Study On The Synthesis Of AcetylTri-n-ButylCitrate And Pilot Design

AcetylTri-n-ButylCitrate is one kind of outward appearance colorless transparent liquid. It is be internationally recognized as an non-toxic plasticizer at present, In opposite to the traditional phthalic acid ester plasticizer it is green environmental protection merit in professions and so on be widely applied in medicine health, food packing, child toy, having the broad prospects for development. Take the citric acid as raw material, through the esterification and the acylation responded that synthesizes ATBC is the general synthetic method. The key lies in selects the appropriate catalyst to guarantee the product's purity and luster, and reduction production cost as far as possible. This article studies' innovation lies in take the solid acidify as the esterification reaction's catalyst, take NaHSO₄ as the acylation reaction's catalyst, finally obtained the product purity is not only high, moreover solved the formerly question that decolorized difficultly. The catalyst easy to separate, the redundant use is simple, and the stability is good. In obtained each technological parameter under the condition to carry on the experimental line design.First, this article introduced in the plasticizer's application and the present world's production and the demand status, then had carried on the narration to the new non-toxic plasticizer ATBC's nature research and the production status of domestic and foreign. From this may see, ATBC compares the similar products to have the obvious superiority, the development potential is big, especially in domestic, designs a reasonable industry production line to have the very realistic significance.Second, uses the sol-gel law load phosphorus tungsten to prepare the most effective solidification acid catalyst to use in the esterification response. The findings indicated that the solidification acid catalysis' effect factor to be many. In the fixed phospho-wolframic acid solution and under the hydrochloric acid density condition, explored each kind of factor take the esterification rate as the target to solidify the acid catalysis effect the influence, obtained the ideal catalyst. By 2 g phospho-wolframic acid idea, dissolves with 3 ml distilled water, joins the catalyst activeness which 1 mol/l the hydrochloric acid 3 ml systems result to be the best. Under the same esterification condition obtains, the solid acidify's activation temperature should in 110℃-200℃, the best capacity be 10%. Under the above condition the catalyst esterification rate is high, repeatedly used 7 still had the suitable activeness from now on.Third, in had determined in each step response catalyst's foundation, studies the ATBC synthesis craft route with the orthogonal tests method, and determines the pilot experimental technological parameter through the confirmation experiment, the optimum esterification conditions were determind as follows:molar ration of citric acid to butyl alcohol is 1:4,the mass of catalyst is 3%(based on citric acid),solid quantity is 1/10,reaction time is 4 hours. Mid-product purity is high, the luster is good. Select NaSO₄ as the acylation reaction catalyst. After the reaction fluid's temperature decreased, the catalyst can be separated by the solid state, the response condition be temperate. The technological conditions are: The batch feeding ration (TBC and acid anhydride mole of ratio) 1:1.5, the catalyst amount used 5%, the reaction temperature 70℃, the reaction time is 60min. After reduced pressure distillation recycling acid anhydride, again menses and soda lye wash, after two reduced pressure distillation, the obtained product index of refraction is 1.4429, the purity reaches 99.2%, has achieved the quality requirement.Fourth, obtains the technological conditions through the above experiment, carried on the yearly produced 60 ton ATBC experimental lines' design, and carried on the computation to the material and the quantity of heat. This experimental line production method is the batch operation, the construction cost is low, the simplify operation, Hopefully to realize the industrialization.