Preparation method of methyl dihydrojasmonate

Abstract

The invention belongs to the technical field of preparation of methyl dihydrojasmonate, and particularly relates to a preparation method of methyl dihydrojasmonate, which comprises the following steps: mixing 2-cyclopentylcyclopentanone, eugenol, monopotassium phosphate, sodium hexametaphosphate, sodium hyaluronate and tetrabutylammonium perchlorate, and stirring for 10-15 minutes at 300-800r / min to obtain a mixture A; adding the mixture A into a tank body B, and storing at the temperature of 60 DEG C; and adding the catalyst into the tank body A, and storing at the temperature of 60-80 DEG C. When the methyl dihydrojasmonate is prepared, the purity of the methyl dihydrojasmonate is improved by adopting a method of wrapping atomized water vapor with gas, so that the perfume prepared by adopting the methyl dihydrojasmonate prepared by the invention can prolong the residence time of fragrance and the lasting time of skin moistening and improve the skin moistening effect, and when the perfume is used by men, after the men sweat after exercise, the perspiration does not occur. The fragrance retention time, the skin moistening duration and the skin moistening effect are still excellent.

Description

Technical Field

[0001] The invention belongs to the technical field of synthetic fragrances, and particularly relates to a method for preparing methyl dihydrojasmonate. Background Art

[0002] Methyl dihydrojasmonate is a colorless or light yellow transparent liquid, generally used in the formulation of perfumes. Men's perfumes have been quite popular in recent years. The formulation of men's perfumes takes into account that the perfume can still work after exercise and can effectively cover the body odor of sweat after exercise for a long time to increase male charm. Summary of the invention

[0003] The object of the present invention is to provide a method for preparing methyl dihydrojasmonate to solve the defects pointed out in the above background technology.

[0004] The technical solution of the present invention is:

[0005] A method for preparing methyl dihydrojasmonate comprises the following steps:

[0006] Step S1, mixing 2-cyclopentylcyclopentanone, eugenol, potassium dihydrogen phosphate, sodium hexametaphosphate, sodium hyaluronate and tetrabutylammonium perchlorate, and stirring at 300-800 r / min for 10-15 min to obtain a mixture A;

[0007] Step S2, adding the mixture A into the tank B and storing it at 60°C;

[0008] Step S3, adding the catalyst into tank A and storing it at a temperature of 60-80° C.;

[0009] Step S4, adding the gaseous agent into the tank body C, continuously inputting nitrogen into the tank body C by using an air pump, so that the nitrogen carries the gaseous agent into the tank body A, and then using an atomizer to atomize the mixture A in the tank body B, and under the driving action of the gas, the mixture enters the tank body B, passes through the mixture A, and is discharged through the top opening of the tank body B to obtain the mixture B;

[0010] Step S5, adding mixture B into an electrolytic cell to generate methyl dihydrojasmonate through electrolysis reaction.

[0011] As a further optimization scheme of the present invention, the raw materials for preparing the methyl dihydrojasmonate include, by weight: 5-10 parts of 2-cyclopentylcyclopentanone, 3-6 parts of eugenol, 2-5 parts of potassium dihydrogen phosphate, 15-20 parts of sodium hexametaphosphate, 30-35 parts of sodium hyaluronate, 8-16 parts of tetrabutylammonium perchlorate, 45-50 parts of catalyst, and 50-55 parts of gas agent.

[0012] As a further optimization scheme of the present invention, the preparation process of the catalyst is as follows: (1) mixing bamboo charcoal powder and rare earth, then adding pure water and stirring until completely mixed, and obtaining a basic solution by leaching; (2) mixing dimethyl succinate, tea polyphenols, ethanol and 35% hydrogen peroxide aqueous solution, and storing them at 80-120°C for 28-32 hours to obtain an additive solution; (iii) adding the additive solution to the basic solution, stirring at 60-75r / min for 16-20 hours to obtain a catalyst.

[0013] As a further optimization scheme of the present invention, the raw materials for preparing the catalyst include, by weight: 10-12 parts of dimethyl succinate, 6-10 parts of tea polyphenols, 16-23 parts of ethanol, 35-40 parts of 35% hydrogen peroxide aqueous solution, 60-70 parts of pure water, 4-8 parts of bamboo charcoal powder and 0.5-1.2 parts of rare earth.

[0014] As a further optimization scheme of the present invention, the preparation process of the gas agent is: helium and ozone are filled into the tank C, and oxygen is filled after standing for 20 minutes to obtain the gas agent.

[0015] As a further optimization scheme of the present invention, the raw materials for preparing the gas agent include, by weight: 30-45 parts of oxygen, 0.8-1.5 parts of helium and 15-20 parts of ozone.

[0016] As a further optimization scheme of the present invention, the nitrogen is continuously input for 20-30 minutes at a flow rate of 2-5 (m / s).

[0017] The above-mentioned methyl dihydrojasmonate is prepared by the above-mentioned preparation method of methyl dihydrojasmonate.

[0018] Compared with the prior art, the present invention has the following beneficial effects:

[0019] The method of using gas to entrain atomized water vapor during the preparation of methyl dihydrojasmonate is used to improve the purity of methyl dihydrojasmonate. Meanwhile, helium, ozone and nitrogen have a synergistic effect on each other, thereby achieving a good effect of improving the performance of perfume. Thus, the perfume prepared by using the methyl dihydrojasmonate prepared by the present invention can prolong the retention time of fragrance and the duration of skin moisturizing, thereby improving the skin moisturizing effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 It is a process flow chart of the present invention. DETAILED DESCRIPTION

[0021] The present invention is further described in detail below. It is necessary to point out that the following specific implementation methods are only used to further illustrate the present invention and cannot be understood as limiting the scope of protection of the present invention. Technicians in this field can make some non-essential improvements and adjustments to the present invention based on the above application content.

[0022] Unless otherwise specified, the methods used in the present invention are conventional methods known to those skilled in the art, and the reagents and other materials used are commercially available products unless otherwise specified.

[0023] Effect of a Catalyst on the Properties of Methyl Dihydrojasmonate

[0024] (1) The preparation method of methyl dihydrojasmonate is as follows:

[0025] 8 parts of 2-cyclopentylcyclopentanone, 4 parts of eugenol, 3 parts of potassium dihydrogen phosphate, 17 parts of sodium hexametaphosphate, 32 parts of sodium hyaluronate and 12 parts of tetrabutylammonium perchlorate were mixed, and stirred at 500 r / min for 12 min to obtain a mixture A;

[0026] Add mixture A into tank B and store it at 60°C;

[0027] 48 parts of catalyst were added into tank A and stored at 70°C;

[0028] 53 parts of gas agent are added into tank body C, and nitrogen is continuously input into tank body C by using an air pump (nitrogen is continuously input for 25 minutes at a flow rate of 3 (m / s)), so that the nitrogen carries the gas agent into tank body A, and then the mixture A in tank body B is atomized by using an atomizer, and enters tank body B under the driving action of the gas, passes through the mixture A, and is discharged through the top opening of tank body B to obtain mixture B;

[0029] Adding mixture B into an electrolytic cell to generate methyl dihydrojasmonate through electrolysis reaction;

[0030] The preparation process of the catalyst is as follows: (1) mixing bamboo charcoal powder and rare earth, then adding pure water and stirring until completely mixed, and obtaining a basic solution by leaching; (2) mixing dimethyl succinate, tea polyphenols, ethanol and 35% hydrogen peroxide aqueous solution, and storing them at 100° C. for 30 hours to obtain an additive solution; (3) adding the additive solution to the basic solution, stirring at 65 r / min for 18 hours, and obtaining a catalyst;

[0031] The preparation process of the gas agent is as follows: helium and ozone are filled into a tank C, and after standing for 20 minutes, oxygen is filled in to obtain the gas agent.

[0032] The raw materials for preparing the gas agent include: 38 parts of oxygen, 1.2 parts of helium and 18 parts of ozone;

[0033] The raw material composition of the catalyst is shown in Table 1:

[0034] Table 1

[0035]

[0036] Note: “-” means no addition

[0037] (2) The performance of the above-mentioned methyl dihydrojasmonate sample was tested using the following test method

[0038] Perfume preparation process: 30% ethanol, 12% propylene glycol, 15% salicylates, 5% methrin, 10% glycerol and 28% methyl dihydrojasmonate are mixed, blended, aged, filtered and filled to obtain the finished perfume.

[0039] The methyl dihydrojasmonate prepared in Examples 1 to 3 and Comparative Examples 1 and 2 was used to prepare perfumes. 50 young male volunteers with the same skin quality and age were divided into 5 groups. Two pumps of perfume were sprayed on the back of their hands respectively, and then the effect of the perfume was tested. The results are shown in Table 2:

[0040] Table 2

[0041]

[0042] From the data in Table 2, it can be seen that the perfume prepared by methyl dihydrojasmonate prepared in Examples 1 to 3 has the longest fragrance retention time and skin moisturizing duration, and the best skin moisturizing effect performance;

[0043] By comparing Comparative Examples 1 and 2 with Example 2, it can be seen that the bamboo charcoal powder and rare earth respectively lacking in Comparative Examples 1 and 2 can synergize with each other to prolong the retention time of the perfume, the duration of the moisturizing effect, and improve the moisturizing effect.

[0044] Effects of two-gas agent on the properties of methyl dihydrojasmonate

[0045] (1) Preparation method of methyl dihydrojasmonate: Step reference 1 (1), wherein the gas agent in Table 3 is used to replace the gas agent in Example 2.

[0046] The raw material composition of the gas agent is shown in Table 3:

[0047] Table 3

[0048]

[0049] Note: “-” means no addition

[0050] (2) The performance of the above-mentioned methyl dihydrojasmonate sample was tested using the following test method

[0051] The methyl dihydrojasmonate prepared in Examples 2 and 3 and Comparative Examples 3 and 4 was used to prepare perfume (the perfume preparation method is detailed in Part 1 (2)). 50 young male volunteers with the same skin quality and age were divided into 5 groups. Two pumps of perfume were sprayed on the back of their hands respectively. They were then tested for the effect of the perfume in an outdoor environment at 30°C for 1000 meters. The results are shown in Table 4:

[0052] Table 4

[0053]

[0054] It can be seen from the data in Table 4 that after a 1000-meter long-distance run, the fragrance retention time and skin moisturizing duration of the perfume are shortened, and the skin moisturizing effect is weakened. The fragrance retention time of the perfume prepared by methyl dihydrojasmonate prepared in Example 2 is not as long as that of the perfume prepared by methyl dihydrojasmonate prepared in Example 3. Therefore, the perfume prepared by methyl dihydrojasmonate prepared in Example 3 has the best performance;

[0055] By comparing Example 3 with Comparative Examples 3 and 4, it can be seen that the difference between Example 3 and Comparative Examples 3 and 4 is that Comparative Example 3 does not add helium, and Comparative Example 4 does not add ozone, resulting in poor effects of Comparative Examples 3 and 4. Therefore, it can be seen that helium, ozone and nitrogen work synergistically with each other to achieve a good effect of improving the performance of perfume.

[0056] The above-mentioned embodiments only express several implementation methods of the present invention, and the description thereof is relatively specific and detailed, but it cannot be understood as limiting the scope of the present invention. It should be pointed out that for ordinary technicians in this field, several variations and improvements can be made without departing from the concept of the present invention, which all belong to the protection scope of the present invention.

Claims

1. A method for preparing methyl dihydrojasmonate, characterized in that: The following steps are involved: Step S1, mixing 2-cyclopentylcyclopentanone, eugenol, potassium dihydrogen phosphate, sodium hexametaphosphate, sodium hyaluronate and tetrabutylammonium perchlorate, and stirring at 300-800 r / min for 10-15 min to obtain a mixture A; Step S2, adding the mixture A into the tank B and storing it at 60°C; Step S3, adding the catalyst into tank A and storing it at a temperature of 60-80° C.; Step S4, adding the gaseous agent into the tank body C, continuously inputting nitrogen into the tank body C by using an air pump, so that the nitrogen carries the gaseous agent into the tank body A, and then using an atomizer to atomize the mixture A in the tank body B, and under the driving action of the gas, the mixture enters the tank body B, passes through the mixture A, and is discharged through the top opening of the tank body B to obtain the mixture B; Step S5, adding mixture B into an electrolytic cell to generate methyl dihydrojasmonate through electrolysis reaction.

2. The method for preparing methyl dihydrojasmonate according to claim 1, characterized in that: The raw materials for preparing the methyl dihydrojasmonate include, by weight: 5-10 parts of 2-cyclopentylcyclopentanone, 3-6 parts of eugenol, 2-5 parts of potassium dihydrogen phosphate, 15-20 parts of sodium hexametaphosphate, 30-35 parts of sodium hyaluronate, 8-16 parts of tetrabutylammonium perchlorate, 45-50 parts of catalyst, and 50-55 parts of gas agent.

3. The method for preparing methyl dihydrojasmonate according to claim 1, characterized in that: The preparation process of the catalyst is as follows: (1) mixing bamboo charcoal powder and rare earth, then adding pure water and stirring until completely mixed, and obtaining a basic solution by leaching; (2) mixing dimethyl succinate, tea polyphenols, ethanol and 35% hydrogen peroxide aqueous solution, and storing them at 80-120° C. for 28-32 hours to obtain an additive solution; (3) adding the additive solution to the basic solution, stirring at 60-75 r / min for 16-20 hours to obtain a catalyst.

4. The method for preparing methyl dihydrojasmonate according to claim 3, characterized in that: The raw materials for preparing the catalyst include, by weight: 10-12 parts of dimethyl succinate, 6-10 parts of tea polyphenols, 16-23 parts of ethanol, 35-40 parts of 35% hydrogen peroxide aqueous solution, 60-70 parts of pure water, 4-8 parts of bamboo charcoal powder and 0.5-1.2 parts of rare earth.

5. The method for preparing methyl dihydrojasmonate according to claim 1, characterized in that: The preparation process of the gas agent is as follows: helium and ozone are charged into a tank body C, and after standing for 20 minutes, oxygen is charged to obtain the gas agent.

6. The method for preparing methyl dihydrojasmonate according to claim 5, characterized in that: In parts by weight, the raw materials for preparing the gas agent include: 30-45 parts of oxygen, 0.8-1.5 parts of helium and 15-20 parts of ozone.

7. The method for preparing methyl dihydrojasmonate according to claim 1, characterized in that: The nitrogen is continuously input at a flow rate of 2-5 (m / s) for 20-30 min.

8. A methyl dihydrojasmonate, characterized in that The methyl dihydrojasmonate is prepared by the preparation method of methyl dihydrojasmonate according to any one of claims 1 to 7.

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