A kind of method for preparing isobornyl acetate by esterification of camphene

A technology of isobornyl acetate and camphenyl acetate, applied in the field of chemical technology, can solve problems such as increased production cost, cumbersome process operation, low product yield, etc., and achieves the effect of improving service life and reducing polymerization reaction.

Inactive Publication Date: 2011-12-14
FUZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Before the 1970s, sulfuric acid was used as a catalyst in industrial production, but when sulfuric acid was used as a catalyst, it had the disadvantages of cumbersome process operation, many side reactions, corrosion of equipment, and environmental pollution by waste water, which has been basically eliminated.
Chinese patent CN1036950A discloses a method for synthesizing isobornyl acetate with natural mordenite as a catalyst. The disadvantage of this method is that the product yield is low, the by-products are difficult to separate, resulting in low product purity, large investment and energy consumption
Chinese patent CN101372453A discloses a method for synthesizing isobornyl acetate with an acidic cation exchange resin as a catalyst, which adopts a fixed-bed continuous reaction process. Although the method has a higher single-pass yield, the catalyst life is short, making production Increased costs, and a large amount of organic waste needs to be processed, which increases the burden on environmental protection
Chinese patent CN101921191A discloses a method for preparing isobornyl acetate with a synthetic molecular sieve as a catalyst. Although the method improves the selectivity of isobornyl acetate and is environmentally friendly, it fails to solve the problem of camphene's easy polymerization and water pairing. The effect of catalyst activity

Method used

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  • A kind of method for preparing isobornyl acetate by esterification of camphene

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Using industrial camphene and industrial acetic acid as raw materials, put them into the raw material mixing tank V-101 at a molar ratio of 1:1.1, mix them evenly with stirring, and preheat them to 40°C with steam. The moisture content in the reactor feed was controlled to less than 50 ppm by adding acetic anhydride, and 200 ppm of hydroquinone was added. Suspended bed reactor R-101 is used, and the reactor is equipped with CT800 with an ion exchange capacity of 5.2mmol / g accounting for 80% of the reactor volume +Cation exchange resin, the resin is pre-soaked with acetic acid and acetic anhydride, and the fully mixed raw materials in V-101 are pumped into the reactor R-101 with the raw material pump P-101 at a speed of 0.2m / min, so that the catalyst is evenly suspended in the In the reactor, the reaction temperature is set at 40°C, and the feed space velocity of the reactants is 3.780 h -1 , the reaction pressure is normal pressure. The conversion rate of camphene is ...

Embodiment 2

[0042] Using industrial camphene and industrial acetic acid as raw materials, put them into the raw material mixing tank V-101 at a molar ratio of 1:2.0, mix them evenly with stirring, and preheat them to 40°C with steam. The moisture content in the reactor feed was controlled to be less than 50 ppm by adding acetic anhydride, and 50 ppm of hydroquinone was added. Suspended bed reactor R-101 is used, and the reactor is equipped with CT800 with an ion exchange capacity of 5.2mmol / g accounting for 70% of the reactor volume + Cation exchange resin, the resin is pre-soaked with acetic acid and acetic anhydride, and the raw materials that are completely mixed in V-101 are pumped into the reactor R-101 with the raw material pump P-101 at a speed of 0.1m / min, so that the catalyst is evenly suspended in the In the reactor, the reaction temperature is controlled at 20°C, and the space velocity of the reactants is 0.10 h -1 , the reaction pressure is 1.0MPa. The conversion rate of ca...

Embodiment 3

[0044] Using industrial camphene and industrial acetic acid as raw materials, put them into the raw material mixing tank V-101 at a molar ratio of 1:1.5, mix them evenly with stirring, and preheat them to 30°C with steam. By adding acetic anhydride, the moisture content in the reactor feed is controlled to be less than 50 ppm, and 100 ppm of p-benzoquinone is added. Suspension bed reactor R-101 is used, and the reactor is equipped with an ion exchange capacity of 4.8mmol / g NKC-9 catalyst accounting for 60% of the reactor volume. The resin is soaked in acetic acid and acetic anhydride in advance, and the V-101 is completely mixed. The final raw material is pumped into the reactor R-101 with the raw material pump P-101, the speed is 0.5m / min, so that the catalyst is evenly suspended in the reactor, the reaction temperature is controlled at 100°C, and the space velocity of the reactant is 6.0h -1 , the reaction pressure is normal pressure. The conversion rate of camphene is 71.2...

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Abstract

The invention relates to a continuous preparation method for synthesizing isobornyl acetate by esterification of camphene and acetic acid. Using camphene and acetic acid as raw materials, using solid acid as a catalyst, and adding a certain amount of polymerization inhibitor and acetic anhydride, the esterification reaction is carried out under certain process conditions in a catalyst bed filled with suspension, and the target product acetic acid is obtained. Isobornyl. The invention has the advantages of mild reaction conditions, long service life of the catalyst, good product quality, high raw material conversion rate, continuous production and simple operation, and can be widely used in large-scale industrial production of isobornyl acetate.

Description

technical field [0001] The invention belongs to the field of chemical technology, and more specifically relates to a method for preparing isobornyl acetate through esterification of camphene. Background technique [0002] Isobornyl acetate is an important chemical raw material - an intermediate in the synthesis of camphor. It is used as a spice because of its fragrance and pine leaf smell. It can be used mainly as a fragrance for making soap, and can also be used as an air disinfectant and insecticide. Sprays, sprays, etc. [0003] At present, there are not many industrial studies on the production of isobornyl acetate by esterification of camphene, and most of the industrial production is at the level of batch production, while the production process route of the batch stirred tank is long, time-consuming and labor-intensive, and the catalyst is easy to stir during the stirring process. At the same time, there are differences in reaction residence time, temperature and raw...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/14C07C67/04
Inventor 郑辉东王碧玉王莹淑邱挺
Owner FUZHOU UNIV
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