A kind of betaine salicylic acid co-crystal and preparation method and application thereof
A technology of salicylic acid and betaine, which is applied in the field of cosmetics and medicine, can solve skin and eye irritation problems, achieve the effects of reducing allergies, adjustable particle size, and reducing irritation
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[0034] The preparation method of a betaine salicylic acid co-crystal provided by the invention comprises the following steps:
[0035] S1 adds solvent, betaine, salicylic acid in the autoclave, adds solvent and betaine and salicylic acid in the autoclave, stirs under the first pressure and the first temperature, forms the suspension of betaine and salicylic acid liquid.
[0036] Specifically, the solvent can be liquid CO 2 , petroleum ether and ethyl acetate. Among them, liquid CO is preferred 2 , liquid CO 2 It is non-toxic, non-flammable and affordable. The molar ratio of betaine to salicylic acid is 1:1, and the solid-liquid ratio of the sum of betaine+salicylic acid to solvent is 1:4-1:6 (kg:L). The autoclave refers to a reactor operated under high pressure. The pressure of the autoclave is set to 10-30MPa, preferably 20MPa; the temperature is set to 110-130°C, preferably 115°C; the stirring speed is 600-750r / min, preferably is 700r / min; the stirring time is 1-8h, pr...
Embodiment 1
[0045] A preparation method of betaine salicylic acid co-crystal:
[0046] S1 adds liquid CO to the autoclave 2 , betaine, salicylic acid, wherein the molar ratio of betaine and salicylic acid is 1:1, and the sum of betaine+salicylic acid and the solid-liquid ratio of solvent are 1:5 (kg:L). The pressure of the autoclave was set to 20MPa, the temperature was set to 115°C, the stirring speed was 700r / min, and stirred for 4h to form a suspension of betaine and salicylic acid;
[0047] S2 pumps the suspension to the high-pressure homogenizer by the high-pressure pump, passes through the homogenizing valve, and the pressure of the homogenizing valve is set to 800bar;
[0048] S3 decompresses the receiving chamber of the homogenizer to normal pressure at normal temperature to make the liquid CO 2 Volatile to obtain betaine salicylic acid co-crystal.
[0049] The molecular structure of betaine-salicylic acid co-crystal is as follows figure 1 shown, the molecular formula is C 12...
Embodiment 2
[0197] The difference from Example 1 is that the pressure of the homogenization valve in S2 is set to 600 bar. The single crystal data and hydrogen spectrum data of the betaine-salicylic acid co-crystal tested were the same as in Example 1, and the purity was over 98%.
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