A kind of polyglycerol fatty acid ester and preparation method thereof
A technology of fatty acid ester and polyglycerol, which is applied in the field of polymers, can solve the problems of difficult separation of catalyst and product, poor quality of polyglycerol, and low yield of polyglycerol, and achieve the effects of enhanced reaction activity, increased content, and high catalytic activity
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[0029] A kind of preparation method of polyglycerol fatty acid ester of the present invention, comprises the following steps:
[0030] (1) Under the condition of vacuum degree of 0.05-0.1MPa, add glycerin while stirring, after heating to 60-80°C, add 0.1-0.5wt% solid strong acid catalyst, continue to heat up to 100-120°C, heat preservation reaction 2 ~5h, filtered to obtain the mixed polyglycerol;
[0031] (2) carrying out short-range molecular distillation and purification of the mixed polyglycerol to obtain polyglycerol;
[0032] (3) Add polyglycerin with a molar ratio of (1.1-1.3): 1 to the liquid fatty acid while stirring, then add a mixed catalyst of 0.2-1% of the fatty acid weight, heat up to 210-230°C, and vacuum at 0.08-0.1 MPa, reacting for 1.5-2.5 hours, the polyglycerin fatty acid ester can be prepared.
[0033]In the present invention, glycerin is preliminarily preheated at 60-80°C under pressure conditions, and then dehydration polymerization is carried out at 1...
Embodiment 1
[0064] The preparation method of the polyglycerol fatty acid ester of the present embodiment may further comprise the steps:
[0065] (1) Under the condition of vacuum degree of 0.05MPa, add glycerin while stirring, after heating to 60°C, add 0.1wt% solid strong acid catalyst, continue to heat up to 100°C, keep warm for 2 hours, and filter to obtain the mixed polyglycerin.
[0066] Wherein, the preparation method of solid strong acid catalyst comprises the following steps:
[0067] (i) Sodium lignosulfonate and diatomaceous earth were dissolved in acetic acid solution at a mass ratio of 10:1 to prepare a 1wt% solution, then added dropwise to a 10wt% sodium hydroxide solution, stirred and filtered to obtain beads ;
[0068] (ii) Add the beads into the soaking solution with a concentration of 1wt% to soak, and fully absorb at 30°C, filter and add to epichlorohydrin, then add potassium persulfate, and react at 50°C for 3h to prepare Obtain solid strong acid catalyst;
[0069] W...
Embodiment 2
[0076] The preparation method of the polyglycerol fatty acid ester of the present embodiment may further comprise the steps:
[0077] (1) Under the condition of a vacuum of 0.07MPa, add glycerin while stirring, after heating to 70°C, add 0.3wt% solid strong acid catalyst, continue to heat up to 110°C, keep warm for 3 hours, and filter to obtain the mixed polyglycerin.
[0078] Wherein, the preparation method of solid strong acid catalyst comprises the following steps:
[0079] (i) Sodium lignosulfonate and diatomaceous earth were dissolved in acetic acid solution at a mass ratio of 20:1 to prepare a 5wt% solution, then added dropwise to a 15wt% sodium hydroxide solution, stirred and filtered to obtain beads ;
[0080] (ii) Add the beads into the soaking solution with a concentration of 5wt% to soak, and fully absorb at 40°C, filter and add to epichlorohydrin, then add potassium persulfate, and react at 60°C for 4h to prepare Obtain solid strong acid catalyst;
[0081] Wher...
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Abstract
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