Method for preparing low grade aliphatic acid polyatomic alcohol mixing ester and application thereof in tobacco

A low-level fatty acid and polyol technology, applied in the field of tobacco flavors and fragrances, can solve the problems of unsuitable production of tobacco flavors and fragrances, complicated process, and large environmental pollution, and achieve low cost, increased reaction yield, and low environmental pollution. Effect

Inactive Publication Date: 2008-09-10
ZHENGZHOU TOBACCO RES INST OF CNTC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Concentrated sulfuric acid and p-toluenesulfonic acid are used as catalysts, the process is complicated, the corrosion is strong, and the environment is polluted
Although the enzyme-catalyzed synthesis of polyol esters has selectivity in the esterification site, the cost is too high and it is not suitable for the production of flavors and fragrances for tobacco

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Weigh 7.5g of TiSiW activated at 300°C for 2 hours 12 o 40 / TiO 2 1. Add 598g of butyric acid into a 2000ml three-necked flask, and place it in an oil bath reactor with mechanical stirring. After the catalyst is fully dispersed, add 152g of xylitol and 50ml of cyclohexane, and continue stirring to form a uniform suspension. Control the temperature at 90°C, react for 2 hours, stop the reaction, filter the reaction solution to remove the catalyst, distill off the cyclohexane and excess butyric acid from the filtrate, dissolve it in 1000ml ethyl acetate, wash the ethyl acetate solution with saturated sodium bicarbonate After washing to neutrality, wash with deionized water for 3 times, collect the oil phase and dry it with sodium bisulfate, then evaporate under reduced pressure to remove ethyl acetate to obtain 343 g of light yellow viscous oily substance with a yield of about 82%. The catalyst is reused after regeneration.

[0022] Quantitative analysis by high perform...

Embodiment 2

[0025] Weigh 8.2g of TiSiW activated at 300°C for 2 hours 12 o 40 / TiO 2 663g of valeric acid was added into a 2000ml three-necked flask, and placed in an oil bath reactor. After the catalyst was fully dispersed, 152g of xylitol and 50ml of cyclohexane were added, and the stirring was continued to form a uniform suspension. Control the temperature at 90°C, react for 2 hours, stop the reaction, filter the reaction solution to remove the catalyst, distill off the cyclohexane and excess valeric acid from the filtrate, dissolve it in 1000ml ethyl acetate, wash the ethyl acetate solution with saturated sodium bicarbonate After washing to neutrality, wash with deionized water for 3 times, collect the oil phase and dry it with sodium bisulfate, then evaporate under reduced pressure to remove ethyl acetate to obtain 364 g of light yellow viscous oily substance with a yield of about 78%. The catalyst is reused after regeneration.

[0026] Quantitative analysis by high performance li...

Embodiment 3

[0029] Weigh 8.5 g of H 3 PW 12 o 40 / SiO 2 1. Add 663g of isovaleric acid into a 2000ml three-neck flask, and place it in a microwave reactor with mechanical stirring. After the catalyst is fully dispersed, add 180g of glucose and 50ml of cyclohexane, and continue stirring to form a uniform suspension. Control the temperature in an oil bath at 90°C. After reacting for 2 hours, stop the reaction, filter the reaction solution to remove the catalyst, and distill off cyclohexane and excess valeric acid from the filtrate, dissolve it in 1000ml ethyl acetate, and dilute the ethyl acetate solution with saturated carbonic acid After washing with sodium hydrogen to neutrality, and then washing with deionized water three times, the oil phase was collected and dried with sodium bisulfate, and then the ethyl acetate was removed by rotary evaporation to obtain 362 g of light yellow viscous oily substance with a yield of about 88%. The catalyst is reused after regeneration.

[0030] Qu...

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PUM

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Abstract

The invention relates to a preparation method for low-level fatty acid and polyol mixed ester and application thereof. The preparation method comprises the following steps that: heteropoly acid is used as catalyst; low-level fatty acid and polyol are used as reaction material; esterification reaction is carried out to the reaction material at a certain temperature; polyol mixed ester products of the invention are obtained by purifying the reaction material. The preparation method has the advantages of adopting solid-supported heteropoly acid to catalyze the synthesis of low-level fatty acid and polyol and improving reaction rate and yield significantly. As the method is short in reaction time, high in yield and capable of utilizing catalyst repeatedly, the cost is relatively lower and the environmental pollution is little. The operation of adding the low-level fatty acid and polyol mixed ester prepared by the invention into cigarettes can have significant flavoring effect, which can enrich flavor, coordinate cigarette flavour, reduce stimulation and improve aftertaste, so as to integrally promote the sensory quality of cigarettes.

Description

Technical field: [0001] The patent of the present invention relates to a preparation method of a tobacco spice-lower fatty acid polyol mixed ester and its application in tobacco. The method uses lower fatty acid and polyhydric alcohol contained in tobacco as raw materials, carries out esterification under the condition of immobilized heteropolyacid catalysis, and obtains lower fatty acid polyhydric alcohol mixed ester. Adding the low-level fatty acid polyol mixed ester prepared by the method to tobacco products can have obvious flavoring effect. technical background: [0002] C has been found in tobacco 1 ~C 34 Among them, formic acid, acetic acid, propionic acid, butyric acid, isobutyric acid, valeric acid, isovaleric acid, β-methylvaleric acid, hexanoic acid and other volatile lower fatty acids are important for the sensory quality of tobacco leaves. influences. For flue-cured tobacco, the content of volatile organic acids in tobacco leaves with full aroma is significa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08A24B15/30B01J23/30B01J27/188
CPCY02P20/584
Inventor 李鹏曾世通胡军宗永立
Owner ZHENGZHOU TOBACCO RES INST OF CNTC
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