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A technology of zinc glycerol and glycerol, which is applied in the field of zinc glycerol preparation, can solve the problems of difficult phase separation and separation of zinc glycerol and glycerin, the loss of glycerin and washing solvent, and the cost of zinc acetate is relatively expensive, so as to achieve easy control, low requirements and low conditions mild effect
Active Publication Date: 2016-08-31
INST OF RESOURCES UTILIZATION & RARE EARTH DEV GUANGDONG ACAD OF SCI
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Problems solved by technology
According to the different zinc sources, the reaction difficulty and reaction conditions are different: if zinc acetate is used as the zinc source, the reaction with glycerol is easier to proceed without a catalyst, and it can be directly reacted at 110~160°C to form glycerol zinc, but due to The cost of zinc acetate is relatively expensive, and the reaction produces strongly irritating and corrosive acetic acid, which is rarely used in production; if zinc oxide, zinc carbonate, zinc hydroxide and other inorganic zinc sources are used, catalysis, high temperature, pressure, and microwave are generally required. Reaction and other harsh conditions
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Embodiment 1
[0020] Add 30g of zinc oxide, 1.5g of zinc formate, and 200g of methylcyclohexane into a 1000mL three-necked flask equipped with a stirrer, a thermometer, a reflux condenser, and a water separator, stir for 5 minutes, add 0.6g of glyceryl monostearate, and continue Stir for 5 minutes, then add 40.88g of glycerin, and heat up to 110°C under stirring. As the reaction progresses, the amount of water collected on the water separator gradually increases until the amount of water does not increase after 3 hours of reaction. Cool, filter with isopropyl Washed twice with alcohol and dried to obtain 57.20 g of white powdery zinc glycerol solid. After calculation, the yield relative to zinc oxide is 99.4%, and the zinc content is 42.25%.
Embodiment 2
[0022] Add 46g of zinc carbonate, 4g of acrylic acid, and 180g of n-propyl acetate into a 500mL three-necked flask equipped with a stirrer, thermometer, reflux condenser, and water separator. After stirring for 30 minutes, add 0.5g of Span-60, continue stirring for 10 minutes, and then add 35g of Glycerin was heated to 103°C under stirring, reacted for 4 hours, cooled, filtered with suction, washed twice with ethanol, and dried to obtain 55.86 g of white powdery zinc glycerol solid. After calculation, the yield relative to zinc oxide is 96.65%, and the zinc content is 42.81%.
Embodiment 3
[0024] Add 30g of zinc oxide, 3g of acetic acid, and 180g of toluene into a 500mL three-necked flask equipped with a stirrer, thermometer, reflux condenser, and water separator. After stirring for 30 minutes, add 0.3g of Span-80, continue stirring for 5 minutes, and then add 35.28g of glycerol. The temperature was raised to 112°C under stirring, reacted for 2.5 hours, cooled, filtered with suction, washed once with methanol, and dried to obtain 56.66 g of white powdery zinc glycerol solid. After calculation, the yield relative to zinc oxide is 99.05%, and the zinc content is 42.30%.
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Abstract
The invention relates to a preparation method of glyzinc, and belongs to the field of chemical synthesis. The preparation method comprises the following steps of adding a zinc source, a catalyst and an aprotic solvent into a reactor according to a mass ratio being 1:(0.05 to 0.15): (2 to 10); performing stirring for 5 to 30min; then, adding dispersing agents accounting for 0.3 to 3 percent of the mass of the zinc source; performing stirring for 5 to 10 min so that the zinc source and the catalyst are uniformly dispersed in a solvent; then, adding glycerol (the mol ratio of the glycerol to the zinc source is (1 to 1.2):1); raising the temperature to 100 to 150 DEG C under the stirring condition; taking a reaction for 2 to 4 hours; performing cooling and suction filtration; performing washing by C<1 to 3> monohydric alcohol, and then performing suction filtration and drying to obtain the glyzinc. The invention provides the preparation method with the advantages that the process is simple; the operation is convenient; the reaction conditions are mild; the temperature can be easily controlled. The glyzinc synthesis is performed in the aprotic solvents; through the addition of dispersing agents, reaction substances cannot agglomerate or deposit on the device wall; after the reaction, the filtering and the separation can be directly performed; the washing is easy.
Description
technical field [0001] The invention relates to a preparation method of zinc glycerol, which belongs to the field of chemical synthesis. Background technique [0002] Glycerol zinc (Zinc glycerolate, Glyzinc), also known as glycerol zinc complexes (Zinc glycerolate complexes), molecular formula (C 3 h 6 o 3 Zn) x , is a wide range of fine chemicals, with good barrier, anti-ultraviolet properties, non-toxic, non-coloring, can be used as plastic light stabilizer, heat stabilizer and rubber vulcanization activator. Zinc glycerol is often used as an important component of cosmetics, which plays the role of lubrication, anti-ultraviolet radiation, etc., and is also often used as a zinc supplement and a drug for treating skin diseases. At present, the preparation methods of zinc glycerol all adopt the direct reaction of zinc source and glycerin, and the amount of glycerol is generally 3-10 times of the mass of zinc source. According to the different zinc sources, the reaction...
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IPC IPC(8): C07C29/70C07C31/28
CPCC07C29/70C07C31/28
Inventor 孔振兴戴子林危青李桂英
Owner INST OF RESOURCES UTILIZATION & RARE EARTH DEV GUANGDONG ACAD OF SCI
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