Method for preparing terpin hydrate by virtue of continuous hydration

A technology for obtaining hydrated terpene diol and hydrated terpene diol, which is applied in the field of continuous hydration to prepare hydrated terpene diol, can solve the problems of long time consumption, long reaction time, low production efficiency, etc., and achieves reduced production cost and simple production process. , the effect of improving production efficiency

Active Publication Date: 2012-10-10
FUJIAN SENFA BIOTECH
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  • Summary
  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

Since the hydration reaction needs to consume water in the aqueous acid solution, the concentration of the acid water after the reaction in the intermittent hydration is several points higher than that before the reaction, and the higher concentration of the acid water will directly dehydrate the terpene diol into alcohol, and continue to Dehydration produces terpene by-products, resulting in a decrease in yield
Simultaneously, because the intermittent hydration reaction time is longer, the retention time of the product terpene diol in the acid aqueous solution also increases correspondingly, resulting in the obtained hydrated terpene diol crystals being older, with large particles and high acid content, which will bring problems to the subsequent dehydration process. It is troublesome and brings a lot of waste water and waste acid to the production
And, according to the analysis of the production situation, although this hydration reaction belongs to a mature traditional process, there are still some obvious shortcomings as follows: 1) the hydration yield is not high: in production, the pinene hydration reaction makes the weight of the hydration terpene diol The yield is generally around 85%, and in relatively good factories, the yield of terpene diol hydrate can only reach about 90%, which is only 70% of the theoretical yield, and there is still a lot of room for improvement; 2) Treatment Low capacity and low production efficiency
Because the intermittent hydration reaction takes a long time, usually more than 20 hours, and the solid content in the reactor after the reaction is high, it takes a long time to discharge, so each reactor can only produce one batch per day Terpene diol hydrate, even if calculated at a weight yield of 90%, the daily production capacity is less than 1.5 tons of terpene diol hydrate; 3) The quality of the terpene diol hydrate obtained is unstable
Due to the long reaction time, the hydrated terpene diol crystal particles are relatively coarse, and the acid water and oil content contained therein vary greatly, which brings great inconvenience to the subsequent treatment and dehydration reaction, not only produces a large amount of waste water, but also thus increasing the cost of production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1) Prepare a sulfuric acid aqueous solution with a concentration of 25%;

[0024] 2) Drop into 2.85 tons of 25% concentration of sulfuric acid aqueous solution and 1.908 tons of turpentine in a reaction kettle of 5 cubic meters, and heat and stir;

[0025] 3) Maintain the temperature of the reactor at 25~35°C throughout the continuous hydration production process;

[0026] 4) After 15 hours of reaction, start the production operation of continuous feeding and continuous discharging. On the first day of continuous feeding and continuous discharging, a total of 2.684 tons of raw material turpentine and 0.842 tons of water were added, and 2.984 tons of hydrated terpene diol and 0.653 tons of red oil were produced, with an average acid water concentration of 27.6%; 2.243 tons of raw turpentine and 0.745 tons of water, 2.432 tons of hydrated terpene diol and 0.564 tons of red oil were produced, with an average acid water concentration of 28.1%; on the third day, a total of ...

Embodiment 2

[0030] 1) Prepare sulfuric acid and phosphoric acid aqueous solutions with a concentration of 28.2%;

[0031] 2) Put 2.93 tons of 28.2% sulfuric acid and phosphoric acid aqueous solution and 1.48 tons of turpentine into the reactor of 5 cubic meters, and heat and stir;

[0032] 3) Maintain the temperature of the reactor at 25~35°C throughout the continuous hydration production process;

[0033] 4) After 10 hours of reaction, start the production operation of continuous feeding and continuous discharging. On the first day of continuous feeding and continuous discharging, a total of 2.313 tons of raw material turpentine and 0.752 tons of water were added, and 2.524 tons of hydrated terpene diol and 0.563 tons of red oil were produced, with an average acid water concentration of 30.5%; 2.211 tons of raw turpentine and 0.785 tons of water, 2.236 tons of hydrated terpene diol and 0.474 tons of red oil were produced, with an average acid water concentration of 30.7%; on the third d...

Embodiment 3

[0037] 1) Prepare a sulfuric acid aqueous solution with a concentration of 30.4%;

[0038]2) Put 3.42 tons of 30.4% sulfuric acid aqueous solution and 1.54 tons of pinene into a 5 cubic meter reactor, and heat and stir;

[0039] 3) Maintain the temperature of the reactor at 25~35°C throughout the continuous hydration production process;

[0040] 4) After 8 hours of reaction, start the production operation of continuous feeding and continuous discharging. On the first day of continuous feeding and continuous discharging, 2.508 tons of raw pinene and 0.965 tons of water were added, and 2.754 tons of hydrated terpene diol and 0.582 tons of red oil were produced, with an average acid water concentration of 32.3%; Add 2.354 tons of raw pinene and 0.712 tons of water, and produce 2.497 tons of terpene diol hydrate and 0.498 tons of red oil. 1 ton of terpene diol hydrate and 0.528 tons of red oil, the average concentration of acid water is 32.2%; on the fourth day, 2.234 tons of ra...

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Abstract

The invention discloses a method for preparing terpin hydrate by virtue of continuous hydration. The method is characterized by comprising the following steps of: under the conditions of certain acidity, temperature and acid water quantity, carrying out the continuous hydration on turpentine or pinene utilized as a raw material in a way of continuously feeding and discharging; and controlling the reaction temperature by adjusting the acid water concentration and the quantity of the acid water and red oil according to the detection data and the weight of materials, thus obtaining the terpin hydrate. Compared with the traditional intermittent hydration method, the method can be used for improving the production efficiency of the terpin hydrate by more than 30%, achieving the yield of 100% and improving the yield by 10%, and has the advantages of being high in production efficiency and yield, simple and convenient in technology, free from pollution, low in production cost, and the like.

Description

technical field [0001] The present invention relates to a method for continuous hydration, in particular to a method for preparing terpene diol hydrate through continuous hydration. Background technique [0002] Terpineol is a bulk spice product, with an annual domestic output of more than 30,000 tons. It is widely used in pharmaceuticals, soaps, cosmetics, blending essences, and foaming agents for flotation of non-ferrous metals. It is the main export variety in my country, and the export market There are also signs of increasing year by year, and export prices have been relatively stable. my country is rich in turpentine resources, with an annual output of more than 100,000 tons, and its main component is pinene. The most important way to utilize turpentine is to synthesize terpineol. [0003] At present, there are mainly two methods for producing terpineol with pinene as a raw material: one-step method and two-step method: one-step method is that pinene is directly hydra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C35/08C07C29/04
Inventor 许鹏翔黄金龙刘学东
Owner FUJIAN SENFA BIOTECH
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