Preparation method for one-step method synthesis alpha-terpilenol
A technology of terpineol and one-step method is applied in the field of preparation of one-step synthesis of α-terpineol, can solve the problems of low conversion rate, difficult separation and recovery, unsatisfactory selectivity, etc., and achieves low investment, simple steps, low cost effect
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[0028] A kind of preparation method of synthesizing α-terpineol by one-step method, comprises the following steps:
[0029] A. Synthesis of α-terpineol crude product: Prepare acid water and add emulsifier to fully dissolve it, add it to the reaction kettle, then add the main raw materials to the reaction kettle to raise the temperature and react; when the reaction temperature is close to the holding temperature, stop heating and rely on the reaction Exotherm naturally rises to the holding temperature; when the reaction temperature exceeds the control temperature, add the prepared acid water to the reactor, and use the acid water to cool down to keep it within the temperature range required for the reaction. When the pinene is less than 12%, it will It is the end point of the reaction; after static discharge of acid, the crude product of α-terpineol is washed with alkali to make the crude product of α-terpineol weakly alkaline; the crude product of α-terpineol after washing is l...
Embodiment 1
[0034]A kind of preparation method of synthesizing α-terpineol by one-step method, comprises the following steps:
[0035] A. Synthesis of α-terpineol crude product: Prepare 400g of 28% phosphoric acid water and add 0.3g of emulsifier 1631 to fully dissolve, 200g of which is added to the reaction kettle, and then 300g of β-pinene content 95.5% turpentine is added to the reaction kettle Moderate temperature rise reaction; stop heating when the reaction temperature is close to 65°C, and naturally rise to 73-75°C by the reaction heat to keep warm; when the reaction temperature exceeds 75°C, add the prepared acid water to the reactor, and use acid water to cool down Keep it within the temperature range required for the reaction. During the sampling test, when the pinene is less than 12%, it is the end of the reaction; after 4.5 hours of reaction, the crude product pinene remains 11.9%, the total alcohol is 61.8%, α-terpineol is 53.5%, and γ-terpineol is 2.2%.
[0036] B. Separati...
Embodiment 2
[0038] A kind of preparation method of synthesizing α-terpineol by one-step method, comprises the following steps:
[0039] A, synthesis of α-terpineol crude product: prepare 400g of 18% sulfuric acid water and add 0.3g of emulsifier benzalkonium bromide to fully dissolve, wherein 200g is added in the reactor, and then 300g of turpentine is added to the reactor and heated up for reaction; Stop heating when the reaction temperature is close to 58°C, and naturally rise to 63-65°C by exothermic reaction to keep warm; when the reaction temperature exceeds 65°C, add the prepared acid water to the reaction kettle, and use acid water to cool down to keep it at within the temperature range required for the reaction. During sampling detection, when pinene is less than 12%, it is the end point of the reaction; through standing to discharge acid, and carrying out alkali washing to the crude product of α-terpineol, the crude product of α-terpineol is weakly alkaline; The washed α-terpine...
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Abstract
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