SU789492A1 - Method of purifying terpenic or sesquiterpenic aldehydes - Google Patents
Method of purifying terpenic or sesquiterpenic aldehydes Download PDFInfo
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- SU789492A1 SU789492A1 SU782657204A SU2657204A SU789492A1 SU 789492 A1 SU789492 A1 SU 789492A1 SU 782657204 A SU782657204 A SU 782657204A SU 2657204 A SU2657204 A SU 2657204A SU 789492 A1 SU789492 A1 SU 789492A1
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- SU
- USSR - Soviet Union
- Prior art keywords
- aldehydes
- purifying
- sesquiterpenic
- terpenic
- citral
- Prior art date
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Description
Изобретение относитс к химическ технологии, конкретно, к способу очистки терпеновых или сесквитерпеновых альдегидов, примен емых в качестве душистых веществ и полупродуктов тонкого органического синтез При очистке терпеновых или сескв терпеновых альдегидов ректификацией происходит заметна изомеризаци ,На ример при изомеризации цитрал при температуре в кубе 130 С при 10 мм рт.ст. даже в стекл нной аппаратуре и в атмосфере аргона степень изомеризации цитрал составл ет 25%,а .при 175°С - 100%, 1 Продуктами изомеризации вл етс З-алкенали, а также циклические продукты, наличие которых значитель но ухудшает парфюмерные качества целевого продукта. Цель иэооретени - повьшение качеств целевого продукта. Поставленна цель достигаетс способом очистки терпеновых или сесквитерпеновых альдегидов путем ректификации в присутствии триэтаноламиновыас солей органических вз тых в количестве кислот С, - Cijci I ,0,5-5% jBec.%, Отличительным признаком способа вл етс проведение ректификации в присутствии триэтаноламиновых солей органических кислот Cg, вз тых в количестве 0,5-5 вес,% Пример 1. В ректификационную аппаратуру из нержавеющей стали (колонна насадочна высотой 4м, диаметром 50 мм, 20 теоретических тарелок) непрерывно направл ют сверху сырой цитраль (1 л/ч), который содержит гераниал и нерал (об-и Jb-цитрал ) 81,2%, других изомеров цктрал 0,3% и вьацекип щие смолистые примеси. Ректифицируют при 10 мм рт.ст. в верхушке колонны, температура в кубе 130°С, флегмовое число 4. Флегму направл ют в колонну через миристат триэтаноламина. Ректифицируют 22,1 кг сырого цитрал . Получают 11,3 кг дистилл та, содержащего 97,3% гераниал и нерал , 0,5% других изомеров цитрал и 2,2% вышекип щих примесей. Кубовый остаток направл ют на повторную непрерывную ректификацию. Пример 2.В стекл нную ректификационную аппаратуру, состо щую из четырехлитровой колСы и насадочной колонны с 28 теоретическимиThe invention relates to chemical technology, specifically, to a method for purification of terpene or sesquiterpene aldehydes used as fragrances and intermediates for fine organic synthesis. When purifying terpene or sesquus terpene aldehydes by distillation, isomerization is noticeable. at 10 mm Hg even in glass equipment and in argon atmosphere, the degree of isomerization of citral is 25%, and at 175 ° C - 100%, 1 Isomerization products are 3-alkeneals, as well as cyclic products, the presence of which significantly affects the perfume quality of the target product . The goal of ioretreni is to increase the qualities of the target product. This goal is achieved by the method of purification of terpene or sesquiterpene aldehydes by rectification in the presence of triethanolamine salts of organic acids taken in quantity of C acids, - Cijci I, 0.5-5% jBec.%, A distinctive feature of the method is to conduct rectification in the presence of triethanolamine salts of organic acids Cg, taken in an amount of 0.5-5% by weight. Example 1. Stainless steel distillation apparatus (packed column 4 m in height, 50 mm in diameter, 20 theoretical plates) is continuously sent from the top with raw citral ü (1 l / h), which contains geranial and neral (ob-and Jb-citral) 81.2%, other isomers 0.3 ml of citral and viscous resinous impurities. Rectified at 10 mm Hg. at the top of the column, the temperature in the cube is 130 ° C, the reflux number is 4. The reflux is directed to the column through triethanolamine myristate. 22.1 kg of crude citral are rectified. 11.3 kg of distillate containing 97.3% geranial and nonral, 0.5% other isomers of citral and 2.2% of above-boiling impurities are obtained. The bottoms are sent to re-continuous distillation. Example 2. In a glass distillation apparatus consisting of a four-liter column and a packed column with 28 theoretical
Claims (1)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SU782657204A SU789492A1 (en) | 1978-06-19 | 1978-06-19 | Method of purifying terpenic or sesquiterpenic aldehydes |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SU782657204A SU789492A1 (en) | 1978-06-19 | 1978-06-19 | Method of purifying terpenic or sesquiterpenic aldehydes |
Publications (1)
Publication Number | Publication Date |
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SU789492A1 true SU789492A1 (en) | 1980-12-23 |
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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SU782657204A SU789492A1 (en) | 1978-06-19 | 1978-06-19 | Method of purifying terpenic or sesquiterpenic aldehydes |
Country Status (1)
Country | Link |
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SU (1) | SU789492A1 (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0320728A2 (en) * | 1987-12-12 | 1989-06-21 | Hoechst Aktiengesellschaft | Process for the stabilization of aldehydes |
-
1978
- 1978-06-19 SU SU782657204A patent/SU789492A1/en active
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0320728A2 (en) * | 1987-12-12 | 1989-06-21 | Hoechst Aktiengesellschaft | Process for the stabilization of aldehydes |
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