Method for continuously producing pinane by pinene and device therefor

Abstract

The invention relates to a method for continuously producing pinane by pinene and a device therefor. The method comprises the following steps: (1) placing catalyst into a fixed bed reactor, replacing air with nitrogen, then preheating hydrogen before feeding the hydrogen into a gas and liquor mixer; preheating the pinene by a liquor preheater and then feeding the preheated pinene into the gas and liquor mixer; evenly mixing the preheated pinene with hydrogen in the gas and liquor mixer and then feeding the mixture into the fixed bed reactor to carry out hydrogenation; (2) cooling the hydrogenated material; (3) carrying out gas-liquid separation on the cooled reaction mass to obtain a menthane liquid product, returning the separated hydrogen to the fixed bed reactor. The invention also relates to a device for continuously producing pinane by pinene. The method and the device of the invention facilitate the improvement of the unstable state in the hydrogenation production of the pinane by the pinene, improve production efficiency, promote convenient utilization of the automatic control system in the production process and facilitate the reduction of human operational errors; in addition, the invention features stable quality of the product, safe operation, high efficiency and low energy consumption and convenient expansion of production scale.

Description

technical field [0001] The invention relates to a continuous production method and a device for preparing pinane from pinene. Background technique [0002] Pinene is the main component of turpentine. Catalytic hydrogenation of pinene to produce pinane, which can then be used as spices, medical intermediates or other products, can increase the added value of turpentine processed products. [0003] At present, there are two methods for industrially producing pinane from pinene: a batch hydrogenation production process and a continuous fixed-bed hydrogenation production process. [0004] The existing batch hydrogenation production process is to put pinene in the batch hydrogenation reactor for hydrogenation reaction, after the raw materials and catalysts are put into the hydrogenation reactor in proportion, nitrogen and hydrogen are replaced several times, and then the pressure is increased under the stirring of the agitator 1. Heating up and carrying out the hydrogenation re...

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Problems solved by technology

The separated catalyst can only be reused 3 to 10 times, and needs to be replaced afterwards. The service life is short, the number of recycling and regeneration is high, and the consumption is large; in order to maintain full gas-liquid contact and stirring effect, the hydrogen in the hydrogenation reactor accounts for about 40% of the volume, in this way, the effective volume of the hydrogenation reactor is reduced, and because the batch hydrogenation production process includes feed, nitrogen hydrogen replacement, temperature rise, pressure increase, hydrogenation reaction, filtration, pressure reduction, temperature reduction, etc. Multiple operating steps, complex procedures, long time-consuming, low efficiency, high energy consumption; under the same production scale, the hydrogenation reactor and related auxiliary equipment are required to be large in size, occupy a large space, and labor-intensive; intermittent hydrogenation During production, gas replacement is required every time the material is fed into and out of the reactor, resulting in a large waste of hydrogen and nitrogen; due to the existence of the above problems, it is difficult to automate control in production, and the pressure and temperature are unstable, which makes it difficult to control the cis-trans ratio of pinane, and the product quality is stable. Poor performance, difficult to scale up production

[0005] At present, there are problems in the continuous fixed-bed hydrogenation process: first, the price of the precious metal catalyst used is high; even if a low-priced non-precious metal catalyst is used, the service life is generally only 1 month, and the longest is no more than 3 months. About one month makes the production operation process become loaded down with trivial details, and production cost increases; The 2nd, according to the purposes of pinane product as spice intermediate, think that cis-pinane is high, and the activity of carrying out the following reaction is high, therefore in production except pinane is required The yield of alkane products is high, and the selectivity of cis-pinane is also required; the third is that the degree of automation of the production process is low

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