SU1680632A1 - Method for obtaining lead oxobromide - Google Patents
Method for obtaining lead oxobromide Download PDFInfo
- Publication number
- SU1680632A1 SU1680632A1 SU4605491L SU4605491L SU1680632A1 SU 1680632 A1 SU1680632 A1 SU 1680632A1 SU 4605491 L SU4605491 L SU 4605491L SU 4605491 L SU4605491 L SU 4605491L SU 1680632 A1 SU1680632 A1 SU 1680632A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- lead
- oxonitrate
- lead oxide
- oxobromide
- ammonium nitrate
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims abstract description 15
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 12
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910000464 lead oxide Inorganic materials 0.000 claims abstract description 8
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 claims abstract description 8
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims abstract description 5
- 230000003993 interaction Effects 0.000 claims description 2
- 239000011541 reaction mixture Substances 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims 1
- 238000002955 isolation Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 238000004904 shortening Methods 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000000047 product Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Из обретение относится к способам полученияоксонитрата свинца и позволяет сократитьпродолжительность процесса и упростить его В соответствии с изобретениемоксонитрат свинца получают путем обработкиоксида свинца раствором нитрата аммония при молярном соотношении 1:1,5- 3 в среде диметилформамида или диметил- сульфоксида при 50°С и постоянном перемешивании с последующим отделениемосадка и сушкой em. Выход продукта 90%, продолжительность процесса составляет15 мин. 1 табл.The acquisition relates to methods for producing lead oxonitrate and allows shortening the process and simplifying it. According to the invention, lead oxonitrate is obtained by treating lead oxide with a solution of ammonium nitrate at a molar ratio of 1: 1.5-3 in dimethylformamide or dimethyl sulfoxide at 50 ° C and stirring followed by separation by drying and em. The product yield is 90%, the process duration is 15 minutes. 1 tab.
Description
Изобретение относитс к способам получени оксонитрата свинца, который может быть использован в промышленности неорганического синтеза.The invention relates to methods for producing lead oxonitrate, which can be used in the industry of inorganic synthesis.
Цель изобретени - интенсификаци и упрощение процесса.The purpose of the invention is to intensify and simplify the process.
Способ заключаетс в том, что оксид свинца обрабатывают раствором нитрата аммони в диметилформамиде (ДМФА) или диметилсульфоксиде (ДМСО) при мол рном соотношении оксид свинца:нитрат аммони , равном 1:1,5-3.The method consists in that the lead oxide is treated with a solution of ammonium nitrate in dimethylformamide (DMF) or dimethyl sulfoxide (DMSO) at a molar ratio of lead oxide: ammonium nitrate equal to 1: 1.5-3.
Взаимодействие исходных компонентов по предлагаемому способу идет и при обычной температуре, однако нагревание реакционной смеси увеличивает скорость процесса. Выбор температуры процесса (50°С) сделан с учетом свойств используемых растворителей и технических характеристик используемого оборудовани .The interaction of the source components of the proposed method is at a normal temperature, however, the heating of the reaction mixture increases the speed of the process. The choice of process temperature (50 ° C) was made taking into account the properties of the solvents used and the technical characteristics of the equipment used.
П р и м е р. В реактор внос т 2,23 г (0,01 моль) оксида свинца и 1,19 г (0.015 моль) нитрата аммони (мол рное соотношение 1:1,5), приливают 50 мл ДМСО и нагревают 15 мин при 50°С и посто нном перемешивании . Отфильтровывают бесцветный осадок. Выход 2,5 г (90%).PRI me R. 2.23 g (0.01 mol) of lead oxide and 1.19 g (0.015 mol) of ammonium nitrate (molar ratio 1: 1.5) are introduced into the reactor, 50 ml of DMSO are added and heated for 15 minutes at 50 ° C and constant mixing. The colorless precipitate is filtered off. Yield 2.5 g (90%).
Найдено,%. РЬ 75,7.Found,%. Pb 75.7.
Вычислено,%: РЬ 74.75.Calculated,%: Pb 74.75.
Результаты остальных примеров представлены в таблице,The results of the remaining examples are presented in the table,
Как видно из данных примеров 1-8, дл получени оксонитрата свинца, оптимальным соотношением исходных вл етс 1:1,5-3. При соотношении меньшем, чем 1:1,5, продукт загр знен оксидом свинца, а увеличение соотношени исходных больше чем 1:3 не приводит к получению дополнительного положительного эффекта.As can be seen from the data of examples 1-8, for the preparation of lead oxonitrate, the optimal baseline ratio is 1: 1.5-3. When the ratio is less than 1: 1.5, the product is contaminated with lead oxide, and an increase in the ratio of the starting materials to more than 1: 3 does not result in an additional positive effect.
Как видно из данных примеров 9-10, ацетонитрил и метанол непригодны дл получени оксонитрата свинца предлагаемым способом, так как в их среде не достигаетс полного превращени оксида свинца, который в конечном результате загр зн ет целевой продукт.As can be seen from the data of examples 9-10, acetonitrile and methanol are unsuitable for obtaining lead oxonitrate by the proposed method, since in their environment, complete conversion of lead oxide is not achieved, which ultimately contaminates the target product.
Таким образом, предлагаемый способ позвол ет по сравнению с прототипом упсл СThus, the proposed method allows comparison with the prototype ups C
О 00 О О Ы ГОO 00 O O S GO
ростить процесс за счет сокращени числа операций, в также сократить врем протекани процесса с 10 дней до 15 мин.to increase the process by reducing the number of operations, and also to reduce the time of the process from 10 days to 15 minutes.
Claims (1)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU884605491A SU1680631A1 (en) | 1988-11-14 | 1988-11-14 | Method for obtaining lead oxoacetate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU1680632A1 true SU1680632A1 (en) | 1991-09-30 |
Family
ID=21409431
Family Applications (3)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU4605491K SU1680633A1 (en) | 1988-11-14 | 1988-11-14 | Method for obtaining lead oxonitrate |
| SU884605491A SU1680631A1 (en) | 1988-11-14 | 1988-11-14 | Method for obtaining lead oxoacetate |
| SU4605491L SU1680632A1 (en) | 1988-11-14 | 1988-11-14 | Method for obtaining lead oxobromide |
Family Applications Before (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU4605491K SU1680633A1 (en) | 1988-11-14 | 1988-11-14 | Method for obtaining lead oxonitrate |
| SU884605491A SU1680631A1 (en) | 1988-11-14 | 1988-11-14 | Method for obtaining lead oxoacetate |
Country Status (1)
| Country | Link |
|---|---|
| SU (3) | SU1680633A1 (en) |
-
1988
- 1988-11-14 SU SU4605491K patent/SU1680633A1/en active
- 1988-11-14 SU SU884605491A patent/SU1680631A1/en active
- 1988-11-14 SU SU4605491L patent/SU1680632A1/en active
Non-Patent Citations (1)
| Title |
|---|
| 1.Appl. Chem. and Biotechnol, 1974. 24. N 10, 571-581. * |
Also Published As
| Publication number | Publication date |
|---|---|
| SU1680633A1 (en) | 1991-09-30 |
| SU1680631A1 (en) | 1991-09-30 |
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