Octadecanoyl tributyl citrate plasticizer and preparation thereof
Inactive Publication Date: 2008-09-03
LANZHOU UNIVERSITY OF TECHNOLOGY
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[0008] However, the current citric acid ester products generally have the disadvantages of thermal stability, low temperature flexibility, solvent extraction resistance and migration resistance in actual use, which limits the scope of use of the existing citric acid ester plasticizers.
The main reason for the ubiquitous application of existing citrate plasticizers is that the relative molecular weight of the plasticizer is small, the ratio of the number of nonpolar aliphatic carbon atoms to the number of polar groups (A p / P o )improper
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[0044] The preparation method of tributyl octadecanoyl citrate plasticizer, according to the above-mentioned formula batching, its step is:
[0045] (1) Synthesis of tributyl citrate: add citric acid, n-butanol, water-carrying agent and catalyst in the reaction kettle, heat up to reflux under stirring, react to anhydrous generation, distill and recover excess butanol to obtain citric acid tributyl ester;
[0046] (2) Synthesis of octadecanoyl chloride: Add stearic acid in the reaction kettle, add phosphorus trichloride dropwise when stirring and raising the temperature to 50°C, drop it in about 1 hour, heat up to 75°C for heat preservation reaction, and last for 3 hours , then cooled to room temperature, static layering to obtain octadecanoyl chloride;
[0047] (3) Synthesis of octadecanoyl tributyl citrate: Add tributyl citrate and catalyst in the reaction kettle, stir and heat up to 70°C, add octadecanoyl chloride dropwise, and the generated hydrogen chloride is passed thro...
Embodiment 1
[0049] (1) Synthesis of tributyl citrate: Add 22kg of citric acid, 38.5kg of n-butanol, 39kg of toluene and 0.5kg of catalyst into the reactor, start stirring, heat up to reflux, keep warm and reflux until anhydrous to form , open the vacuum system, distill under reduced pressure to remove excess n-butanol, toluene and water, cool down and discharge the material when there is no distilled component, and obtain tributyl citrate. The n-butanol obtained by distillation is recycled.
[0050] (2) Synthesis of octadecanoyl chloride: Accurately weigh 80.5kg of stearic acid and add it to the reaction kettle, stir and heat up to 50°C, add 19.5kg of phosphorus trichloride dropwise, drop it within 1 hour, and heat up to 75°C Insulate the reaction for 3 hours, then cool to room temperature, and statically separate to obtain octadecanoyl chloride.
[0051] (3) Synthesis of octadecanoyl tributyl citrate
[0052]Accurately weigh 43.5kg of tributyl citrate, add 1.5kg of catalyst into the re...
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Abstract
The invention provides octade carbonyl tributyl citrate plasticizer and preparation method thereof. The composition of octade carbonyl tributyl citrate plasticizer (in mass percent): tributyl citrate 43.5-53.8%, octade carbonyl chloride 45.2-55.0%, catalyst 1.0-1.5%. The preparation method comprises: (1) adding citric acid, butylalcohol, water-carrying agent and catalyst into reaction kettle, stirring, heating up until reflowing to obtain tributyl citrate; (2) adding stearic acid into reaction kettle, stirring, heating up to 50 degree and then adding phosphorous trichloride and heating up to 75 degree to perform thermal insulating reaction for 3 hours and layering to obtain octade carbonyl chloride; (3) adding tributyl citrate and catalyst in the reaction kettle, stirring, heating up to 70 degree and then adding octade carbonyl chloride to obtain chlorine hydride and the chlorine hydride being absorbed in water containing soda in drier, when the pH of the water containing soda is constant, the reaction being stopped and the product being subjected to neutralizing, cleaning, pump filtering under reduced pressure to obtain octade carbonyl tributyl citrate.
Description
technical field [0001] The present invention relates to a kind of preparation method of plasticizer, especially the technological method of octadecyl tributyl citrate. Background technique [0002] Although the carcinogenicity of traditional plasticizers phthalates is still inconclusive, due to their potential dangers, Western Europe, North America, Japan and other developed countries are very cautious about the use of phthalates. attitude, and put forward stricter requirements and restrictions, such as stopping the industrial production of new phthalate plasticizers, in food packaging, children's toys, medical equipment and other fields with high hygienic requirements August 2003 The use of bis(2-ethylhexyl) phthalate (DOP) will be banned from 1st. [0003] Citrate plasticizer is a promising non-toxic accelerator. Compared with the traditional "standard plasticizer" DOP, it has good resin compatibility, high plasticizing efficiency, low volatility, and cold resistance. Li...
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