Integrated process of synthesizing acetyl tributyl citrate by using activated carbon immobilized p-toluenesulfonic acid catalyst
A technology of acetyl tributyl citrate and tributyl citrate, which is applied in the field of synthesis of plasticizer acetyl tributyl citrate (ATBC), can solve the problems of long production cycle, large product loss, and environmental pollution. Achieve the effect of less three wastes, less equipment corrosion and high product quality
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Embodiment 1
[0031] An integrated method for the synthesis of acetyl tributyl citrate by activated carbon immobilized p-toluenesulfonic acid catalyst, comprising the following steps:
[0032] (1) Catalyst (TsOH / C) preparation
[0033] Weigh 1 kg of activated carbon for sugar liquid decolorization, soak it in 10 kg of p-toluenesulfonic acid solution with a mass concentration of 25%, stir it at room temperature for 20 hours, filter it after loading, and dry it at 90°C to constant weight to obtain the activated carbon. For the toluenesulfonic acid catalyst (TsOH / C), the mass ratio of p-toluenesulfonic acid in the catalyst calculated by the weight gain method is 35%.
[0034] (2) Preparation of tributyl citrate
[0035] Add 21.0kg (0.1kmol) of citric acid monohydrate, 31.9kg (0.43kmol) of n-butanol and 0.168kg of the above catalyst TsOH / C (monowater 0.8% of the mass of citric acid), stirred and reacted at 120°C for 4.0h, synthesized TBC, measured the acid value according to GB 1668-81, the e...
Embodiment 2
[0039] An integrated method for the synthesis of acetyl tributyl citrate by activated carbon immobilized p-toluenesulfonic acid catalyst, comprising the following steps:
[0040] (1) Catalyst (TsOH / C) preparation
[0041] Weigh 1 kg of activated carbon for decolorization of sugar liquid and soak it in 25 kg of p-toluenesulfonic acid solution with a mass concentration of 27%, stir and immobilize it at room temperature for 30 hours, filter it after immobilization, and dry it at 110°C to constant weight to obtain activated carbon immobilized p-toluene For the sulfonic acid catalyst (TsOH / C), the mass ratio of p-toluenesulfonic acid in the catalyst is calculated by the weight gain method to be 45%.
[0042] (2) Preparation of tributyl citrate
[0043] Add 21.0kg (0.1kmol) of citric acid monohydrate, 37.1kg (0.5kmol) of n-butanol and 0.105kg of the above catalyst TsOH / C (monowater 0.5% of the mass of citric acid), stirred and reacted at 140°C for 3.0h, synthesized TBC, measured t...
Embodiment 3
[0047] An integrated method for the synthesis of acetyl tributyl citrate by activated carbon immobilized p-toluenesulfonic acid catalyst, comprising the following steps:
[0048] (1) Catalyst (TsOH / C) preparation
[0049] Weigh 1 kg of activated carbon for sugar liquid decolorization and soak it in 40 kg of p-toluenesulfonic acid solution with a mass concentration of 30%, stir and immobilize it at room temperature for 40 hours, filter it after immobilization, and dry it at 100°C to constant weight to obtain activated carbon immobilized p-toluene For the sulfonic acid catalyst (TsOH / C), the mass ratio of p-toluenesulfonic acid in the catalyst is calculated by the weight gain method to be 55%.
[0050] (2) Preparation of tributyl citrate
[0051] Add 19.2kg (0.1kmol) of anhydrous citric acid, 33.4kg (0.45kmol) of n-butanol and 0.288kg (anhydrous 1.5% of the mass of citric acid), stirred and reacted at 110°C for 6.0h, synthesized TBC, measured the acid value according to GB 1668-...
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