SU732209A2

SU732209A2 - Method of purifying niobium and tantalum hydroxides from fluorine

Info

Publication number: SU732209A2
Application number: SU772547930A
Authority: SU
Inventors: Геннадий Никифорович Дубошин; Владимир Гаврилович Майоров; Артур Григорьевич Бабкин; Леонид Иринеевич Склокин
Original assignee: Институт химии и технологии редких элементов и минерального сырья Кольского филиала АН СССР
Priority date: 1977-12-01
Filing date: 1977-12-01
Publication date: 1980-05-05

Description

II

Изобретение относитс к способ очистки гидроокисей ниоби и тантала от фтора и может быть использовано в технологии получени чистых соединений ниоби и тантала.The invention relates to a method for the purification of niobium and tantalum hydroxides from fluorine and can be used in the technology of obtaining pure compounds of niobium and tantalum.

По основному авт. св. № 552296 известен способ очистки гидроокисей ниоби и тантала 6т фтора путем промывки их раствора соли алюмини .According to the main author. St. No. 552296 is a known method for the purification of niobium hydroxides and tantalum with 6t of fluorine by washing their solution of an aluminum salt.

Степень очистки от фтора составл ет 97-98%. Содержание алюмини в конечном продукте повышаетс до 0,1-0,4 мас.%.The degree of purification from fluorine is 97-98%. The aluminum content in the final product is increased to 0.1-0.4 wt.%.

Недостаток способа состоит в относительно большом загр знении конечного продукта алюминием.The disadvantage of this method is the relatively large contamination of the final product with aluminum.

Цель изобретени заключаетс в снижении содержани алюмини в конечном продукте,The purpose of the invention is to reduce the aluminum content in the final product.

Дл этого промывку ведут в присутствии кислоты при рН 0,1-1,2.For this, washing is carried out in the presence of acid at a pH of 0.1-1.2.

Пример 1. КЮОг гидроокиси ниоби , содержащей 35% п тиокиси ниоби и 8,3% фтора, добавл ют 1 лExample 1. Niobium CUOg hydroxide containing 35% niobium pentoxide and 8.3% fluorine is added 1 l

раствора, содержащего 48,5 г/л АЬСв, (25О% от теоретически необходимого расхода дл св зывани фтора в AUF ) и 5 г/л нес (рН f)acTBopa 0,8). Пульпу перемешивают в течение 1 час при температуре 5Q+5 С. Отфильтрованный осадок снова обрабатывают аналогичным раствором при тех же услови х.a solution containing 48.5 g / l ABCB, (25O% of the theoretically required flow rate for binding fluorine in AUF) and 5 g / l carrying (pH f) acTBopa 0.8. The pulp is stirred for 1 hour at a temperature of 5Q + 5 ° C. The filtered precipitate is again treated with the same solution under the same conditions.

После фильтрации осадок гидроокиси дл отделени от маточника дважды про10 мывают раствором 5 г/л НС6 .при Т:Ж-1:10 и перемешивают в течение 1 час при комнатной температуре. Содержание фтора в промытой гидроокисиAfter filtration, the hydroxide precipitate is washed twice with a solution of 5 g / l HC6. For T: W-1: 10 and separated for 1 hour at room temperature for separation from the mother liquor. The fluorine content in the washed hydroxide

JJ 0,25%, что соответствует сгепени очистки от фтора 97,0%. Содержание алюмини 0,002% (здесь и далее по отноше- ншо к п тиокиси металла).JJ 0.25%, which corresponds to a fluorine clearance of 97.0%. The aluminum content is 0.002% (hereinafter, relative to the metal thioxide).

Пример 2. Промывку гидрооки-Example 2. Washing hydrokoy-

Claims

2 sinobium is carried out with a solution containing 54 g / l AB (from the theoretical consumption for binding fluorine in AUFg) and 5 g / l HY (pH of the solution is 1.2) with the same conditions as in Example 1. For separation from the mother liquor using a solution of 5 g / l HNO. After washing, the fluorine content in the hydroxide is 0.28%, which corresponds to a purification degree of 96.6%. The aluminum content is 0.003%, Example 3. The washing of niobium hydroxide is carried out with a solution containing 87 g / l ABg (SO) g (35O% cx theoretical consumption for binding fluorine in AUFj) and 50 g / l N (solution pH 0, 1) under the same conditions as in Example 1. A solution of 5O g / l HgS O is used for separation from the mother liquor. After washing, the fluorine and hydroxide content is 0.135%, which corresponds to a purity level of 98.2%. The aluminum content is 0.01%. Example 4. Niobium hydroxide was washed with 48.5 g / l ARCRg (250% of theoretical consumption for binding fluorine in ABF) and 10 g / l HgS O under the same conditions as in Example 1. For separation from the mother liquor using a solution of 10 g / l N S O (pH of a solution of 0.9). After washing, the fluorine content in the hydroxide is 0.16%, which corresponds to a purification degree of 98.1%. The aluminum content is 4 0.002%. Example 5. To 1OO g of tantalum hydroxide containing 38.3% tantalum pentoxide and 4.4% fluorine, add 1 solution containing 49.4 g / l AnW oz) s (300% of the theoretical consumption for fluorine binding in APP) and 5 g / l HzBO (pH of the solution is 0.9) and stirred for 1 hour at a temperature. The filtered precipitate is subjected to the same treatment a second time. The precipitate after the second filtration is washed twice with a solution containing 5 g / l HgSQ, with stirring for 1 hour. After washing, the fluorine content in the hydroxide is 0.1%, which corresponds to a purification degree of 97.7%. The aluminum content is 0.002%. Thus, the proposed method allows reducing the aluminum content in the final product while maintaining the degree of purification from fluorine in the same range as in the known method. Claims of the method of purification of niobium and tantalum hydroxides from fluorine according to the author. St. No. 552296, characterized in that, in order to reduce the aluminum content in the final product, the washing is carried out in the presence of an acid at a pH of 0.1-1.2.