Получение никеля Рэнея

[7myst]

Уважаемые! А не подскажите ли методу получения сего реагента. Заранее благодарен и с праздником!

[Pickuper]

Это мутно. И муфель нужен.

[gvozd]

Методика из органикума

[7myst]

Спасиба за методику, а нет ли поподрбней чегонить про получение самого сплава? Зарание спасиба

[gvozd]

Сам сплав, как верно заметили, без муфеля никак.

 

Process for producing the modified Raney nickel catalyst according to the present invention is essentially similar to conventional ones for producing Raney nickel catalyst Typically, predetermined amounts of nickel, aluminum, and iron are mixed first and, if necessary, at least one metal selected from the group consisting of chromium, molybdenum, tungsten, cobalt, manganese, and titanium may be added thereto. The mixture is then melted at a temperature of 1200° to 2000° C. to produce a precursor alloy. After being sat still and cooled, the precursor alloy is crushed into powder or granule with suitable size and then developed in a solution of alkali metal hydroxide. Finally, the thus-obtained product is washed with distilled or ion-exchanged water to obtain the modified Raney nickel catalyst.

[gvozd]

Есть вариант сделать катализатор Урушибары (тот же скелетный никель, только в более мягких условиях).

 

To a 100 ml rb flask, fitted with a mechanical stirrer and containing 10 g of zinc dust and 3 ml water there was added 3 g of NiCl2x6H2O (of a "chemically pure" grade, IMHO, it is not necessary, purity of zinc is more important), dissolved in 10 ml of water, and the stirring begun. A vigorous reaction took place and the contents of the flask almost ran over; after 15 minutes stirring was stopped and the reaction mass was diluted with tap water and transferred into a 500 ml rb flask, where it was washed several times with tap water and the last time - with distilled water. The precipitated nickel was a dark-gray solid that did not differed much in color from the original zinc dust, when wet. It was digested with 160 ml of 13% acetic acid for 5 min. Zinc dissolution in acetic acid was exothermic and was accompanied by a violent evolution of a hydrogen gas, at the end black catalyst raised to the surface of the solution. All was then filtered with suction on a Schott filter, washed with 200 ml of distilled water and with small amount of IPA. The filtrate had a greenish color.

 

Ten ml of solution prepared from 2 g of crystalline nickel chloride is warmed to 80-90°C and added, over a period of 1-2 minutes with stirring, to 5 g of zinc dust, which has been mixed with a small amount of water and placed in a water bath of the same temperature. Immediately afterward, the precipitate is filtered off with a sintered glass filter and washed with a small amount of hot distilled water. It is then plunged into 100 ml of 10% sodium hydroxide solution as quickly as possible and left standing for 15-25 minutes on a water bath at 50-60°C with occasional stirring. The supernatant liquid is decanted, and the remainder is washed with two 40 ml portions of distilled water at 50-60°C. Then the wash-water is replaced by ethanol. The catalyst, containing 0.45 g of nickel adhering to 2 g of zinc, is thus obtained. The last step, in which ethanol replaces the wash-water, can be omitted when reduction is to be carried out in an aqueous solution.

 

Сама ссылка: http://www.erowid.org/archive/rhodium/chem...urushibara.html

[Pickuper]

Вряд ли это равнозначная замена.

[gvozd]

Не знаю, насколько равнозначна-сам пользовался только продажным никелем Ренея. Но у человека есть возможность это проверить (As far as the author is aware, all reductions which Raney catalysts promote are effected as well in the presence of an Urushibara catalyst, and the activities of the Urushibara catalysts are, under both ordinary and high pressures, by no means lower than displayed by Raney catalysts.).

 

to 7myst: если решишь делать Урушибару-отпишись, пожалуйста, с результатами, интересно насколько он хорош.

[7myst]

Огрмное спасибище за метдики :aj: :0457aj:

Просто собрался обессеривать такое соединение (та гидразиндиуксусная кислота кончилась почти, и о результатах с ней я тоже обещал отписаться , скоро отпишусь):

 

О результе скоро скажу, ещё раз спасиба за методики!