SU52780A1 - Method for preparing rhenium catalyst for alcohol dehydrogenation - Google Patents
Method for preparing rhenium catalyst for alcohol dehydrogenationInfo
- Publication number
- SU52780A1 SU52780A1 SU52780A1 SU 52780 A1 SU52780 A1 SU 52780A1 SU 52780 A1 SU52780 A1 SU 52780A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- rhenium catalyst
- alcohol dehydrogenation
- rhenium
- hours
- preparing rhenium
- Prior art date
Links
- WUAPFZMCVAUBPE-UHFFFAOYSA-N Rhenium Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 title description 8
- 229910052702 rhenium Inorganic materials 0.000 title description 8
- 239000003054 catalyst Substances 0.000 title description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title description 4
- 238000006356 dehydrogenation reaction Methods 0.000 title description 3
- 150000001299 aldehydes Chemical class 0.000 description 7
- 150000002576 ketones Chemical class 0.000 description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 239000007795 chemical reaction product Substances 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- DVARTQFDIMZBAA-UHFFFAOYSA-O Ammonium nitrate Chemical compound [NH4+].[O-][N+]([O-])=O DVARTQFDIMZBAA-UHFFFAOYSA-O 0.000 description 2
- HOJYZCWLNWENHS-UHFFFAOYSA-O Ammonium perrhenate Chemical compound [NH4+].[O-][Re](=O)(=O)=O HOJYZCWLNWENHS-UHFFFAOYSA-O 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000003197 catalytic Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229910052803 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- -1 for example Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000003472 neutralizing Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910052904 quartz Inorganic materials 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Description
Каталитическа дегидрогенизаци спиртов, вз тых в парообразном состо нии , примен ема с целью получени альдегидов или кетонов, вл етс давно известной реакцией.The catalytic dehydrogenation of alcohols, taken in vapor form, used for the production of aldehydes or ketones, has been a long known reaction.
Наиболее часто примен емым катализатором вл етс металлическа медь, обладающа тем недостатком, что реакци протекает не количественно; в ее присутствии наблюдаетс заметное разложение продуктов реакции , т. е. альдегидов или кетонов. Другие металлы, например, никель, платина, кобальт, железо и др. в еще большей степени разлагают продукт реакции или же требуют нагревани до весьма высокой температуры, т.е. дают худшие результаты, чем медь.The most commonly used catalyst is metallic copper, which has the disadvantage that the reaction is not quantitative; in her presence, a noticeable decomposition of the reaction products, i.e., aldehydes or ketones, is observed. Other metals, for example, nickel, platinum, cobalt, iron, etc., further decompose the reaction product or require heating to a very high temperature, i.e. give worse results than copper.
Авторами установлено, что мелко раздробленный рений, способ приготовлени которого разработан авторами , каталитически разлагает пары спиртов, дава большие выходы альдегидов и кетонов, чем медь. При этом разложение продуктов реакции (т. е. альдегидов или кетонов) почти не имеет места. Таким образом, рениевые катализаторы, обслуживающие в р де случаев близкие к количественным выходы альдегидов или кетонов, значительно превосход т медные катализаторы .The authors found that finely crushed rhenium, the method of preparation of which was developed by the authors, catalytically decomposes alcohol vapors, giving greater yields of aldehydes and ketones than copper. In this case, the decomposition of the reaction products (i.e., aldehydes or ketones) almost does not take place. Thus, rhenium catalysts, serving in a number of cases close to quantitative yields of aldehydes or ketones, are significantly superior to copper catalysts.
Дисперсный рений готовитс следующим путем: металл раствор етс Dispersed rhenium is prepared as follows: the metal is dissolved
в минимальном количестве 10%-й азотной кислоты, полученный раствор выпариваетс досуха на вод ной бане и полученна смесь нитрата и перрената аммони восстанавливаетс электролитическим водородом в кварцевой трубке в течение 6-7 часов. Режим восстановлени : 1,5-2 часа при 150- 170°, 1 час при , 2 часа при 250-400° и 2 часа при 400°.in a minimum amount of 10% nitric acid, the resulting solution is evaporated to dryness in a water bath and the resulting mixture of ammonium nitrate and ammonium perrhenate is reduced by electrolytic hydrogen in a quartz tube within 6-7 hours. Recovery mode: 1.5-2 hours at 150-170 °, 1 hour at 2 hours at 250-400 ° and 2 hours at 400 °.
При сохранности указанных условий катализатор получаетс практически одного качества, т. е. вл етс своего рода стандартным катализатором.If these conditions are preserved, the catalyst is obtained of almost the same quality, i.e. it is a kind of standard catalyst.
Дегидрирование спиртов производитс путем пропускани их паров над дисперсным рением при 250- 500 в отсутствии воздуха.The dehydrogenation of alcohols is carried out by passing their vapors over dispersed rhenium at 250-500 in the absence of air.
Вариантом указанного способа получени альдегидов и кетонов может служить применение рени , нанесенного на пористые керамические носители путем, пропитывани их раствором перрената аммони , высушивани на вод ной бане и последующего восстановлени водородом по указанному выше способу.A variant of this method of producing aldehydes and ketones can be the use of rhenium deposited on porous ceramic carriers by impregnating them with ammonium perrhenate solution, drying in a water bath and subsequent reduction with hydrogen according to the above method.
Пары полученного альдегида (или кетона) конденсируютс в холодильнике и охлажденном приемнике вместе с парами непрореагировавшего спирта, от которого потом отдел ютс перегонкой . Остаток паров улавливаетс путем промывани через воду.The vapors of the resulting aldehyde (or ketone) are condensed in a refrigerator and cooled receiver along with vapors of unreacted alcohol, from which they are then separated by distillation. The residue vapor is trapped by rinsing through water.
Отход щий газ собираетс в аспираторе .The waste gas is collected in an aspirator.
Предмет изобретени .The subject matter of the invention.
Способ получени рениевого катализатора дл дегидрогенизации спирта путем растворени металлического рени в азотной кислоте, нейтрализации аммиаком, выпаривани раствораA method of producing a rhenium catalyst for dehydrogenating an alcohol by dissolving metallic rhenium in nitric acid, neutralizing with ammonia, evaporating the solution
и восстановлени полученной таким образом смеси перрената и нитрата аммони водородом при высокой температуре , отличающийс тем, что восстановление ведут сначала при температуре 150-170° в течение 1 - 2 часов, затем, в течение 1 часа при 170-250°, в течение 2 часов при 250 - 400° и наконец 2 часа при 400°.and reducing the mixture of perrhenate and ammonium nitrate thus obtained with hydrogen at a high temperature, characterized in that the reduction is carried out first at a temperature of 150-170 ° for 1 to 2 hours, then for 1 hour at 170-250 ° for 2 hours at 250 - 400 ° and finally 2 hours at 400 °.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4560803A (en) * | 1982-09-21 | 1985-12-24 | Exxon Research & Engineering Co. | Catalysts and process for oxidation of olefins to ketones |
| US4560805A (en) * | 1982-09-21 | 1985-12-24 | Exxon Research & Engineering Co. | Catalysts and process for the conversion of olefins to ketones |
| US4649223A (en) * | 1983-07-25 | 1987-03-10 | Exxon Research & Engineering Co. | Catalysts and process for the conversion of olefins to ketones |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4560803A (en) * | 1982-09-21 | 1985-12-24 | Exxon Research & Engineering Co. | Catalysts and process for oxidation of olefins to ketones |
| US4560805A (en) * | 1982-09-21 | 1985-12-24 | Exxon Research & Engineering Co. | Catalysts and process for the conversion of olefins to ketones |
| US4649223A (en) * | 1983-07-25 | 1987-03-10 | Exxon Research & Engineering Co. | Catalysts and process for the conversion of olefins to ketones |
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