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Preparation method of dehydroabietic acid

A technology of dehydroabietic acid and rosin, applied in the field of rosin disproportionation reaction, can solve the problems of increased equipment investment, large solvent loss, complicated operation, etc., and achieve the effects of less three wastes, convenient post-treatment, and high conversion rate

Active Publication Date: 2012-09-12
广西贺州华川林产科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the loss of solvent is very large, which increases the investment of equipment, the operation is more complicated, the cost is high, and it is not conducive to reducing energy saving and emission reduction from the source.

Method used

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  • Preparation method of dehydroabietic acid
  • Preparation method of dehydroabietic acid

Examples

Experimental program
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preparation example Construction

[0024] Catalyst preparation

[0025] (1) carrier preparation: ZrOCl 2 ·8H 2 Slowly add 322 g of O to 100 mL of deionized water with constant stirring. 85 ml of aqueous ammonia solution with a mass concentration of 25% was added dropwise to the formed solution to adjust the pH value to 10. Seal the formed hydroxide sol together with the mother liquor, cook at 95°C for 60 hours, filter the resulting precipitate, wash it with deionized water, and wash it with AgNO 3 Cl in it cannot be detected - exist. The filter cake was dried at 120°C for 8 hours and then calcined at 450°C for 2 hours to obtain ZrO 2 carrier with a specific surface area of ​​165m 2 / g, the pore volume is 0.25mL / g. Then, the prepared ZrO 262 grams and γ-Al 2 o 3 51 grams were mixed and extruded into rods, dried at 120°C for 24 hours, and then calcined at 600°C for 4 hours in a muffle furnace. The carrier specific surface area is 183m 2 / g, the pore volume is 0.47mL / g.

[0026] (2) Loading of the ac...

Embodiment 1

[0028] In a 250 ml three-necked bottle, add 31 grams of ground commercially available rosin, Pt / ZrO 2 -γ-Al 2 o 3 (the loading capacity of Pt is 1% by carrier mass) 6 grams of solid acid catalysts, 150 grams of 1-methyl-3-butylimidazolium tetrafluoroborate ionic liquid constitutes reaction system, connects reflux condenser, is heated to 110 ° C, reflux reaction for 5 hours, stop heating, after the reaction system is cooled to room temperature (20 ° C), add 100 mL of toluene to the reaction system for extraction, obtain the upper layer liquid and the lower layer precipitate, the lower layer precipitate is a solid acid catalyst and ionic liquid, Recycling and reuse, take the upper layer and carry out rotary concentration to remove toluene to obtain the crude product of disproportionated rosin (i.e. concentrate), the crude product is subjected to silica gel column chromatography (eluent is petroleum ether: ethyl acetate = 5: 1 (volume ratio)) , TLC follow-up detection (developi...

Embodiment 2

[0030] In a 250 ml three-necked bottle, add 31 grams of ground commercially available rosin, Pt / ZrO 2 -γ-Al 2 o 3 (the loading of Pt is 0.25% by carrier mass) 9 grams of solid acid catalyst, 300 grams of 1-methyl-3-octyl imidazolium bisulfate ionic liquid constitute reaction system, connect reflux condenser, be heated to 80 ℃ , reacted for 10 hours, after the reaction system was cooled to room temperature (20°C), 100 mL of toluene was added to the reaction system for extraction, and the upper layer and the lower layer were obtained. The lower layer was solid acid catalyst and ionic liquid, which were recycled and reused. The toluene was removed by rotary concentration to obtain the crude product of disproportionated rosin (i.e. concentrate), the crude product was subjected to silica gel column chromatography (eluent was petroleum ether: ethyl acetate=5:1 (volume ratio)), followed by TLC detection (developing solvent was Petroleum ether: ethyl acetate=5: 1 (volume ratio)), co...

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Abstract

The invention discloses a preparation method of dehydroabietic acid, comprising the following steps of: adding rosin into a solid acid catalyst and an ionic liquid as shown in the formula (I) to form a reaction system, performing a reflux condensation reaction for 1-10h at 80-150 DEG C, adding toluene into the reaction system for extraction after the reaction, taking a supernatant and concentrating, and letting a concentrate undergo column chromatography to obtain dehydroabietic acid. The solid acid catalyst and the ionic liquid as shown in the formula (I) are reused; according to the solid acid catalyst, ZrO2 and gamma-Al2O3 are used as carriers and Pt is used as an active component, wherein the mass ratio of the carrier ZrO2 to gamma-Al2O3 is 1:1 and load capacity of the active component is 0.1-1% according to the weight of the carriers. The solid acid and the ionic liquid are used to prepare dehydroabietic acid. The technology is easy to operate, conversion rate is high, ''three wastes (waste gas,waste water and industrial residue)'' are less, post-treatment is convenient, and the solid acid and the ionic liquid are repeatedly usable. The preparation method provided by the invention is an economical, practical, green and environmentally friendly technology.

Description

(1) Technical field [0001] The invention relates to a disproportionation reaction of rosin promoted by an ionic liquid, in particular to a method for preparing dehydroabietic acid through disproportionation of rosin under the action of an acidic catalyst. (2) Background technology [0002] Rosin is an extremely abundant renewable resource in nature. In the world's rosin market, China's rosin production dominates. But so far, the deep processing of rosin products in China is not enough, the price is low, and the added value is not high. In order to make full use of rosin, a rich renewable resource, develop new fine chemicals and increase technical content to meet the needs of various domestic industries and strengthen the international market. The development and research of rosin deep-processing products have always attracted much attention, and the research on rosin deep-processing has extremely important significance. [0003] Dehydroabietic acid is one of the important ...

Claims

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Application Information

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IPC IPC(8): C07C61/29C07C51/347
CPCY02P20/584
Inventor 裴文胡卫雅孙莉方锡武孙孟展
Owner 广西贺州华川林产科技有限公司
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