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Improved method for producing 2-alkylene alicyclic ketone

A technology for alkylene aliphatic and alicyclic ketone, which is applied in the field of environment-friendly production of 2-alkylene alicyclic ketone, can solve the problems of easy self-polymerization and slow production speed of aliphatic aldehyde, and achieves reduction of by-products and production speed. Increased, enhanced selectivity and yield effects

Inactive Publication Date: 2013-01-16
TIANJIN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are still the disadvantages of slow formation of the main product and easy self-polymerization of fatty aldehydes, so it is necessary to further improve the technology

Method used

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  • Improved method for producing 2-alkylene alicyclic ketone
  • Improved method for producing 2-alkylene alicyclic ketone
  • Improved method for producing 2-alkylene alicyclic ketone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041]Embodiment 1 A kind of method adopting clean technology to synthesize 2-alkylene cycloaliphatic ketones comprises the following steps:

[0042] (1) Put a certain amount of alicyclic ketones, fatty aldehydes, weakly basic ion exchange resins, acids (chemical compounds) and aqueous solutions containing metal ions into the reactor at one time and mix them at room temperature, then heat up to 30°C. Continue to react until the basic reaction of aliphatic aldehyde is complete;

[0043] (2) separate resin, water layer (phase) and oily phase (organic phase) from the reaction mixture that step (1) obtains, for the resin that still has reactivity, can be used for next batch of reaction use, the resin that loses activity sends to regenerate; the water phase can be recycled;

[0044] (3) the oil phase (organic phase) that step (2) obtains adopts vacuum distillation to remove the light fraction containing unreacted cycloaliphatic ketone and some low boiling point substances, and thi...

Embodiment 2

[0046] Embodiment 2 A kind of method adopting clean technology to synthesize 2-alkylene alicyclic ketones comprises the following steps:

[0047] (1) First put alicyclic ketone, weakly basic ion exchange resin, acid (active compound) and aqueous solution containing metal ions into the reactor at one time, after heating up to 50°C, add aliphatic aldehyde dropwise under stirring, and then maintain Continue to react at this temperature until the basic reaction of aliphatic aldehyde is complete;

[0048] (2) separate resin, water layer (phase) and oily phase (organic phase) from the reaction mixture that step (1) obtains, for the resin that still has reactivity, can be used for next batch of reaction use, the resin that loses activity sends to regenerate; the water phase can be recycled;

[0049] (3) the oil phase (organic phase) that step (2) obtains adopts vacuum distillation to remove the light fraction containing unreacted cycloaliphatic ketones and low boilers, and the light...

Embodiment 3

[0051] Embodiment 3 A kind of method adopting clean technology to synthesize 2-alkylene alicyclic ketones comprises the following steps:

[0052] (1) Put a certain amount of alicyclic ketones and aliphatic aldehydes into the reactor, heat up to 70°C, and then put in a mixture of weakly basic ion exchange resins, acids (active compounds) and aqueous solutions containing metal ions, and then maintain this temperature Continue to react until the basic reaction of fatty aldehyde is complete;

[0053] (2) separate resin, water layer (phase) and oily phase (organic phase) from the reaction mixture that step (1) obtains, for the resin that still has reactivity, can be used for next batch of reaction use, the resin that loses activity sends to regenerate; the water phase can be recycled;

[0054] (3) the oil phase (organic phase) that step (2) obtains adopts vacuum distillation to remove the light fraction containing unreacted cycloaliphatic ketones and low boilers, and the light fra...

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Abstract

The invention discloses an improved method for producing 2-alkylene alicyclic ketone. In the method, alicyclic ketone and aliphatic aldehyde are used as raw materials, and the reaction of amine type alkalescent ion exchange resin in the presence of an acid compound and metal ions is utilized to generate the 2-alkylene alicyclic ketone. After an organic phase is separated out, a catalyst system can be recycled. The 2-alkylene alicyclic ketone is an important intermediate for synthesizing a plurality of spices (such as methyl dihydrojasmonate and delta-lactone). The method gets rid of a traditional unrecoverable solution catalysis system, replaces the traditional unrecoverable solution catalysis system by a recoverable and recyclable catalysis system, reconstructs an original process by a clean production technology and also realizes the saving and the sufficient utilization of resources and environmental protection.

Description

【Technical field】 [0001] The invention relates to the field of fine chemicals in chemical engineering—preparation of spice intermediates, which replaces the original process with clean production technology, and simultaneously realizes resource conservation and full utilization, as well as environmental protection, especially an environmentally friendly production 2- The method of alkylene cycloaliphatic ketones. 【Background technique】 [0002] The condensation reaction of aldehydes and ketones is a common reaction to increase carbon chains, and many new compounds can be formed, which is a very important class of organic synthesis reactions. An important intermediate in the synthesis of many spices (such as methyl dihydrojasmonate, δ-lactone) - 2-alkylene alicyclic ketones are obtained through condensation reactions using aliphatic aldehydes and alicyclic ketones as raw materials: [0003] R: alkyl [0004] [000...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/74C07C49/647B01J31/38B01J31/32B01J31/34B01J31/28B01J31/30B01J31/26
CPCY02P20/584
Inventor 孙波高志国沈润贺昌荣
Owner TIANJIN UNIVERSITY OF TECHNOLOGY
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