Method for synthesizing di(ethylene) chlorine rhodium (I) dimer

A dimer, hydrated rhodium trichloride technology, applied in chemical instruments and methods, compounds containing elements of group 8/9/10/18 of the periodic table, organic chemistry, etc., can solve the problem of reducing product yield and purity , Restricting large-scale production, low reaction efficiency and other problems, to achieve the effect of improving synthesis yield, improving yield and simplifying the operation process

Active Publication Date: 2014-07-02
浙江微通催化新材料有限公司
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  • Application Information

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Problems solved by technology

People mostly synthesize di(ethylene)chlororhodium(I) dimer by this method; but in the actual scale-up production, because the method is divided into two reactions, the operation is more complicated, and ethylene is introduced by bubbling, and the reaction efficiency is low , the reaction time is long, so that part of rhodium chloride is reduced to simple rhodium, which greatly reduces the product yield and purity, and limits large-scale production

Method used

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  • Method for synthesizing di(ethylene) chlorine rhodium (I) dimer
  • Method for synthesizing di(ethylene) chlorine rhodium (I) dimer
  • Method for synthesizing di(ethylene) chlorine rhodium (I) dimer

Examples

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Effect test

Embodiment 1

[0023] Add 20g (76mmol) rhodium trichloride hydrate into 30mL water, stir and dissolve at 50°C, after the rhodium trichloride is completely dissolved, add it to a 1L autoclave, then add 350mL of 95% ethanol, and set the autoclave at 1MPa Pressure nitrogen was replaced three times to remove the air, and the nitrogen was pressurized to 1MPa for the third time and kept for 30 minutes to check the tightness of the autoclave. After confirming the seal, replace the nitrogen with 1MPa ethylene three times, and finally adjust the ethylene pressure in the autoclave to 1MPa, start the stirring reaction, control the temperature at 30°C, and continue to feed ethylene gas when the pressure starts to decrease to keep the pressure at the set value. After continuing the reaction for 1 hour, release ethylene to bring the pressure in the autoclave to atmospheric pressure, inject 30.5 g of 20% sodium hydroxide solution with nitrogen, and continue to feed ethylene gas after sealing, keep the press...

Embodiment 2

[0025] Control reaction temperature 50 ℃, other reactant charging amount and experimental condition are the same as embodiment 1, finally obtain di(ethylene)chlororhodium (I) dimer 11.9g, yield 80.5%, have a small amount of elemental rhodium because reaction temperature is too high generate.

Embodiment 3

[0027] Maintain 2MPa ethylene pressure reaction. The feeding amount of other reactants and the experimental conditions are the same as in Example 1, and finally 12.9 g of di(ethylene)chlororhodium (I) dimer is obtained, with a yield of 87.3%.

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Abstract

The invention discloses a method for synthesizing di(ethylene) chlorine rhodium (I) dimer. The method comprises the following steps: firstly, adding a certain amount of water which is as much as 1-10 times of the mass of rhodium trichloride hydrate into rhodium trichloride hydrate in a high-pressure reaction kettle, wherein the dissolving temperature is 50-80 DEG C; after rhodium trichloride hydrate is completely dissolved, adding C1-C3 alcohol used as a solvent which is as much as 10-50 times of the mass of rhodium trichloride hydrate, inside the high-pressure reaction kettle, heating and stirring to react taking ethylene of one barometric pressure instead of high pressure ethylene as a reactant, pressurizing to react for 0.5-2 hours, pressing a degassed alkali solution, continuously reacting for 0.5-1 hours, after the reaction is accomplished, releasing the ethylene inside the high pressure kettle, replacing the ethylene by using nitrogen, filtering and washing a reaction mixture in water and alcohol in the presence of nitrogen, and drying in vacuum at the room temperature so as to obtain the nacarat di(ethylene) chlorine rhodium (I) dimmer. The method has the characteristics that the synthesis yield can be increased, the cost is lowered, the reaction time is shortened, the operation process is simplified and the like.

Description

technical field [0001] The invention relates to a method for synthesizing di(ethylene)chlororhodium (I) dimer, belonging to the technical field of rhodium catalyst preparation. Background technique [0002] Catalytic reactions involving precious metals are of great significance to chemical engineering. As an important catalytic material, rhodium has been widely used in petrochemical, pharmaceutical, fine chemical, and environmental protection fields. It shows excellent activity in acylation, olefin isomerization and carbonylation reactions. Organometallic rhodium complexes are widely used in homogeneous catalysis. Di(ethylene)chlororhodium(I) dimer, as an important organometallic rhodium complex, is widely used in the synthesis of other rhodium catalysts, or directly used in catalysis reaction. The synthesis of bis (ethylene) rhodium chloride (I) dimer was first reported by Cramer and Richard in Inorganic Chemistry, 1,722-3, they used RhCl 3 ·(H 2 O)X was dissolved in me...

Claims

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Application Information

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IPC IPC(8): C07F15/00
Inventor 潘剑明刘斌沈炯陈波马银标谢智平阮晓东王惟
Owner 浙江微通催化新材料有限公司
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