CN101885673A - Nature-identical 2,3-butanedione flavor and preparation method thereof - Google Patents
Nature-identical 2,3-butanedione flavor and preparation method thereof Download PDFInfo
- Publication number
- CN101885673A CN101885673A CN2010102227261A CN201010222726A CN101885673A CN 101885673 A CN101885673 A CN 101885673A CN 2010102227261 A CN2010102227261 A CN 2010102227261A CN 201010222726 A CN201010222726 A CN 201010222726A CN 101885673 A CN101885673 A CN 101885673A
- Authority
- CN
- China
- Prior art keywords
- reaction
- acetaldehyde
- dimethyl diketone
- spices
- composite catalyst
- 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.)
- Pending
Links
Abstract
The invention relates to a nature-identical 2,3-butanedione flavor and a preparation method thereof. The nature-identical 2,3-butanedione flavor contains the following components in parts by weight: 1000 parts of acetaldehyde and 1-10 parts of composite catalyst. By adopting the technology of the invention, the raw materials are accessible, the conversion rate of the raw materials is high, the conditions of the two-step reaction are mild, the content of 2,3-butanedione in the product is high, the natural degree is high, the production technology is clean, mass production can be realized, the production cost is low, and three wastes can not be generated.
Description
Technical field
The present invention relates to a kind of natural equivalent 2,3-dimethyl diketone spices and technology of preparing thereof.
Background technology
2, the 3-dimethyl diketone claims di-acetyl again, is called for short DC, molecular formula is CH3COCOCH3, is the important spices that a kind of yellow to light green has strong cream fragrance, and FEMA numbers 2370, CAS 431-03-8, be widely used in preparing butter flavour, strawberry flavour, aroma essence, piglet feed essence, the stiffening agent that also can be used as gelatin also can be used as medicine in addition, agricultural chemicals and fine chemicals (as heterogeneous ring compound) synthetic intermediate.
The preparation dimethyl diketone mainly contains following several method both at home and abroad at present:
1, natural goods extraction method: from the essential oil that contains dimethyl diketone, adopt free method to make, can't suitability for industrialized production because raw material expensive product cost is too high.2, methylethylketone oxidation style: this method has been carried out a lot of concrete deep researchs both at home and abroad, can adopt different oxygenants to prepare dimethyl diketone, as Sodium Nitrite oxidation style, tin anhydride ozone oxidation method, air oxidation process etc., but owing to pollute heavy, catalyzer costs an arm and a leg, the oxidizing condition harshness, complex process, rare natural equivalent high purity product.3, methylethylketone oximate method, this method is the method that present domestic manufacturer generally adopts, be under the acid effect, to carry out oximation reaction with methylethylketone and nitrous acid ester, through crystallization, hydrolysis, processes such as distillation prepare dimethyl diketone, this technology is seriously polluted equally, and nitrous acid ester toxicity is big, and products obtained therefrom purity is low, and the natural equivalent degree is poor.4, isobutyric aldehyde vapour phase oxidation process, this method is raw material with the isobutyric aldehyde, uses atmospheric oxidation, and research is more both at home and abroad in the recent period, generally believes to be better than 1～3 method, but exists reaction complicated, and side reaction reaches pollution problem more, and product natural equivalent degree is poor.5, microbe fermentation method, though this method can obtain the natural equivalent dimethyl diketone, because of productive rate is low, investment is big, fermentation waste water is administered difficult and is difficult to large-scale production.
Summary of the invention
The present invention is exactly at the problems referred to above, proposes a kind of new technical scheme.Step of the present invention is simple, is convenient to operation, and cost is low, adopt that the technology of the present invention obtains 2,3-dimethyl diketone product fragrance is pure, can accomplish scale production.
Technical scheme provided by the invention is:
Natural equivalent 2,3-dimethyl diketone spices comprises acetaldehyde and composite catalyst, the weight ratio relation of acetaldehyde and composite catalyst: 1000 parts acetaldehyde needs 1～10 part composite catalyst proportioning.
Acetaldehyde is to be produced by the fermentation method alcohol dehydrogenase.
Natural equivalent 2, the preparation method of 3-dimethyl diketone spices may further comprise the steps:
The first step, in pressure reaction still, add the acetaldehyde and the composite catalyst of required weight proportion relation, temperature of reaction is controlled at 20～180 ℃, and reaction pressure is controlled at 0.2～2.5Mpa, and the reaction times is 1.8～3 hours, the full gear of lowering the temperature then is at last with standby behind the reacting liquid filtering composite catalyst;
Add saturated Fe on second step, the reaction fractionating tower continuously
3+The reaction solution of salts solution and the first step preparation, rectifying obtains 2, the 3-dimethyl diketone, 60～85 ℃ of reactive distillation cat head temperature, control of reflux ratio is 1～5, and the reaction fractionating tower interior reaction temperature is at 80～110 ℃.
Acetaldehyde is to be produced by the fermentation method alcohol dehydrogenase.
Adopt the technology of the present invention raw material to be easy to get, the feed stock conversion height, the two-step reaction mild condition, product 2,3-dimethyl diketone content height, natural degree height, the production technique cleaning is produced on a large scale, and production cost is low, does not have " three wastes ".
Acetaldehyde is to be produced by the fermentation method alcohol dehydrogenase, keeping 2, the 3-dimethyl diketone
14The C specific activity.
Gained natural equivalent 2,3-dimethyl diketone spices be through gas chromatographic analysis 2,3-dimethyl diketone content 〉=99% (wt).Natural degree is through the natural degree assess and determine 2 of Shanghai radiation institute of Pharmaceutical Research, the 3-dimethyl diketone
14C specific activity 15.2DPM/g.C, 2, the natural degree of 3-dimethyl diketone is 98%, fragrance is pure.
Embodiment
Natural equivalent 2,3-dimethyl diketone spices comprises acetaldehyde and composite catalyst, the weight ratio relation of acetaldehyde and composite catalyst: 1000 parts acetaldehyde needs 6 parts composite catalyst proportioning.
Acetaldehyde is to be produced by the fermentation method alcohol dehydrogenase.
Natural equivalent 2, the preparation method of 3-dimethyl diketone spices may further comprise the steps:
The first step, in pressure reaction still, add the acetaldehyde and the composite catalyst of required weight proportion relation, temperature of reaction is controlled at 20～180 ℃, and reaction pressure is controlled at 0.2～2.5Mpa, and the reaction times is 1.8～3 hours, the full gear of lowering the temperature then is at last with standby behind the reacting liquid filtering composite catalyst;
Add saturated Fe on second step, the reaction fractionating tower continuously
3+The reaction solution of salts solution and the first step preparation, rectifying obtains 2, the 3-dimethyl diketone, 60～85 ℃ of reactive distillation cat head temperature, control of reflux ratio is 1～5, and the reaction fractionating tower interior reaction temperature is at 80～110 ℃.
Should be noted that at last: above embodiment is only in order to illustrate that technical scheme of the present invention is not intended to limit; Although with reference to preferred embodiment the present invention is had been described in detail, those of ordinary skill in the field are to be understood that: still can make amendment or the part technical characterictic is equal to replacement the specific embodiment of the present invention; And not breaking away from the spirit of technical solution of the present invention, it all should be encompassed in the middle of the technical scheme scope that the present invention asks for protection.
Claims (4)
1. natural equivalent 2, and 3-dimethyl diketone spices is characterized in that, comprises acetaldehyde and composite catalyst, and the weight ratio relation of acetaldehyde and composite catalyst: 1000 parts acetaldehyde needs 1～10 part composite catalyst proportioning.
2. according to the described natural equivalent 2 of claim 1,3-dimethyl diketone spices is characterized in that, acetaldehyde is to be produced by the fermentation method alcohol dehydrogenase.
3. according to the described natural equivalent 2 of claim 1, the preparation method of 3-dimethyl diketone spices is characterized in that,
May further comprise the steps:
The-step, in pressure reaction still, add the acetaldehyde and the composite catalyst of required weight proportion relation, temperature of reaction is controlled at 20～180 ℃, and reaction pressure is controlled at 0.2～2.5Mpa, and the reaction times is 1.8～3 hours, the full gear of lowering the temperature then is at last with standby behind the reacting liquid filtering composite catalyst;
Add saturated Fe on second step, the reaction fractionating tower continuously
3+The reaction solution of salts solution and the first step preparation, rectifying obtains 2, the 3-dimethyl diketone, 60～85 ℃ of reactive distillation cat head temperature, control of reflux ratio is 1～5, and the reaction fractionating tower interior reaction temperature is at 80～110 ℃, and products obtained therefrom is natural equivalent 2,3-dimethyl diketone spices.
4. according to the described natural equivalent 2 of claim 3, the preparation method of 3-dimethyl diketone spices is characterized in that, acetaldehyde is to be produced by the fermentation method alcohol dehydrogenase.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102227261A CN101885673A (en) | 2010-06-30 | 2010-06-30 | Nature-identical 2,3-butanedione flavor and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102227261A CN101885673A (en) | 2010-06-30 | 2010-06-30 | Nature-identical 2,3-butanedione flavor and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101885673A true CN101885673A (en) | 2010-11-17 |
Family
ID=43071791
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010102227261A Pending CN101885673A (en) | 2010-06-30 | 2010-06-30 | Nature-identical 2,3-butanedione flavor and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101885673A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103159603A (en) * | 2013-02-28 | 2013-06-19 | 河南华龙香料有限公司 | Clean production method of 2,3-heptadione |
| CN109206305A (en) * | 2018-10-30 | 2019-01-15 | 盐城市春竹香料有限公司 | A method of diacetyl is continuously prepared using reactive distillation column |
-
2010
- 2010-06-30 CN CN2010102227261A patent/CN101885673A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103159603A (en) * | 2013-02-28 | 2013-06-19 | 河南华龙香料有限公司 | Clean production method of 2,3-heptadione |
| CN109206305A (en) * | 2018-10-30 | 2019-01-15 | 盐城市春竹香料有限公司 | A method of diacetyl is continuously prepared using reactive distillation column |
| CN109206305B (en) * | 2018-10-30 | 2021-07-20 | 盐城市春竹香料有限公司 | Method for continuously preparing butanedione by using reactive distillation column |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102276464B (en) | Method for producing methyl acetoacetate | |
| CN101544548A (en) | Method for preparing aldehydes or ketones by oxidizing alcohols with oxygen | |
| CN111187148B (en) | Method for simultaneously preparing o-hydroxy phenetole and 1, 3-benzodioxole-2-one | |
| CN106916060B (en) | Preparation method of high-purity p-hydroxyacetophenone | |
| CN102126953A (en) | Preparation method of nonanal and methyl formylcaprylate | |
| CN102311332A (en) | Method for producing succinic acid | |
| JPH01146840A (en) | Production of ehther carboxylic acid | |
| CN105175229A (en) | Catalytic hydrogenation synthesis method for prenyl alcohol | |
| CN101885673A (en) | Nature-identical 2,3-butanedione flavor and preparation method thereof | |
| CN102452871B (en) | Method for catalytic oxidation of cyclic ketone | |
| CN111875493B (en) | Method for synthesizing borneol by using imidazole acidic ionic liquid | |
| CN101323567B (en) | Process for preparing cinnamate and derivates thereof | |
| CN103193636B (en) | A kind of method of synthesizing 2,3-butanediol ester | |
| CN110950745B (en) | Preparation method of phenylacetaldehyde | |
| KR101317924B1 (en) | Synthetics method of Glycopyrrolate and pharmaceutical formulations containing this active ingredient | |
| CN103288626A (en) | Method for co-producing adipic acid and nitrocyclohexane | |
| CN107088437B (en) | Catalyst for synthesis of isobornyl acetate and synthesis method of isobornyl acetate | |
| CN107805201A (en) | A kind of preparation method of MDJ | |
| CN107602393A (en) | A kind of method that benzyl position C H keys are direct oxidation into ketone or acid | |
| CN105175220A (en) | Hydrogenation catalytic synthesis method of isopentenol | |
| CN102452923B (en) | Method for catalytically oxidizing lactone | |
| CN111187146A (en) | Method for producing 2-methyl-3-buten-2-ol | |
| CN107445828B (en) | Method for synthesizing glyoxylic acid esters | |
| CN109824483B (en) | New method for preparing nopol | |
| CN109574814A (en) | A kind of method that toluene liquid phase catalytic oxidation prepares benzaldehyde and benzyl alcohol |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20101117 |