KR810001553B1 - Process for recovering and regeneration of rodium catalyst - Google Patents
Process for recovering and regeneration of rodium catalyst Download PDFInfo
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- KR810001553B1 KR810001553B1 KR1019800000354A KR800000354A KR810001553B1 KR 810001553 B1 KR810001553 B1 KR 810001553B1 KR 1019800000354 A KR1019800000354 A KR 1019800000354A KR 800000354 A KR800000354 A KR 800000354A KR 810001553 B1 KR810001553 B1 KR 810001553B1
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- recovering
- regeneration
- rhodium
- catalyst
- rodium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/90—Regeneration or reactivation
Abstract
Description
본 발명은 로듐 화합물을 촉매로 사용하는 반응에서 최종생 성물을 분리하고 남은 이액으로 부터 로듐을 회수하여 다시 반응에 사용할 수 있게 하는 방법이다.The present invention is a method of separating the final product in the reaction using a rhodium compound as a catalyst and recovering the rhodium from the remaining two liquids to be used for the reaction again.
여러가지 반응에 광범위하게 사용되는 로듐 화합물 촉매는 백금족 금속화합물중의 하나이다. 이런 백금족 금속화합물은 한정된 자원이란 점과 고가의 귀금속류란 점으로 해서 화학공업에서는 사용된 촉매의 회수 및 재생이 필수적인 공정으로 되고 있다. 일반적으로 촉매를 쇠후하여 재생할 때는 아래와 같은 점을 고려하여야 한다.Rhodium compound catalysts which are widely used in various reactions are one of the platinum group metal compounds. These platinum group metal compounds are limited resources and expensive precious metals, making the recovery and regeneration of catalysts used in the chemical industry essential. In general, the following considerations should be taken into account when the catalyst is degenerated.
첫째, 일정한 형태가 아니면 촉매로서의 구실을 하지 못하는 경우와First, if it does not serve as a catalyst,
둘째, 어떤 특정한 형태로 주어질 필요없이, 여러가지 다양한 형태의 화합물로 반응기에 넣어도 반응중에 활성화된 형태로 바뀌어서 반응에 참여하는 경우로 크게 나누어 볼 수가 있다.Second, there is no need to be given in any particular form, it can be divided into the case of participating in the reaction by changing to the activated form during the reaction of the various types of compounds in the reactor.
그러나 둘째 경우에도 가속 사용할 경우 생기는 촉매 회손으로 궁극적으로는 첫번째 경우와 같이 특정한 형태로 재생 해야한다.However, even in the second case, the catalyst loss caused by the accelerated use ultimately needs to be recycled in a specific form as in the first case.
그리고 지금까지 알려진 로듐화합물의 회수 및 재생방법은 반응의 반응물질 각 반응조건 및 최종생성물이 각각 다르기 때문에 일률적으로 한가지 방법만을 사용해서 로듐화합물을 회수, 재생할 수가 없이 각 반응마다 그 공정에 알맞는 방법을 선택해서 사용하는 단점이 있었다.Since the recovery and regeneration methods of rhodium compounds known to date are different from each reaction condition and the final product of the reactants of the reaction, a method suitable for each reaction can not be recovered and regenerated using only one method. There was a drawback to using it.
본 발명의 특징은 이런 단점을 극복하여 대부분의 화학반응에 사용된 로듐화합물을 일정형태로 회수, 재생에 적용이 가능하고 회수율 또한 높다는 것이다. 좀더 구체적으로 방법을 언급하면 아래와 같다. 최종 생성물을 분리하고 남은 이액을 증발기와 진공펌프를 사용해서 용매를 제거한 다음 알칼리 금속 수산화물 예컨대 수산화나트륨, 수산화칼륨이든지 수산화암모늄등으로 pH를 맞추어 가며 환류시킨 다음, 실온에서 하루동안 방치하면 로듐화합물이 포함된 침전물이 가라앉는다. 이것을 여과한뒤 케이크를 진공오븐에서 하루동안 건조 시킨 후, 분해 플라스크에 넣고 적당량의 무기산으로 유기물을 분해시킨다. 여기서 무기산이라 함은 황산, 질산을 말하는데 각각 단독으로 사용할 수 있으나 2가지 산을 혼합하여 사용할 수도 있다. 유기물이 완전분해된 혼탁액을 석영도가니에 옮긴뒤 알칼리금속 수산화물이나 수산화 암모늄을 가한다. 더이상 이것이 반응을 하지 않을 때까지 넣고 가스버니로 가열한다. 도가니속의 용액이 투명한 노란색이 될때까지 가열한 다음 실온으로 식히고 이것을, 증류수로 녹여서 비이커에 옮긴 다음 다시 알칼리 금속의 수산화물이나 수산화 암모늄을 넣는다. 이것을 넣으면 주황색 침전이 생겨나기 시작한다. 더이상 주황색 침전이 생기지 않을 때까지 다시 알칼리 금속의 수산화물이나 수산화 암모늄을 넣은뒤 하루동안 방치한 다음 여과한다. 여과된 침전물에 염산을 가하여 완전히 녹인다음 물중탕으로 염산 냄새가 나지 않을 때까지 건조시키면 염화로듐의 수화물(RhC13H2O)을 얻는다.It is a feature of the present invention to overcome this disadvantage that the rhodium compounds used in most chemical reactions can be applied to recovery and regeneration in a certain form, and the recovery rate is also high. More specifically, the method is as follows. After separating the final product and removing the solvent by using an evaporator and a vacuum pump to remove the solvent, and refluxed to adjust the pH to alkali metal hydroxides such as sodium hydroxide, potassium hydroxide or ammonium hydroxide, and left at room temperature for one day to rhodium compound The sediment contained subsides. After filtering this, the cake was dried in a vacuum oven for one day, and then placed in a decomposition flask to decompose organic matter with an appropriate amount of inorganic acid. In this case, the inorganic acid refers to sulfuric acid and nitric acid, but each may be used alone, or two acids may be mixed and used. The organically decomposed turbidity is transferred to a quartz crucible and alkali metal hydroxide or ammonium hydroxide is added. Insert until it no longer reacts and heat with gas bunnies. The solution in the crucible is heated to a clear yellow color, cooled to room temperature, dissolved in distilled water, transferred to a beaker, and then added with alkali metal hydroxide or ammonium hydroxide. When you add it, an orange precipitate begins to form. Add alkali metal hydroxide or ammonium hydroxide until no orange precipitates anymore, leave for one day, and filter. Hydrochloric acid is added to the filtered precipitate to completely dissolve it and then dried in a water bath until no smell of hydrochloric acid is obtained to obtain a hydrate of rhodium chloride (RhC1 3 H 2 O).
다음의 실시에는 본 발명을 더욱 상세히 예증하여 줄 것이나 이에 국한된다는 것은 아니다.The following examples will illustrate, but are not limited to, the present invention in more detail.
[실시예]EXAMPLE
로듐화합물이 촉매로 사용된 반응에서 최종 생성물을 분리하고 남은 이액 100g(로듐은 염화로듐의 수화물로 환산할 경우 40㎎(0.151m mole)이 들이 있다.)을 증발기로 용매를 증발시킨 뒤 수산화 나트륨 용액으로 pH를 6.5로 맞추고, 환류시킨 다음 실온에서 하루동안 방치하여 여과한다. 여과한 케이크에 황산 20을 넣고 가열하면서 질산을 넣어 유기물을 완전 분해시킨다. 이용액을 석영도가니에 옮긴다음 수산화나트륨을 넣은 뒤로 가열하고 식힌다. 이것을 증류수로 녹인다음 수산화 나트륨을 넣고 침전물을 여과한뒤 염산을 가해 침전물을 녹인다. 이용액을 물중탕으로 염산을 날려보낸뒤 39㎎(0.148m mole)의 염화로듐 3수화물을 얻었다. 이때 얻어진 염화로듐 3수화물(RhC13. 3H2O)의 회수율은 97.5%이었다.In the reaction where the rhodium compound was used as a catalyst, 100 g of the remaining liquid (the rhodium contained 40 mg (0.151 m mole) in the case of hydrate of rhodium chloride) after evaporation of the solvent by an evaporator was dissolved in sodium hydroxide. The solution is adjusted to pH 6.5, refluxed and left to filter at room temperature for one day. 20 sulfuric acid was added to the filtered cake and nitric acid was added while heating to completely decompose the organic matter. Transfer the solution to a quartz crucible, add sodium hydroxide, heat and cool. Dissolve this in distilled water, add sodium hydroxide, filter the precipitate, and add hydrochloric acid to dissolve the precipitate. Hydrochloric acid was blown into the water bath and 39 mg (0.148 m mole) of rhodium chloride trihydrate was obtained. The resulting recovery of rhodium chloride trihydrate (RhC1 3. 3H 2 O) was 97.5%.
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KR1019800000354A KR810001553B1 (en) | 1980-01-31 | 1980-01-31 | Process for recovering and regeneration of rodium catalyst |
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KR1019800000354A KR810001553B1 (en) | 1980-01-31 | 1980-01-31 | Process for recovering and regeneration of rodium catalyst |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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KR100729402B1 (en) * | 2006-09-29 | 2007-06-15 | 차상용 | A composition for ionizing rhodium, and a method of ionizing or plating rhodium by using the same |
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- 1980-01-31 KR KR1019800000354A patent/KR810001553B1/en active
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR100729402B1 (en) * | 2006-09-29 | 2007-06-15 | 차상용 | A composition for ionizing rhodium, and a method of ionizing or plating rhodium by using the same |
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