CN101823960A - Method for preparing monomenthyl succinate sodium aliphatate - Google Patents
Method for preparing monomenthyl succinate sodium aliphatate Download PDFInfo
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- CN101823960A CN101823960A CN200910232167A CN200910232167A CN101823960A CN 101823960 A CN101823960 A CN 101823960A CN 200910232167 A CN200910232167 A CN 200910232167A CN 200910232167 A CN200910232167 A CN 200910232167A CN 101823960 A CN101823960 A CN 101823960A
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- succinate sodium
- monomenthyl succinate
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- sodium aliphatate
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Abstract
The invention discloses a method for preparing monomenthyl succinate sodium aliphatate. The method comprises the following steps of: 1, adding menthol crystal into a reaction vessel, raising the temperature and stirring the menthol crystal until the solid substance in the reaction vessel is melted completely, and adding succinic anhydride to perform heat preservation reaction; 2, after the reaction is finished, adding water to perform reflux, standing the reaction product to separate liquid from the reaction product, adding ethyl acetate to perform extraction, combining organic phases, drying, filtering and desolventizing; 3, adding petroleum ether to be used as a recrystallizing solvent, dissolving and recrystallizing the mixture, adding the recrystallization product into another reaction vessel, adding methyl tertiary butyl ether to be used as a reaction solvent, and heating to perform reflux; and 4, adding aqueous solution of sodium carbonate dropwise, refluxing to separate water, filtering the product directly, and performing vacuum drying to obtain the monomenthyl succinate sodium aliphatate. The method has the advantages of scientific material selection, proper proportion, simpleness, suitability for industrial production, short reaction time, high yield and good quality of products.
Description
Technical field
The invention belongs to preparation method as the technology, particularly a kind of monomenthyl succinate sodium aliphatate of freshener, coolant agent raw material.
Background technology
Along with the raising of expanding economy and the people's lives water product and the level of consumption, the human consumer is to the demand of food and also more and more higher to the requirement of food taste.In products such as daily use chemicals, food, personal care, the demand of freshener is also in continuous expansion, and the demand of foreign market expands day by day, and the demand of domestic market is also in continuous expansion.
As widely used coolant agent abroad, the sodium salt of monomethyl succinate can provide cooling effect pleasant, long lasting, without sensation of pricking, its cooling effect is different with other coolant agents again simultaneously, and especially it is in the utilization better effects if that contains in the alcoholic beverage.But there is not the synthetic report of its industrialization at present.
Summary of the invention
The object of the present invention is to provide a kind of reaction times short, yield is high, cost is low, the industrialized process for preparing of the monomenthyl succinate sodium aliphatate of good product quality.
The technical solution that realizes the object of the invention is: a kind of preparation method of monomenthyl succinate sodium aliphatate may further comprise the steps:
The first step adds mentha camphor in the reactor, heats up, stirs, and solid all melts to the still, adds Succinic anhydried, insulation reaction subsequently;
In second step, reaction adds entry and refluxes, and leave standstill separatory after finishing, and adds ethyl acetate extraction subsequently, merges organic phase, drying, filtration, precipitation;
The 3rd step added sherwood oil as recrystallization solvent, and dissolving-recrystallization adds crystalline product in another reactor, added methyl tertiary butyl ether as reaction solvent, reflux;
The 4th step dripped aqueous sodium carbonate, reflux water-dividing, and direct filtration goes out product, and vacuum-drying obtains monomenthyl succinate sodium aliphatate.
The present invention compared with prior art, its remarkable advantage: (1) selection science, proportioning is suitable, method is simple, is applicable to suitability for industrialized production; (2) reaction times is short, yield is high, good product quality; (3) reduce environmental pollution, do not add any organic solvent, it is synthetic to belong to solventless method; (4) cost is low, makes convenient cheap being easy to get of monomenthyl succinate sodium aliphatate, promotes the utilization of monomenthyl succinate sodium aliphatate in wider scope.
Embodiment
The industrialized process for preparing of monomenthyl succinate sodium aliphatate of the present invention comprises the steps:
(1) mentha camphor is added in the reactor, be warming up to 110-140 ℃, open to stir, solid all melts to the still, reaches 110 ℃ to temperature in the kettle, adds Succinic anhydried subsequently; Adopting mentha camphor and Succinic anhydried is raw material, its separately weight percent be respectively 60～50%, 50～60% of reaction mixture.
(2) keep 110-140 ℃ of reaction 6-18 hour;
(3) after reaction finishes, add entry, refluxed 2 hours, left standstill separatory 30 minutes, add ethyl acetate separatory extraction while hot subsequently, merge organic phase, drying is filtered precipitation;
(4) add sherwood oil as recrystallization solvent, dissolving-recrystallization;
(5) crystalline product is added in the still, add methyl tertiary butyl ether as reaction solvent, reflux 15 minutes;
(6) drip aqueous sodium carbonate, reflux water-dividing 5 hours;
(7) filter out product, vacuum-drying.
Below in conjunction with embodiment the present invention is done further detailed description.
Embodiment 1
The preparation of menthyl succinate sodium salt
Earlier 156.27 kilograms of mentha camphor are added in the reactor, open and stir, treat that temperature in the kettle reaches 110 ℃, add 100 kilograms of Succinic anhydrieds, keep 110 ℃ of reactions 12 hours, add 200 kg of water subsequently, refluxed 2 hours.Cold slightly, standing demix 30 minutes, separatory while hot, water is used 200 kilograms of ethyl acetate extractions once again, separatory.Merge organic phase, anhydrous sodium sulfate drying filters, and ethyl acetate is reclaimed in distillation.After the ethyl acetate distillation is finished, 300 kilograms of sherwood oils are added in the reactor, refluxed 60 minutes.Cold slightly, be delivered to crystallization kettle, stirring and crystallizing under-5 ℃ of conditions.The centrifugal white products that obtains, content 99.9%, obtains 250 kilograms of monomethyl succinates, yield 96% by fusing point 62-63 ℃.
Above-mentioned monomethyl succinate is added reactor, add 800 kilograms of methyl tertiary butyl ethers subsequently, the mixing solutions of 1 kilogram of yellow soda ash of Dropwise 5 and 58 kg of water is opened stirring and refluxing and was divided water 5 hours subsequently.Cooling.Centrifuging.Product 100 degree vacuum-dryings 12 hours obtain the menthyl succinate sodium salt.
Embodiment 2
The preparation of menthyl succinate sodium-salt aqueous solution
Earlier 156.27 kilograms of mentha camphor are added in the reactor, open and stir, treat that temperature in the kettle reaches 110 ℃, add 100 kilograms of Succinic anhydrieds, keep 110 ℃ of reactions 10 hours, add 200 kg of water subsequently, refluxed 2 hours.Cold slightly, standing demix 30 minutes, separatory while hot, water is used 200 kilograms of ethyl acetate extractions once again, separatory.Merge organic phase, anhydrous sodium sulfate drying filters, and ethyl acetate is reclaimed in distillation.After the ethyl acetate distillation is finished, 300 kilograms of sherwood oils are added in the reactor, refluxed 15 minutes.Cold slightly, be delivered to crystallization kettle, stirring and crystallizing under-5 ℃ of conditions.The centrifugal white products that obtains, content 99.9%, obtains 250 kilograms of monomethyl succinates, yield 96% by fusing point 62-63 ℃.
Above-mentioned monomethyl succinate is added reactor, and temperature rises to 70 degree, to all being molten into liquid, the mixing solutions of 1 kilogram of yellow soda ash of Dropwise 5 and 254.5 kg of water.Insulated and stirred 10 hours.Reaction filters out mechanical impurity after finishing, and gets 500 kilogram of 50% menthyl succinate sodium-salt aqueous solution.
Embodiment 3
The preparation of menthyl succinate sodium salt:
Earlier 156.27 kilograms of mentha camphor are added in the reactor, open and stir, treat that temperature in the kettle reaches 110 ℃, add 100 kilograms of Succinic anhydrieds, keep 140 ℃ of reactions 6 hours, add 200 kg of water subsequently, refluxed 2 hours.Cold slightly, standing demix 30 minutes, separatory while hot, water is used 200 kilograms of ethyl acetate extractions once again, separatory.Merge organic phase, anhydrous sodium sulfate drying filters, and ethyl acetate is reclaimed in distillation.After the ethyl acetate distillation is finished, 300 kilograms of sherwood oils are added in the reactor, refluxed 30 minutes.Cold slightly, be delivered to crystallization kettle, stirring and crystallizing under-5 ℃ of conditions.The centrifugal white products that obtains, content 99.9%, fusing point 62-63 ℃, yield 94%.
Above-mentioned monomethyl succinate is added reactor, add 800 kilograms of methyl tertiary butyl ethers subsequently, the mixing solutions of 1 kilogram of yellow soda ash of Dropwise 5 and 58 kg of water is opened stirring and refluxing and was divided water 5 hours subsequently.Cooling.Centrifuging.Product 100 degree vacuum-dryings 12 hours obtain the menthyl succinate sodium salt.
Claims (6)
1. the preparation method of a monomenthyl succinate sodium aliphatate is characterized in that, may further comprise the steps:
The first step adds mentha camphor in the reactor, heats up, stirs, and solid all melts to the still, adds Succinic anhydried, insulation reaction subsequently;
In second step, reaction adds entry and refluxes, and leave standstill separatory after finishing, and adds ethyl acetate extraction subsequently, merges organic phase, drying, filtration, precipitation;
The 3rd step added sherwood oil as recrystallization solvent, and dissolving-recrystallization adds crystalline product in another reactor, added methyl tertiary butyl ether as reaction solvent, reflux;
The 4th step dripped aqueous sodium carbonate, reflux water-dividing, and direct filtration goes out product, and vacuum-drying obtains monomenthyl succinate sodium aliphatate.
2. the preparation method of monomenthyl succinate sodium aliphatate according to claim 1, it is characterized in that mentha camphor in the first step and Succinic anhydried separately weight percent be respectively 60～50%, 50～60% of reaction mixture.
3. the preparation method of monomenthyl succinate sodium aliphatate according to claim 1 is characterized in that temperature of reaction 110-140 ℃ of the intensification in the first step; 110-140 ℃ of insulation reaction temperature, the reaction times is 6-18 hour.
4. the preparation method of monomenthyl succinate sodium aliphatate according to claim 1 is characterized in that the return time in second step is 2 hours, leaves standstill separatory 30 minutes.
5. the preparation method of monomenthyl succinate sodium aliphatate according to claim 1 is characterized in that the return time in the 3rd step is 15 minutes～60 minutes.
6. the preparation method of monomenthyl succinate sodium aliphatate according to claim 1 is characterized in that the time of reflux water-dividing is 5 hours in the 4th step.
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| Application Number | Priority Date | Filing Date | Title |
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| CN200910232167A CN101823960A (en) | 2009-12-02 | 2009-12-02 | Method for preparing monomenthyl succinate sodium aliphatate |
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| CN200910232167A CN101823960A (en) | 2009-12-02 | 2009-12-02 | Method for preparing monomenthyl succinate sodium aliphatate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110204445A (en) * | 2019-06-12 | 2019-09-06 | 广东广益科技实业有限公司 | Water-soluble freshener and preparation method thereof |
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2009
- 2009-12-02 CN CN200910232167A patent/CN101823960A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110204445A (en) * | 2019-06-12 | 2019-09-06 | 广东广益科技实业有限公司 | Water-soluble freshener and preparation method thereof |
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Application publication date: 20100908 |