Terpinol CAS 8000-41-7

A kind of new technology of Terpinol, comprises the following steps:

The first step, synthesizing terpene diol hydration: mixing 272g of industrial grade turpentine or α-pinene or β-pinene with acid water with a mass fraction of 20 to 75% into the reactor, The acid-water mixture is made of sulfuric acid, phosphoric acid, p-toluenesulfonic acid, chloroacetic acid, or two or more of them mixed with water to form a catalyst, and polyvinyl alcohol, organic One or more than one of the amine salts is used as an emulsifier, and the hydration reaction is carried out under the stirring condition of 100-1000rpm (preferably 400-800rpm) to generate crystalline terpene diol hydrate, and ultrasonic waves are used for the initial 2-4h of the reaction Aids in emulsification. The quality of water is 1～3 times of turpentine quality, preferably 1～2 times; The quality of catalyst is 20～75% of turpentine quality, preferably 25～50%; The quality of emulsifier is 0.001～0.2% of turpentine quality , preferably 0.01-0.1%; the reaction temperature is 20-75°C, preferably 20-60°C; the reaction time is 12-36h, preferably 18-24h. Turpentine is one or more mixtures of gum turpentine, sulfate turpentine, wood turpentine, and dry distillation turpentine. Its active ingredients are α-pinene and β-pinene. Industrial-grade α-pinene or β-pinene and α-pinene or β-pinene from other natural essential oils (such as eucalyptus oil, camphor oil, etc.) were used instead of turpentine as reaction raw materials.

In the second step, stop stirring after the hydration reaction is over, and use ultrasonic waves to vibrate and stir for a certain period of time, then settle and stratify, and release an acid-water mixture containing a small amount of terpene hydration diol from the bottom of the reactor, and the acid-water mixture after further clarification is prepared. When the appropriate ratio is reached, all of them are recovered for the next reaction.

In the third step, the crystalline product left in the reactor is neutralized and washed once with a NaOH aqueous solution with a mass fraction of 3-5%. During the washing process, the acidic catalyst remaining between the crystals is fully recovered After the alkaline washing solution is recovered, an appropriate amount of NaOH can be added to prepare an aqueous solution with a mass fraction of 5% for the next batch of neutralization and washing.

In the fourth step, the crystallized product that has been neutralized and washed by alkali is then washed with water under the action of ultrasonic intensification until the washing liquid is neutral to weakly alkaline. The washing liquid is released, and the washing liquid recovered each time is used for washing the next batch of reaction products, and the washing water that cannot be reused is put into the neutralization tank for clarification before recycling.

The fifth step, dehydration of terpene diol to synthesize Terpinol: the hydrated terpene diol crystallization product obtained through neutralization and water washing and the unseparated red oil contained in it are transferred to the dehydration reactor under the action of adding water and stirring, and are mixed with sulfuric acid, Phosphoric acid, p-toluenesulfonic acid, chloroacetic acid and other commonly used inorganic or organic acids or a mixture of two or more are used as catalysts, and within 1 hour after adding materials, ultrasonic waves are used to assist in accelerating the hydration of terpene diol in aqueous media. Dispersion and dissolution, dehydration reaction of terpene diol to produce Terpinol crude product commonly known as butter. In the dehydration reaction process, the quality of water is 1 to 2 times the quality of terpene diol hydrate and red oil, preferably 1 to 1.5 times; the quality of the catalyst is 0.1 to 2.5% of the quality of terpene diol hydrate and red oil, preferably 0.1 ~1.0%; the reaction temperature is 60~120°C, preferably 80~110°C; the reaction time is 2~12h, preferably 3~6h.

The sixth step is to separate and refine Terpinol: After the hydration reaction and dehydration reaction are completed, the lower acid layer is separated by standing. The crude terpineol product of the upper layer oil obtained, that is, butter, is neutralized with an aqueous sodium hydroxide solution with a mass fraction of 2 to 10% and washed with water until the washing liquid is neutral and slightly alkaline (pH=7 to 9), The crude product was obtained by standing and stratifying, and then the Terpinol product meeting the standard was obtained through vacuum distillation and continuous rectification.