SU16658A1 - Method of producing titanium tetrachloride - Google Patents
Method of producing titanium tetrachlorideInfo
- Publication number
- SU16658A1 SU16658A1 SU21459A SU21459A SU16658A1 SU 16658 A1 SU16658 A1 SU 16658A1 SU 21459 A SU21459 A SU 21459A SU 21459 A SU21459 A SU 21459A SU 16658 A1 SU16658 A1 SU 16658A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- titanium
- titanium tetrachloride
- iron
- producing titanium
- solution
- Prior art date
Links
- 238000000034 method Methods 0.000 title description 13
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 title description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 229910052742 iron Inorganic materials 0.000 description 5
- IYVLHQRADFNKAU-UHFFFAOYSA-N oxygen(2-);titanium(4+);hydrate Chemical compound O.[O-2].[O-2].[Ti+4] IYVLHQRADFNKAU-UHFFFAOYSA-N 0.000 description 5
- 239000002244 precipitate Substances 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical group O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 description 3
- 235000011121 sodium hydroxide Nutrition 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 239000006286 aqueous extract Substances 0.000 description 2
- 238000004061 bleaching Methods 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 159000000014 iron salts Chemical class 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 229910001018 Cast iron Inorganic materials 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical class [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- BEFDCLMNVWHSGT-UHFFFAOYSA-N ethenylcyclopentane Chemical compound C=CC1CCCC1 BEFDCLMNVWHSGT-UHFFFAOYSA-N 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-O hydridodioxygen(1+) Chemical compound [OH+]=O MYMOFIZGZYHOMD-UHFFFAOYSA-O 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 229910000398 iron phosphate Inorganic materials 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- FWFGVMYFCODZRD-UHFFFAOYSA-N oxidanium;hydrogen sulfate Chemical compound O.OS(O)(=O)=O FWFGVMYFCODZRD-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229940075582 sorbic acid Drugs 0.000 description 1
- 235000010199 sorbic acid Nutrition 0.000 description 1
- 239000004334 sorbic acid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Inorganic materials O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- JUWGUJSXVOBPHP-UHFFFAOYSA-B titanium(4+);tetraphosphate Chemical compound [Ti+4].[Ti+4].[Ti+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O JUWGUJSXVOBPHP-UHFFFAOYSA-B 0.000 description 1
- AKMXMQQXGXKHAN-UHFFFAOYSA-N titanium;hydrate Chemical compound O.[Ti] AKMXMQQXGXKHAN-UHFFFAOYSA-N 0.000 description 1
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Description
Существующие сдособы производства треххпористогр титана, имеющего широкое промышленное применение при различных восстановительных процессах (при отбепке тканей, при восстановлении и обесцвечивании органических красителей , содей золота, платины н т. д.) основаны, г.тавннм образом, на восстановлении чистого четыреххлористого титана электролизом или каким-либо другим подход щим методом. Четыреххлористый титан, в свою очередь, получаетс нагреванием карбида титана и.тги смеси двуокиси титана с углеродом в струе хлора, равно как и растворением в сол ной кислоте гидрата окиси титана, вл ющегос продуктом разложени ильменита (титанистой руды) при прокаливании его с углем и серной кислотой . Указанные методы получени четыреххлористого титана из карбида, двуокиси или гидрата титана имеют р д .недостатков. В частности, при существуйщеы гидратном способе процесс осложн етс необходимостью сложных приемов дл удалени солей железа, обычно сопровождающих гидрат окиси титана.Existing methods for the production of titanium trichporistogr, which has wide industrial application in various restoration processes (in fabric bleaching, in the reduction and bleaching of organic dyes, gold, platinum, etc.) are based, in a similar way, on the reduction of pure titanium tetrachloride by electrolysis any other suitable method. Titanium tetrachloride, in turn, is obtained by heating titanium carbide and the mixture of titanium dioxide and carbon in a stream of chlorine, as well as by dissolving titanium oxide hydrate in hydrochloric acid, which is a product of decomposition of ilmenite (titanium ore) during calcination with carbon and sulfuric acid. These methods for producing titanium tetrachloride from carbide, dioxide or titanium hydrate have a number of disadvantages. In particular, when the hydrate process exists, the process is complicated by the need for complex techniques to remove iron salts, usually accompanying titanium oxide hydrate.
В предлагаемом способе, дл устранени этих недостатков, водную выт жку, получаемую из сплава ильменита с углем и сульфатами, восстанавливают обычнымIn the proposed method, in order to eliminate these drawbacks, the aqueous extract obtained from an ilmenite alloy with coal and sulphates is reduced by the usual
способом при помощи железного лома, к ней прибавл ют фосфорной кислоты, затем, промытый осадок, дл получени гидрата окиси титана, обрабатывают раствором едкого натра до щелочной реакции .by means of iron scrap, phosphoric acid is added to it, then the washed precipitate, to obtain titanium oxide hydrate, is treated with caustic soda solution until alkaline.
Способ состоит в том, что измельченна руда (ильменит), содержаща до 50% двуокиси титана, смешивают с 50 г древесноугольного порошка и 2 кг серной кислоты уд. в. 1,84 и нагревают в-чугунном котле емкостью в 5 литров. Нагревание ведут сначала при температуре около 100° С до прекращени всаучивани массы, а затем, температуру нагревани постепенно повыпгают до обильного выделени паров серного ангидрида и сильного загустевани массы. Охлажденную массу выщелачивают холодной водой в несколько приемов до извлечет ни всех,растворимых веществ. Раствору дают отсто тьс и при помощи сифона сливают прозрачную жидкость. В растворе наход тс сернокислые соли титана и железа.The method consists in the fact that crushed ore (ilmenite) containing up to 50% of titanium dioxide is mixed with 50 g of charcoal powder and 2 kg of sulfuric acid beats. at. 1.84 and heated in a 5-liter cast iron boiler. The heating is first carried out at a temperature of about 100 ° C until the mass has been tempered, and then, the heating temperature is gradually raised to a copious liberation of sulfuric anhydride vapor and a strong thickening of the mass. The cooled mass is leached with cold water in several steps until it extracts all soluble substances. The solution is allowed to stand and a clear liquid is drained by means of a siphon. Sulfuric salts of titanium and iron are in solution.
Хот фосфорнокислое железо, (окисное) не осаждаетс из кислых растворов, но во избежание загр знени выпавшего фосфорнокислого титана . продуктами гидролиза железных солей, окисные соли железа перевод т обычным способомAlthough iron phosphate (oxide) is not precipitated from acidic solutions, it is to avoid contamination of the precipitated titanium phosphate. iron salts hydrolysis products, iron oxide salts are converted in the usual way
iE закисные, дл чего к раствору п|)иба±л ют избыток железного дома и ведут восстановление до тех пор, пока раствор не окраситс в слабый фиолетовый цвет. Затем, раствор нагревают до 60° С fa прибавл ют |ф6сфорной кислоты уд. в. 1,7 из расчета 250 г 1 слоты на один килрграмм руды. Раствор нагревают до кипени , выдавший осадок отфильтровывают на большой воронке Бюхнера и проыывают подкисленной серной кислотой водой до удалени железа и, затем, несколько раз чистой водой до удаленна серной кислоты; Далее, осадок неренос т, в объемистую фарфоровую чашку и обрабатывают ЗОо/о-ным раствором едкого натра до щелочной реакции. Выпавший гидрат окисного титана промываЪт холодной водой -и отфильтровывают, продолжа промывание до прекращени реакции на фосфор. Фильтрование лучше производить при уменьшенном давлении дл возможного обезвоживани . Осадок высушиваетс на пористых глин ных тарелка;х И раствор етс в сол нрй кислоте . в. 1,19 дл получени растворов четыреххлористогр титана чтакой концентраций , котора соответствовала бы концентрации техническово треххлористого титана, т.-е. до Т : С1з. Нет необxOflHMOCT 0t в получении более концентрйрованных растворов, так как, треххлорйстый титан плохо растворим в концентрированной сол ной кислоте и цри бблыпей концентрации выпадает во врем электролиза ,в виде: кристаллов Т: СЬ. 5HQI, неудобных дл работы и хранени . В дальнейшем полученный четыреххлористый титанобычным электролитическим методом перевод т в треххлористый титан.iE is soured, for which an excess of the iron house is brought to the solution | ib ± ± and a reduction is carried out until the solution turns a weak violet color. Then, the solution is heated to 60 ° C; fa is added with a fd of a sorbic acid beats. at. 1.7 at the rate of 250 g 1 slot per kilr of ore. The solution is heated to a boil, the precipitated precipitate is filtered on a large Buchner funnel and rinsed with acidified sulfuric acid water to remove iron and then several times with pure water to remove the sulfuric acid; Next, the precipitate is not transferred to a voluminous porcelain dish and treated with 30–30% caustic soda to an alkaline reaction. The precipitated titanium oxide hydrate is washed with cold water — and is filtered off, continuing to be washed until the reaction to phosphorus has ceased. Filtration is best done at reduced pressure for possible dehydration. The precipitate is dried on a porous clay plate; x and dissolves in hydrochloric acid. at. 1.19 to obtain solutions of titanium tetrachloride with a concentration that would correspond to the concentration of technical titanium trichloride, i.e. T: S1z. It is not necessary to obtain more concentrated solutions, since trichloride titanium is poorly soluble in concentrated hydrochloric acid and occurs at the time of electrolysis, in the form of: T: Ch crystals. 5HQI, inconvenient for handling and storage. Subsequently, the titanium tetrachloride obtained by the electrolytic method is converted to titanium trichloride.
Предмет патента.The subject of the patent.
Способ получени четыреххлористого титана растворением в сол ной кислоте гидрата окиси , полученного разложением HfebTvfенита прокаливанием с углем и серной кислотой, отличающийс тем, что полученную из сплава водную выт йску , в цел х перевода окисных солей железа в закисные, восстанав.чивают обычным способом при помощи железного лома до по влени слабой фиолетовой окраски, после чего прибэ влают при нагревании фосфорную кислоту, а полученной осадок, после промывки подкисленной, а затем чистой водой, дл получени гидрата окиси титана, обрабатывают раствором едкого натра до ще.т1Очной реакции. jA method of producing titanium tetrachloride by dissolving an hydroxide of an oxide obtained by decomposing HfebTvfenite by calcining with coal and sulfuric acid in hydrochloric acid, characterized in that the aqueous extract obtained from the alloy is reduced to ferrous oxide salts in ferrous acid by the usual method. iron scrap until a violet color is observed, after which the phosphoric acid is heated when heated, and the resulting precipitate, after washing with acidified and then pure water, to obtain titanium oxide hydrate, They are treated with caustic soda solution to the ground. j
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU21459A SU16658A1 (en) | 1927-12-05 | 1927-12-05 | Method of producing titanium tetrachloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU21459A SU16658A1 (en) | 1927-12-05 | 1927-12-05 | Method of producing titanium tetrachloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU16658A1 true SU16658A1 (en) | 1930-09-30 |
Family
ID=48336989
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU21459A SU16658A1 (en) | 1927-12-05 | 1927-12-05 | Method of producing titanium tetrachloride |
Country Status (1)
| Country | Link |
|---|---|
| SU (1) | SU16658A1 (en) |
-
1927
- 1927-12-05 SU SU21459A patent/SU16658A1/en active
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