A kind of method for preparing dodecanedioic acid

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

Active Publication Date: 2021-05-14
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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  • A kind of method for preparing dodecanedioic acid
  • A kind of method for preparing dodecanedioic acid
  • A kind of method for preparing dodecanedioic acid

Examples

Experimental program
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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 preparing dodecanedioic acid. The method uses nitric acid, cyclododecanone and / or cyclododecanol as raw materials, controls the concentration of nitric acid in the reaction process at 65-90 wt%, and produces in the form of reaction crystallization under the action of a catalyst, by controlling the feeding speed and The particle size of the crystallized product can separate the dodecanedioic acid solid in time, reduce the occurrence of side reactions, and improve the reaction selectivity. The unit consumption of nitric acid is reduced; and a simple and feasible mother liquor acid recycling method is provided, which avoids a large-scale nitric acid rectification and concentration process.

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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Patent Type & Authority Patents(China)
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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