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Method for preparing 4-hydroxy-4-methyl-2-pentanone

A technology of methyl and pentanone, applied in the field of preparation of 4-hydroxy-4-methyl-2-pentanone, can solve the problems of easy dehydration, short service period of acid resin, long reaction time, etc., and achieve less side reactions. , The effect of good product quality and short reaction time

Inactive Publication Date: 2010-05-05
CHANGSHU 3F ZHENFU NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] CN1041196 has introduced a kind of method with macroporous strongly acidic cationic resin as carrier, although this method does not need to add phosphoric acid or phthalic anhydride to adjust pH, its shortcoming is that under acidic condition catalysis, the reaction time is much longer than under alkaline condition, And the generated 4-hydroxyl-4-methyl-2-pentanone is easily dehydrated under acidic conditions to generate by-product mesityl oxide
At the same time, the acid resin has a short service life and needs to be activated after 20 hours of use
[0008] In summary, the industrial production of 4-hydroxy-4-methyl-2-pentanone has not yet reached an ideal state, so there is an urgent need for a more economical, non-polluting production method that can improve the quality of finished products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Pump 4.5 tons of industrial acetone with a content of 99% into a 5500L still, and add 200kg of processed macroporous strong basic anion exchange resin D296 and 100Kg of hydrogen with a particle size of about 1mm to 40mm in the reactor at the same time Magnesium oxide particles are used as a catalyst (magnesium hydroxide particles are placed in a mesh bag and placed in a resin), and steam is used to heat the still, so that the evaporated acetone vapor is cooled to 0°C by refrigerated water and then enters the reactor, and the reaction liquid continuously flows back to the still. Control the flow rate, carry out continuous distillation reaction, stop the reaction when the temperature of the still pot rises to 120°C, and carry out rectification operation on the reaction liquid in the still pot to obtain 4-hydroxy-4-methyl-2 - 3.6 tons of pentanone, with a single yield of 79.6%. 0.85 tons of the front fraction (mainly composed of acetone) that is rectified can be returned t...

Embodiment 2

[0017] 4.5 tons of industrial acetone with a content of 99% is pumped into a 5500L still, and 100kg of treated macroporous strong basic anion exchange resin D296 and 200Kg of hydrogen with a particle size of about 1mm to 40mm are added to the reactor at the same time Magnesium oxide particles are used as a catalyst (magnesium hydroxide particles are placed in a mesh bag and placed in a resin), and steam is used to heat the still, so that the evaporated acetone vapor is cooled to 20°C by refrigerated water and then enters the reactor, and the reaction liquid continuously flows back to the still. Control the flow rate, carry out continuous distillation reaction, stop the reaction when the temperature of the still pot rises to 120°C, and carry out rectification operation on the reaction liquid in the still pot to obtain 4-hydroxy-4-methyl-2 - 3.58 tons of pentanone, with a single yield of 79.4%. The 0.86 ton fraction (mainly composed of acetone) of the rectified fraction can be r...

Embodiment 3

[0019] 4.5 tons of industrial acetone with a content of 99% is pumped into a 5500L still, and 150kg of treated macroporous strong basic anion exchange resin D261 and 150Kg of hydrogen with a particle size of about 1mm to 40mm are added to the reactor at the same time Magnesium oxide particles are used as a catalyst (magnesium hydroxide particles are placed in a mesh bag and placed in a resin), and steam is used to heat the still, so that the evaporated acetone vapor is cooled to 10°C by refrigerated water and then enters the reactor, and the reaction liquid continuously flows back to the still. Control the flow rate, carry out continuous distillation reaction, stop the reaction when the temperature of the still pot rises to 120°C, and carry out rectification operation on the reaction liquid in the still pot to obtain 4-hydroxy-4-methyl-2 - 3.64 tons of pentanone, with a single yield of 81%. 0.83 tons of the front cut (mainly composed of acetone) that is rectified can be return...

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Abstract

The invention provides a method for preparing 4-hydroxy-4-methyl-2-pentanone. The method is characterized by comprising the following steps of: adding acetone into a distillation still and carrying out steam heating to obtain acetone steam; cooling the acetone steam to 0-40 DEG C by low-temperature chilled water; adding the cooled acetone steam into a reactor containing a catalyst to react; after the temperature of the distillation still reaches 120 DEG C through continuous distillation reactions, stopping reacting; and filling reaction liquid into the distillation still and separating the reaction liquid to obtain high-purity 4-hydroxy-4-methyl-2-pentanone. The method for preparing the 4-hydroxy-4-methyl-2-pentanone uses the acetone as a raw material and treated ion exchange resin and magnesium hydroxide as a mixed catalyst. Through the continuous distillation reactions, the reaction time is shorter, and more energy can be saved; side reactions are fewer, and the product quality is better. Moreover additives such as phosphoric acid and phthalic anhydride are not needed, thereby reducing environment hazards brought by a large quantity of alkali wastes.

Description

technical field [0001] The invention relates to a chemical production technology, in particular to a preparation method of 4-hydroxy-4-methyl-2-pentanone. Background technique [0002] 4-Hydroxy-4-methyl-2-pentanone, as a high-boiling organic solvent, is mainly used in electrostatic spray paint, cellulose grease paint, printing ink, solvent and paint remover for synthetic resin paint, insecticide, and bactericide Agents, wood preservatives, photographic film, rayon, artificial leather manufacturing, antifreeze, brake fluid and other fields. [0003] The synthesis of 4-hydroxy-4-methyl-2-pentanone is a classic ALDO (aldol condensation) reaction, which is formed by condensation of two molecules of acetone under the action of a catalyst. The synthetic method of reported 4-hydroxyl-4-methyl-2-pentanone mainly contains following several kinds at present: [0004] 1. The traditional method adopts solid sodium hydroxide or solid potassium hydroxide as a catalyst to realize. [0...

Claims

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Application Information

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IPC IPC(8): C07C49/17C07C45/73B01J31/08B01J21/10
Inventor 贺辙钱继新刘遗松李建东邵学青朱文杰严志杰陆继东
Owner CHANGSHU 3F ZHENFU NEW MATERIALS CO LTD
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