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A technology of dihydroquinoline and trimethyl, applied in the direction of organic chemistry and the like, can solve the problems of reducing labor intensity and low productivity, and achieve the effects of reducing labor intensity, low production cost and labor cost.
Inactive Publication Date: 2016-02-24
CHINA PETROLEUM & CHEM CORP +1
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Problems solved by technology
And can significantly reduce labor intensity, save power and labor costs, and solve the problem of low productivity in existing technologies
Method used
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Embodiment 1
[0030] Add 1,000 grams of aniline into a tower reactor with a volume of 2,000 ml, raise the temperature to 120°C, and feed a mixture of aniline, industrial hydrochloric acid, and acetone with a molecular ratio of 5:2:40 from the feed port at the bottom of the reactor at a rate of 100 ml / h The speed is continuously passed into the reactor, during which the temperature of the reactor is kept at 120 ± 5 ° C. After 20 hours, the reaction liquid outlet is sampled and analyzed. The content of 2,2,4-trimethyl-1,2-dihydroquinoline is 33.74%.
Embodiment 2
[0032] Add 1,000 grams of aniline into a tower reactor with a volume of 2,000 ml, raise the temperature to 105°C, and from the feed port at the bottom of the reactor, according to the molecular ratio of aniline, industrial hydrochloric acid, and acetone: 6:1:30, at a speed of 80ml / h It was continuously fed into the reactor, during which the temperature of the reactor was kept at 110±5°C. After 24 hours, the reaction liquid outlet was sampled and analyzed. The content of 2,2,4-trimethyl-1,2-dihydroquinoline was 27.02 %.
Embodiment 3
[0034] Add 1,000 grams of aniline to a fixed-bed reactor with a volume of 2,000 ml, raise the temperature to 150° C., preheat the aniline to 100° C., and continuously feed it into the reactor at a rate of 92 ml / h from the feed port at the bottom of the reactor. Industrial hydrochloric acid and acetone are respectively Continuously feed into the reactor from the feed port at the bottom of the reactor at a rate of 10, 220ml / h, keep the temperature of the reactor at 150±5°C during the period, and take samples from the outlet of the reaction liquid for analysis after 20 hours, 2, 2, 4-three The content of methyl-1,2-dihydroquinoline is 25.10%.
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Abstract
The present invention belongs to the technical field of fine chemical industry, and relates to a method for continuously preparing an anti-aging agent RD monomer 2,2,4-trimethyl-1,2-dihydroquinoline. The method comprises: adding aniline to a reactor, heating to a temperature 80-160 DEG C, continuously introducing aniline, acetone and an acid catalyst into the reactor according to a molecular ratio of 1-10:5-100:1, maintaining the reaction temperature at 80-160 DEG C, and continuously extracting the condensation reaction liquid containing 2,2,4-trimethyl-1,2-dihydroquinoline from the material outlet on the upper portion of the reactor. According to the present invention, the continuous tower-type reactor is used to replace the intermittent kettle type reactor, the continuous operation can reduce the raw material consumption, substantially reduce the power cost, can significantly reduce the labor intensity, can solve the low productivity in the prior art, and can maintain the industrialized production stability and the product quality stability.
Description
technical field [0001] The invention belongs to the technical field of fine chemicals, relates to a method for continuously preparing 2,2,4-trimethyl-1,2-dihydroquinoline, and is a green and environment-friendly preparation process. [0002] The invention relates to a method for preparing 2,2,4-trimethyl-1,2-dihydroquinoline by continuous catalytic condensation, which is an environmentally friendly and efficient preparation process, using continuous tower reactors instead of intermittent kettles Type reactor, continuous operation can reduce raw material consumption, greatly reduce power cost, reduce labor intensity, and maintain the stability of production and product quality. Background technique [0003] 2,2,4-Trimethyl-1,2-dihydroquinoline is a monomer for preparing anti-aging agent RD (anti-aging agent TMQ). The current synthesis method is mainly prepared by condensation reaction of aniline and acetone in the presence of an acidic catalyst. The acid catalysts include li...
Claims
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Application Information
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