A kind of preparation method of high-efficiency retroester pentavalent antimony compound
A pentavalent antimony compound technology, which is applied in the field of preparation of high-efficiency reverse ester pentavalent antimony compounds, to achieve bright colors, reliable and stable products, and transparent products
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[0010] A method for preparing high-efficiency reverse ester pentavalent antimony compound includes the following steps:
[0011] (1) Preparation of reverse ester: Add isooctanoic acid, mercaptoethanol and acid catalyst into a glass-lined reactor at a mass ratio of 1:0.3-0.68:0.0005-0.0015 at the same time. Steam is introduced at a low temperature of 45 Turn on the vacuum pump at -75℃, observe the reaction water flowing out, increase the temperature to 80-90℃ and keep it for 1-4h, continue heating to 100-120℃ and keep it for 1-4h, until the weight of the condensed water reaches the theoretically calculated amount of reaction water Finish the reaction and cool to obtain mercaptoethanol isooctanoate, then transfer the mercaptoethanol isooctanoate to the rectification kettle, rectify the second stage to become the distilled product mercaptoethanol isooctanoate (reverse ester) for use, rectify the second stage The condition is that under vacuum conditions, the temperature is increased...
Embodiment 1
[0020] (1) Preparation of reverse ester: Add 1500 kg of isooctanoic acid and 800 kg of mercaptoethanol into a 2000 glass-lined reactor at the same time, add 1.5 kg of concentrated sulfuric acid, close the feeding port, increase the temperature, and open the agitator at the same time. Fill in the steam, turn on the vacuum pump at 55°C, observe the reaction water flowing out, then raise the temperature to 90°C for 1 hour, then to 100°C for another 3 hours, then measure the weight of the condensation reaction effluent, if it reaches the theoretical output At the end of the reaction, the temperature will be lowered, and it will be pumped into another 3000 rectification reactor to rectify, that is, the temperature will be increased, and the vacuum pump will be turned on at the same time. After the distillation is completed, it becomes the distilled product mercaptoethanol isooctanoate for use.
[0021] (2) Preparation of reverse ester pentavalent antimony: slowly add 350 kilograms of ...
Embodiment 2
[0023] (1) Preparation of reverse ester: Add 1,400 kg of isooctanoic acid and 760 kg of mercaptoethanol into a 2000 glass-lined reactor at the same time, add 1 kg of concentrated sulfuric acid, close the feeding port, increase the temperature, and open the agitator at the same time. Fill in the steam, turn on the vacuum pump at 65℃, observe the reaction water flowing out, then raise the temperature to 80℃ and keep it for 2h, then heat it to 110℃ and keep it for 2h, then measure the weight of the condensation reaction water, if it reaches the theoretical water output At the end of the reaction, the temperature will be lowered, and it will be pumped into another 3000 rectification reactor to rectify, that is, the temperature will be increased, and the vacuum pump will be turned on at the same time. After the distillation is completed, it becomes the distilled product mercaptoethanol isooctanoate for use.
[0024] (2) Preparation of reverse ester pentavalent antimony: slowly add 330...
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