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Aphermate and preparation method thereof
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A technology of averman ester and catalyst, which is applied in the field of averman ester and its preparation, can solve the problems of poor selectivity, complicated process, and low catalytic efficiency, so as to reduce equipment capital investment, reduce production cost, and simplify the preparation process Effect
Active Publication Date: 2020-07-17
江苏馨瑞香料有限公司
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Among them, the catalytic performance of sulfuric acid is better, and the selectivity and conversion rate of the cyclization reaction are high, but the aroma of the product is not pure; the catalytic isomerization performance of molecular sieve and phosphoric acid is strong, and the selectivity of the cyclization reaction is poor; The catalytic efficiency of ion exchange resin is low, the amount of catalyst is large, the reaction time is as long as about 30 hours, and the conversion rate of dihydromyrcene and the yield of averman ester are average
[0003] In addition, when liquid catalysts such as sulfuric acid are used, they need to be washed with water before rectification. The process is complicated and there are many equipments, which increases the capital investment required for equipment, and at the same time brings a lot of sewage, and the treatment of sewage is also greatly Raised the cost of production
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[0027] For this reason, the present invention uses trifluoromethanesulfonic acid as a catalyzer, and the preparation method of the provided Averman ester comprises:
[0028] S1, providing formic acid and a catalyst, the catalyst being trifluoromethanesulfonic acid, mixing the formic acid and the catalyst in a reaction device to obtain a first mixed liquid;
[0029] S2, at a preset temperature, adding dihydromyrcene into the reaction device in batches, allowing the dihydromyrcene to react with the formic acid under the action of the catalyst to obtain a second mixed solution;
[0030] S3, the second mixed liquid is neutralized and rectified to obtain Averman ester.
[0031] In step S2, dihydromyrcene is added in batches at a preset temperature in the first mixed solution formed by mixing trifluoromethanesulfonic acid and formic acid, and the mixture of dihydromyrcene and trifluoromethanesulfonic acid can be controlled. The mass ratio of dihydromyrcene can completely form a sta...
Embodiment 1
[0042] In the there-necked flask, add 4g trifluoromethanesulfonic acid and 420g 95% formic acid successively to form the first mixed solution, and the first mixed solution is heated to 58°C, and 480g 85% dihydromyrcene is added dropwise at a constant speed, and the dropping time After 9 hours, the reaction gave the second mixed solution.
[0043] Sodiumcarbonate is added to the second mixed liquid to neutralize to neutrality, and the formic acid is recovered by rectification to obtain the crude product of Averman ester, and the finished product of Averman ester is obtained by rectification again.
Embodiment 2
[0045] In the there-necked flask, add 4g trifluoromethanesulfonic acid and 360g 95% formic acid successively to form the first mixed solution, the first mixed solution is heated to 58°C, and 480g 85% dihydromyrcene is added dropwise at a constant speed, and the dropping time After 8 hours, the reaction gave the second mixed solution.
[0046] Potassiumcarbonate is added to the second mixed liquid to neutralize to neutrality, and the formic acid is recovered by rectification to obtain the crude product of Averman ester, and the finished product of Averman ester is obtained by rectification again.
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Abstract
The invention relates to aphermate and a preparation method thereof; the preparation method comprises the steps: providing formic acid and a catalyst which is trifluoromethanesulfonic acid, and mixingthe formic acid with the catalyst in a reaction device to obtain a first mixed solution; adding dihydromyrcene into the reaction device in batches at a preset temperature, and enabling the dihydromyrcene to react with formic acid under the action of the catalyst, so as to obtain a second mixed solution; and neutralizing and rectifying the second mixed solution to obtain aphermate. According to the method, trifluoromethanesulfonic acid is used as the catalyst, so that the catalytic efficiency is high, the conversion rate of dihydromyrcene and the yield of aphermate are high, no wastewater is generated, the process is simple, and the cost is low.
Description
technical field [0001] The invention relates to the technical field of fragrances, in particular to averman ester and a preparation method thereof. Background technique [0002] Averman ester is a mixture of 1-(3,3-dimethylcyclohexyl)ethanolformate and 3,3,7-trimethylcycloheptanol formate, which is a synthetic fragrance and is usually used Dihydromyrcene and formic acid are obtained through cyclization and hydration under the action of a catalyst. The catalyst is generally selected from sulfuric acid, phosphoric acid, ion exchange resin, ion membrane, molecular sieve, chloroacetic acid, etc. Among them, the catalytic performance of sulfuric acid is better, and the selectivity and conversion rate of the cyclization reaction are high, but the aroma of the product is not pure; the catalytic isomerization performance of molecular sieve and phosphoric acid is strong, and the selectivity of the cyclization reaction is poor; The catalytic efficiency of the ion exchange resin is l...
Claims
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