A kind of method for preparing terpenoid compound with bifunctional catalyst catalyzing mevalonic acid
A technology of catalyst catalyzing mevalonic acid and bifunctional catalyst, applied in catalysts, hydrocarbons, hydrocarbons and other directions, can solve problems such as low biosynthesis efficiency, achieve suitable reaction conditions, low catalyst cost and simple process flow Effect
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[0033] The invention provides a preparation method of simple process, suitable reaction conditions and high value-added terpenoid products. The method includes: 1) processing the mevalonic acid fermentation broth to obtain dehydrated mevalonolide; 2) adding dehydrated mevalonolide, a solvent, water, a bifunctional catalyst and a resistance to a high-temperature and high-pressure reaction kettle. The polymerization agent is heated to 150-300°C for 2-10 hours, the reaction product is cooled, filtered to obtain a product mixture and a bifunctional catalyst, and the product mixture is separated to obtain terpenoids.
[0034] To further illustrate, the method includes:
[0035] (1) Put the mevalonic acid fermentation broth into a beaker, add a sufficient amount of activated carbon to remove impurities and then centrifuge, filter to obtain a transparent solution, transfer the solution to a three-necked flask, add concentrated sulfuric acid until the pH of the solution is less than 2...
Embodiment 1
[0039] Example 1. Method for preparing terpenoids from mevalonic acid catalyzed by bifunctional catalysts.
[0040] 1) Add activated carbon (>200 mesh) to the mevalonic acid fermentation broth, and remove impurities with activated carbon. After stirring for 1 hour, put it into a centrifuge tube and use a centrifuge for centrifugation (10000r / min, 5min), and take the supernatant. put into a three-necked flask, and the concentrated H 2 SO 4 solution (concentrated H 2 SO 4 The volume ratio of the solution to the fermentation broth is 1:10) into a constant pressure dropping funnel to acidify the supernatant, build a reflux condensing device, and stir at 120 °C for 12 h. After cooling, use the same volume of dichloromethane as the fermentation broth for extraction three times, add anhydrous sodium sulfate to remove water and dry, rotate to remove dichloromethane, use saturated sodium carbonate solution for alkaline washing, and then extract with dichloromethane , repeat the alk...
Embodiment 2
[0042] Example 2. Method for preparing terpenoids from mevalonic acid catalyzed by bifunctional catalysts.
[0043] The bifunctional catalyst used in this example was prepared by the following method: Ni(NO 3 ) 2 ·6H 2 After O (1.98g) was dissolved in deionized water, SiO was added 2 -Al 2 O 3 (2g) Ultrasound for 30min with an ultrasonic instrument, rotary-evaporated to remove excess water, then placed in an oven and dried at 110°C for 12h, taken out, calcined at 500°C for 4h in a tube furnace, and reduced at 150°C for 2h under a hydrogen atmosphere , get Ni / SiO 2 -Al 2 O 3 For the catalyst, the loading of Ni was 20%, and the particle size of Ni was 100 nm.
[0044] 1) For the preparation of dehydrated mevalonolactone, refer to step 1) in Example 1.
[0045] 2) 1.12 g of dehydrated mevalonolactone prepared by the method described in step 1) in Example 1 was added to the high temperature and high pressure reaction kettle, 9 mL of 1,4-dioxane and 3 mL of deionized water...
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