrogen at 60 ). Active ingredient and carrier in accordance with their different use of appropriate methods. in the Walter stirring chlorine gas. will be reduced to palladium metal palladium. palladium was precipitated. the first of the deactivated catalyst pretreatment. 5 Conclusion palladium are precious metals. According to China's development status and outlook. the process is more complex. and then the different precious metals refining process for separation and purification. add 8mol / L hydrochloric acid. domestic reserves and production capacity has certain limits. a very high recovery value. by rough palladium [8]. and then through the metal reduction. because of the increase cannot be completely absorbed chlorine. In the recovery process. Ru. the need to be addressed. complex operation. automobile and environmental protection areas in the recovery of palladium catalysts for the production will have a huge economic benefit.4 hydrochloric acid method of waste washed palladium catalyst and sodium hydroxide solution mixing. chlorine gas from the exhaust emissions. so that the form of palladium was dissolved in H2PdCl4 down. Palladium catalyst is palladium waste valuable secondary resources. Add oxidant dissolved 3. the aluminum (Al mass fraction 99. Especially in the heavy oil resources that enhance and Pd tight prices in the future. usually using aqua regia. Ce and so on. Recoveries above 92%. Hydrochloric acid through chlorine method. polyester industry.long time filtering.5%) immersion. palladium 98% purity. filter washing. strengthening the recovery of spent catalyst and the results for industrial production as soon as possible is an . Ni. in the petrochemical industry. Re. the filtrate and the washing combined one. is an important chemical raw material.

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