Pentenoic acid methylester preparation process
A technology for the preparation of methyl pyretinate, which is applied in the technical field of preparing methyl pyretinate by a method, which can solve the problem of low content and excess of the product methyl pyretinate, and the inability to obtain high-quality methyl pyretinate, etc. question
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Embodiment 1
[0010] Put 5,060 kg (42 kilomoles) of trimethyl orthoacetate with a content of 99.6% in a 10,000-liter pressure reactor with a rectification tower, and raise the temperature to 150-155°C (the reaction pressure can be adjusted by pressing nitrogen or a pressure relief valve ), first add propionic acid (total 74 kg, 1 kilomole) catalyst through injection metering pump at 7.4 kg / hour for a total of 10 hours; after adding catalyst for 1 hour, add 98% content, moisture≤ 0.1% isopentenol (3510 kilograms in total, 4 kilomoles) for 9 hours; as the reaction proceeds, methanol containing a small amount of trimethyl orthoacetate is separated from the top of the rectifying tower, and the reaction temperature is gradually increased to 180-190 °C, and keep warm at 175-185 °C until the prenol content in the pressure reactor is ≤0.5%, the reaction is over, and the reaction time is 13.5 hours. The reaction material was cooled to below 50°C, and the obtained reaction product was subjected to co...
Embodiment 2
[0012] Put 5,783 kg (48 thousand moles) of trimethyl orthoacetate with a content of 99.6% in a 10,000-liter pressure reactor with a rectification tower, and raise the temperature to 150-155 ° C (the reaction pressure can be adjusted by pressing nitrogen or a pressure relief valve ), first add propionic acid (total 74 kg, 1 kilomole) catalyst through injection metering pump at 7.4 kg / hour for a total of 10 hours; after adding catalyst for 1 hour, add 98% content, moisture≤ 0.1% isopentenol (3510 kilograms in total, 4 kilomoles) for 9 hours; as the reaction progresses, methanol containing a small amount of trimethyl orthoacetate is separated from the top of the rectifying tower, and the reaction temperature is gradually increased to 175-180 °C, and keep warm at 175-180 °C until the prenol content in the pressure reactor is ≤0.5%, the reaction is over, and the reaction time is 12 hours. Cool the reaction material to below 50°C, and the obtained reaction product is subjected ...
Embodiment 3
[0014] Put 5,783 kg (48 thousand moles) of trimethyl orthoacetate with a content of 99.6% in a 10,000-liter pressure reactor with a rectification tower and trimethyl orthoacetate made from methyl triethyl ammonium chloride and anhydrous aluminum trichloride 50kg of ionic liquid catalyst, heated up to 150-155°C (the reaction pressure can be adjusted by pressing in nitrogen or a pressure relief valve), through the injection metering pump, add 98% content, moisture ≤0.1% isoamyl at a feeding speed of 390 kg / hour Enol (3510 kg in total, 4 thousand moles) for 9 hours; as the reaction progressed, methanol containing a small amount of trimethyl orthoacetate was separated from the top of the rectifying tower, and the reaction temperature was gradually increased to 170-175 ° C, and 170-175°C heat preservation reaction until the prenol content in the pressure reactor is ≤0.5%, the reaction is over, and the reaction time is 12 hours. Cool the reaction material to below 50°C, and the...
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