CN1348949A - Beta-ionone producing process - Google Patents
Beta-ionone producing process Download PDFInfo
- Publication number
- CN1348949A CN1348949A CN 00125714 CN00125714A CN1348949A CN 1348949 A CN1348949 A CN 1348949A CN 00125714 CN00125714 CN 00125714 CN 00125714 A CN00125714 A CN 00125714A CN 1348949 A CN1348949 A CN 1348949A
- Authority
- CN
- China
- Prior art keywords
- beta
- lonone
- alpha
- production method
- reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A production method for beta-ionone is characterized by that after pseudoionone and methane chloride are mixed, they react under the action of concentrated sulphuric acid, and the resultant is diluted by using water and dilute acid for terminating reaction. After oil-water phase is separated, the water phase is concentrated into the concentrated sulphuric acid for reuse, the oil-phase has its pressure reduced for recovering solvent and rectification is continued, the beta-ionone product is obtained. The said method is simple and easy for operation, and its advantages include good extraction capability of solvent, reaction termination needling a little water or dilute acid and the waste acid easily concentrated so that the cost is lowered and the environment is protected.
Description
Alpha, beta-lonone is important spices, also is the important source material of preparation vitamin A, the present invention relates to a kind of technical scheme of production method of alpha, beta-lonone.
Traditional prepare the technology of alpha, beta-lonone by citrylideneacetone, under the normal pressure, citrylideneacetone carries out ring-closure reaction and generates alpha, beta-lonone under the strong acid effect in methylene dichloride or sherwood oil equal solvent.After the shortcoming of this method is ring-closure reaction, needs to stop, thereby produce a large amount of waste acid waters, increased three wastes processing cost, bring influence to environmental protection simultaneously with a large amount of water or diluted acid water.
The object of the invention is to overcome the defective that exists in the prior art, by selecting suitable solvent, provides a kind of production method of alpha, beta-lonone.
The production method of described alpha, beta-lonone, under the strong acid effect, carry out ring-closure reaction by citrylideneacetone, after it is characterized in that citrylideneacetone and monochloro methane mixing, react at a pipeline reactor with the vitriol oil, then in another pipeline reactor, reaction solution water or diluted acid water dilute, thereby termination reaction, through a continuous stratification device, oil phase separates with water again, and water is applied mechanically through carrying the dense vitriol oil that becomes, oil phase is through decompression, reclaim monochloro methane and get the alpha, beta-lonone crude product,, promptly get the alpha, beta-lonone finished product again through rectifying.
The weight ratio of described citrylideneacetone and monochloro methane is 1: 1.5-10 is preferably 1: 2-4; The weight ratio of the citrylideneacetone and the vitriol oil is 1: 2.5-20 is preferably 1: 3.5-5.5.The temperature of ring-closure reaction is-10-5 ℃, be preferably-2-2 ℃, and the ring-closure reaction time is 1-10 minute, is preferably 2-4 minute.Reaction is the 20-150 normal atmosphere with the pressure of extracting and demixing, is preferably the 80-120 normal atmosphere.Reaction water or diluted acid water stop, and the concentration of its diluted acid water is 45-60%.
This production method is simple; adopt monochloro methane as solvent; and make and be reflected at high pressure and carry out; because the good extracting power of this solvent under the high pressure; termination reaction only needs less water or diluted acid water; the acid-spending strength that produces is high and can directly carry dense applying mechanically, and has both reduced production costs, and helps environment protection again.
Below the invention will be further described with embodiment.
Embodiment 1: citrylideneacetone mixes in a line mixer with the flow of monochloro methane with 300g/h with the 100g/h flow, this mixed solution and flow are the vitriol oil of 350g/h then, in a pipeline reactor, react, temperature of reaction is-5 ℃, pressure is 110 normal atmosphere, and the residence time is 3 minutes.The water of reaction solution and 350g/h flow dilutes in a line mixer then, and temperature is 8 ℃, and mixing time is 1 minute.Carry out continuous stratification again under 110 normal atmosphere, water is carried dense back and is applied mechanically for the vitriol oil, and the oil phase decompression separation reclaims solvent.Continuous rectification then, getting alpha, beta-lonone is 90g/h, content is 98%.
Embodiment 2: operating procedure is the same, and the citrylideneacetone flow is 100g/h, and monochloro methane is 250g/h, and the vitriol oil is 450g/h, temperature of reaction is-2 ℃, and reaction pressure is 120 normal atmosphere, and the residence time is 5 minutes, the water yield is 500g/h, and getting alpha, beta-lonone is 91.2g/h, and content is 97.8%.
Claims (8)
1, the production method of alpha, beta-lonone, under the strong acid effect, carry out ring-closure reaction by citrylideneacetone, after it is characterized in that the citrylideneacetone monochloro methane mixes, react at a pipeline reactor with the vitriol oil, then in another pipeline reactor, reaction solution water or diluted acid water dilute, thereby termination reaction, through a continuous stratification device, oil phase separates with water again, and water is applied mechanically through carrying the dense vitriol oil that becomes, oil phase is through decompression, reclaim monochloro methane and get the jononeionone crude product,, promptly get the alpha, beta-lonone finished product again through rectifying.
2, the production method of alpha, beta-lonone as claimed in claim 1, the weight ratio that it is characterized in that citrylideneacetone and monochloro methane is 1: 1.5-10, the weight ratio of the citrylideneacetone and the vitriol oil is 1: 2.5-20.
3, the production method of alpha, beta-lonone as claimed in claim 1 is characterized in that the ring-closure reaction temperature is-10-5 ℃, and the reaction times is 1-10 minute.
4, the production method of alpha, beta-lonone as claimed in claim 1, pressure is the 20-150 normal atmosphere when it is characterized in that reaction and oil, aqueous phase separation.
5, the production method of alpha, beta-lonone as claimed in claim 1, the concentration that it is characterized in that diluted acid water is 45-60%.
6, the production method of alpha, beta-lonone as claimed in claim 1, the weight ratio that it is characterized in that citrylideneacetone and monochloro methane is 1: 2-4, the weight ratio of the citrylideneacetone and the vitriol oil is 1: 3.5-5.5.
7, the production method of alpha, beta-lonone as claimed in claim 1 is characterized in that the ring-closure reaction temperature is-2-2 ℃, and the reaction times is 2-4 minute.
8, the production method of alpha, beta-lonone as claimed in claim 1, pressure is the 80-120 normal atmosphere when it is characterized in that reaction and oil, aqueous phase separation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00125714 CN1125022C (en) | 2000-10-18 | 2000-10-18 | Beta-ionone producing process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00125714 CN1125022C (en) | 2000-10-18 | 2000-10-18 | Beta-ionone producing process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1348949A true CN1348949A (en) | 2002-05-15 |
| CN1125022C CN1125022C (en) | 2003-10-22 |
Family
ID=4591498
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 00125714 Expired - Lifetime CN1125022C (en) | 2000-10-18 | 2000-10-18 | Beta-ionone producing process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1125022C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106673980A (en) * | 2016-12-24 | 2017-05-17 | 上海弗鲁克科技发展有限公司 | Device and method for continuously producing beta-ionone by using microchannel |
| CN108329200A (en) * | 2018-03-21 | 2018-07-27 | 万华化学集团股份有限公司 | A method of preparing alpha, beta-lonone by raw material of pseudoionone |
| CN109970535A (en) * | 2019-04-23 | 2019-07-05 | 上海应用技术大学 | A kind of preparation method of alpha, beta-lonone |
| CN111285757A (en) * | 2018-12-10 | 2020-06-16 | 上虞新和成生物化工有限公司 | Method for cyclizing pseudo ionone |
| CN113603577A (en) * | 2021-07-30 | 2021-11-05 | 万华化学集团股份有限公司 | Fragrance-controllable beta-ionone and preparation method thereof |
-
2000
- 2000-10-18 CN CN 00125714 patent/CN1125022C/en not_active Expired - Lifetime
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106673980A (en) * | 2016-12-24 | 2017-05-17 | 上海弗鲁克科技发展有限公司 | Device and method for continuously producing beta-ionone by using microchannel |
| CN108329200A (en) * | 2018-03-21 | 2018-07-27 | 万华化学集团股份有限公司 | A method of preparing alpha, beta-lonone by raw material of pseudoionone |
| CN108329200B (en) * | 2018-03-21 | 2021-03-09 | 万华化学集团股份有限公司 | Method for preparing beta-ionone by using pseudoionone as raw material |
| CN111285757A (en) * | 2018-12-10 | 2020-06-16 | 上虞新和成生物化工有限公司 | Method for cyclizing pseudo ionone |
| WO2020119277A1 (en) * | 2018-12-10 | 2020-06-18 | 上虞新和成生物化工有限公司 | Method for cyclization of pseudoionone |
| CN111285757B (en) * | 2018-12-10 | 2021-07-16 | 上虞新和成生物化工有限公司 | Method for cyclizing pseudo ionone |
| CN109970535A (en) * | 2019-04-23 | 2019-07-05 | 上海应用技术大学 | A kind of preparation method of alpha, beta-lonone |
| CN109970535B (en) * | 2019-04-23 | 2021-12-24 | 上海应用技术大学 | Preparation method of beta-ionone |
| CN113603577A (en) * | 2021-07-30 | 2021-11-05 | 万华化学集团股份有限公司 | Fragrance-controllable beta-ionone and preparation method thereof |
| CN113603577B (en) * | 2021-07-30 | 2022-09-20 | 万华化学集团股份有限公司 | Fragrance-controllable beta-ionone and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1125022C (en) | 2003-10-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102627380B (en) | Efficient acidic oil sludge decomposing agent, and preparation method and application thereof | |
| CN101979680B (en) | Method for removing aluminum from rare-earth feed liquid | |
| CN104098156A (en) | Application of poly-dopamine composite magnetic micro-nano particles in oily sewage treatment | |
| CN1125022C (en) | Beta-ionone producing process | |
| CN103524017A (en) | Compound gel breaker for processing abandoned drilling mud at sea | |
| CN102795641A (en) | Novel method for direct extraction recovery of ammonia nitrogen from electrolyzed manganese slag | |
| CN107716118A (en) | A kind of preparation method and applications of Scheelite Flotation collecting agent | |
| CN106673983B (en) | A kind of preparation method of four chloro- 1,4- benzoquinones | |
| CN105854912A (en) | BiPO4-WO3 composite photocatalyst and preparation method thereof | |
| Dolbier Jr et al. | Simultaneity of allene cycloadditions. II. Dimerization of allene | |
| CN100564356C (en) | The synthesis technique of β-Hu Luobusu | |
| CN101831198B (en) | Preparation method of capsanthin | |
| CN101402552B (en) | Method for producing m-cresol with direct hydrolyzation | |
| CN101759532B (en) | Method for extracting magnolol and honokiol from magnolia officinalis | |
| WO2021068991A1 (en) | Method for preparing diosgenin by ternary two-phase aluminum chloride hydrolysis | |
| CN112850675A (en) | Method for extracting chloride ions from wet-process phosphoric acid solution by hydrochloric acid method | |
| CN106222412A (en) | A kind of from containing the method for extracting vanadium vanadium solution | |
| CN109851656A (en) | The technique of pigment and saponin is extracted in a kind of yellow ginger saponin(e | |
| CN108946777A (en) | A kind of method that system reduces Bayer process process alkaline consumption and improves process efficiency | |
| CN104845662A (en) | A method for extracting phenolic compounds in coal liquefaction oil | |
| CN106635144B (en) | A kind of method of phenolic compound concentration and separation in shale oil | |
| CN107758719A (en) | A kind of environmentally friendly extracting process of high-purity ceria | |
| CN107746402B (en) | Method for extracting tocopherol and synchronously recovering metal zinc salt from ultrasonic-assisted deodorized distillate | |
| CN101913605B (en) | Method for separating silicon carbide from silicon carbide micro-powder graded byproducts | |
| WO2019109565A1 (en) | Extraction method and extractant for denitration process in h acid production process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CX01 | Expiry of patent term | ||
| CX01 | Expiry of patent term |
Granted publication date: 20031022 |