Solid catalyst for synthesis of plant growth regulator DA-6
A solid catalyst and carrier technology, applied in physical/chemical process catalysts, organic chemistry, chemical instruments and methods, etc., can solve the problems of cumbersome catalyst preparation, high price, and high cost, to solve environmental pollution and cost increase, and improve the reaction. Rate and conversion rate, the effect of a simple method
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Embodiment a
[0034] 1) Weigh 0.2-0.6g of polyurethane foam microspheres, 100g of alumina powder with a particle size of 200-400 mesh, mix the two, then add 10-20g of water, stir and mix thoroughly, heat-treat at 150°C for 4 hours, and continue to rise Heat treatment at a temperature of 400°C for 3 hours to prepare a porous alumina carrier;
[0035] 2) Soak the porous alumina carrier prepared in step 1) with concentrated sulfuric acid with a concentration of 98% by mass for 1 to 3 hours, wherein the volume ratio of alumina carrier to concentrated sulfuric acid is 1:1 to 1:3; then to filter;
[0036] 3) The solid catalyst was prepared by heat-treating the filtered solid matter at 250° C. for 6 hours.
Embodiment b
[0038] 1) Weigh 0.4-1.2g of polyurethane foam microspheres, 200g of alumina powder with a particle size of 200-400 mesh, mix the two, then add 30g of water, stir and mix thoroughly, heat treatment at 120-180°C for 3-6 hours, continue Elevate the temperature to 350-500°C and heat-treat for 2-4 hours to prepare a porous alumina carrier;
[0039] 2) Soak the porous alumina carrier prepared in step 1) with concentrated sulfuric acid with a concentration of 98% by mass for 1 to 3 hours, wherein the volume ratio of alumina carrier to concentrated sulfuric acid is 1:1 to 1:4; then to filter;
[0040] 3) Heat-treating the filtered solid matter at 200-300° C. for 5-8 hours to prepare a solid catalyst.
[0041] Preparation of plant growth regulator DA-6
Embodiment 1
[0043] Add 54g of n-hexanoic acid and 45g of diethylaminoethanol into the reactor, and then add 1g of the solid catalyst prepared in Example a. Inject N at a rate of 20mL / min 2 , and at the same time connect the condenser tube, heat the reaction material to 130-150 ° C for 2-10 hours, filter out the catalyst, and obtain the plant growth regulator DA-6; sample once every 2 hours, add toluene to dilute the sample by 10 times, and use Gas chromatograph analysis yield.
[0044] From the chromatographic analysis results, it is known that the solid catalyst of the present invention shows a good effect, and the 2h productive rate can reach 56.06%, the 4h productive rate is 75.75%, the 6h productive rate is 87.05%, the 8h productive rate is 93.22%, 8~ There was no significant increase in yield at 10 h. From the consideration of saving cost, the reaction time is beneficial to 8h. The plant growth regulator DA-6 prepared by the method has no pollution to the environment and does not ...
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Abstract
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