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Method for preparation of dodecanedioic acid

A technology of dodecanedioic acid and cyclododecanone, which is applied in the field of preparation of dodecanedioic acid, and can solve problems such as mixed products, affecting product application performance, and lack

Active Publication Date: 2018-05-11
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If dodecanedioic acid is obtained by cooling crystallization, the α-nitrated diacid product will inevitably precipitate out of the solution and be mixed into the product, affecting the application performance of the product
As mentioned in the patent US3637832, prolonging the reaction time in a homogeneous system can reduce the α-nitration product to a certain extent, but it cannot be completely avoided, and because the main and side reactions are series reactions, prolonging the reaction time will cause the main product to be further destroyed. Excessive oxidation, resulting in more by-product dibasic acids, so the gain outweighs the gain
[0007] In summary, there is currently a lack of a more effective method for preparing dodecanedioic acid from cyclododecanone / alcohol through nitric acid oxidation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 266g of 65wt% nitric acid into a 500mL round bottom bottle, add copper nitrate and ammonium metavanadate so that the Cu and V contents are respectively 0.5wt% and 0.2wt%, and the system is heated to a reaction temperature of 75°C in an oil bath, and cyclododecanone / cyclododecanol is 95:5 by mass ratio and continues to join in the flask with molten state, keeps stirring state, keeps reaction temperature constant by controlling oil bath temperature, adds altogether 50g aforementioned raw materials (nitric acid / ( cyclododecanone) after 60min +cyclododecanol) molar ratio=10:1), crystals were precipitated, the reaction was stopped, and the average particle diameter D50=135m was read by an online particle size analyzer. The resulting slurry is quickly evaporated under high vacuum to remove volatile nitric acid and water, and the volatiles are replenished with a cold trap, and the captured nitric acid is weighed and analyzed for acidity, so as to determine the consumption...

Embodiment 2

[0036] Add 247g of 70wt% nitric acid into a 500mL round bottom bottle, add copper oxide and vanadium pentoxide so that the contents of Cu and V are respectively 0.5wt% and 0.2wt%, and the system is heated to a reaction temperature of 75°C through an oil bath, and cyclododecanone / cyclododecanol is 95:5 by mass ratio and continues to join in the flask with molten state, keeps stirring state, keeps reaction temperature constant by controlling oil bath temperature, adds altogether 50g aforementioned raw materials (nitric acid / ( cyclododecanone) after 45min +cyclododecanol) molar ratio=10:1), crystals were precipitated, the reaction was stopped, and the average particle diameter D50=228m was read by an online particle size analyzer. The resulting slurry is quickly evaporated under high vacuum to remove volatile nitric acid and water, and the volatiles are replenished with a cold trap, and the captured nitric acid is weighed and analyzed for acidity, so as to determine the consumpt...

Embodiment 3

[0038] Add 191g of 90wt% nitric acid into a 500mL round bottom bottle, add copper powder and ammonium metavanadate so that the contents of Cu and V are respectively 0.5wt% and 0.2wt%, and the system is heated to a reaction temperature of 65°C through an oil bath, and cyclododecanone / cyclododecanol is 95:5 by mass ratio and continues to join in the flask with molten state, keeps stirring state, keeps reaction temperature constant by controlling oil bath temperature, adds altogether 50g aforementioned raw materials (nitric acid / ( cyclododecanone) after 45min +cyclododecanol) molar ratio=10:1), a large amount of crystals were precipitated, the reaction was stopped, and the average particle diameter D50=298m was read by an online particle size analyzer. The resulting slurry is quickly evaporated under high vacuum to remove volatile nitric acid and water, and the volatiles are replenished with a cold trap, and the captured nitric acid is weighed and analyzed for acidity, so as to ...

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Abstract

The invention provides a method for preparation of dodecanedioic acid. According to the method, nitric acid, cyclododecanone and / or cyclododecanol are used as raw materials are production in the form of reaction crystallization in the presence of a catalyst, the concentration of the nitric acid in the reaction process is controlled at 65 to 90wt%, by controlling of the feeding speed and the grain size of the crystallized product, and in-time separation of the dodecanedioic acid solid, the side reaction is reduced, the selectivity of the reaction is increased, and the unit consumption of thenitric acid is reduced. A simple and easy method for recycling of mother liquor acid is provided, and a large-scale nitric acid distillation concentration process can be avoided.

Description

technical field [0001] The invention relates to a preparation method of long-chain dibasic acid, in particular to a preparation method of dodecanedioic acid. Background technique [0002] 1,12-Dodecanedioic acid is an important long-chain dibasic acid. It is mainly used in the production of nylon PA612, PA1212, PA PACM12 and other high-performance nylons in industry. It is also used in metal cutting fluids and lubricating oils. . [0003] In industry, the most common dibasic acid production process is to oxidize K / A oil (a mixture of cyclohexanol and cyclohexanone) with nitric acid under the catalysis of Cu / V catalyst to produce adipic acid. This production technology is very mature. and widely adopted worldwide. Many technical details about the reaction process mechanism, reactor form and process conditions, crystallization technology, nitric acid concentration technology, catalyst adsorption / desorption technology, tail gas treatment, etc. of nitric acid oxidation of K / A ...

Claims

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Application Information

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IPC IPC(8): C07C51/27C07C51/43C07C55/21
CPCC07C51/27C07C51/43C07C55/21
Inventor 张彦雨陈海波杜旺明边新建黎源孟熙王文
Owner WANHUA CHEM GRP CO LTD
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