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Method for producing pinacolone by using fluidized bed process

A pinaconone and fluidized bed technology, applied in the field of fluidized bed process production of pinaconone, can solve the problems of environmental pollution of waste catalysts and low production capacity, and achieve the advantages of improving competitiveness, simple production equipment and solving environmental protection problems. Effect

Active Publication Date: 2015-03-04
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to overcome the above-mentioned deficiencies of the prior art and provide a method for producing pinacolone with a fluidized bed process, which can effectively solve the problems of low production capacity and environmental pollution caused by waste catalysts

Method used

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  • Method for producing pinacolone by using fluidized bed process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] According to the titanium / aluminum / cerium molar ratio of 3:1:0.1, take 5000ml of aluminum nitrate, titanium tetrachloride and cerium nitrate to make a mixed solution, and use sodium hydroxide precipitant at 60°C and pH 7-8 Neutralization, washing the filter cake with water until the content of impurity ions is less than 0.1%, adding an appropriate amount of binder to the filter cake, and granulating by spray drying. The spray inlet temperature is 370±2°C, the outlet temperature is 185±2°C, and the average particle size of the catalyst is 85 microns.

[0016] Add 30g of the prepared catalyst into the reactor, the raw material pivalic acid, acetic acid / acetone molar ratio is 1:1.2, the reactor temperature is 410±2°C, and the space velocity is 0.7. Continuously react for 4 hours, take a sample every hour, and analyze the samples in the collector by chromatography.

[0017] The regenerator temperature is 520±2°C. Add 3.5% (volume percent) methanol to the air. The air flo...

Embodiment 2

[0019] According to the titanium / aluminum / cerium molar ratio of 3:1.5:0.5, take 5000ml of aluminum sulfate, titanium sulfate and cerium nitrate to make a mixed solution, and neutralize it with the precipitant sodium carbonate at 670°C and pH 7-8. The filter cake is washed with water until the content of impurity ions is less than 0.1%, and an appropriate amount of binder is added to the filter cake, and the filter cake is granulated by spray drying. The spray inlet temperature is 370±2°C, the outlet temperature is 185±2°C, and the average particle size of the catalyst is 75 microns.

[0020] Add 30g of the prepared catalyst into the reactor, the raw material pivalic acid, acetic acid / acetone molar ratio is 1:1.2, the reactor temperature is 410±2°C, and the space velocity is 0.8h -1 . Continuously react for 4 hours, take a sample every hour, and analyze the samples in the collector by chromatography.

[0021] The regenerator temperature is 520±2°C. Add 3.5% (volume percent) ...

Embodiment 3

[0023] According to the titanium / aluminum / cerium molar ratio of 3:1.5:0.1, take 5000ml of aluminum nitrate, titanium tetrachloride and cerium nitrate to make a mixed solution, and make a mixed solution with the precipitating agent sodium hydroxide at 70°C and pH 7-8. Neutralization, washing the filter cake with water until the content of impurity ions is less than 0.1%, adding an appropriate amount of binder to the filter cake, and granulating by spray drying. The spray inlet temperature is 370±2°C, the outlet temperature is 185±2°C, and the average particle size of the catalyst is 70 microns.

[0024] Add 30g of the prepared catalyst into the reactor, the raw material pivalic acid, acetic acid / acetone molar ratio is 1:1.2, the reactor temperature is 405±2°C, and the space velocity is 0.7h -1 . Continuously react for 4 hours, take a sample every hour, and analyze the samples in the collector by chromatography.

[0025] The regenerator temperature is 530±2°C. Add 4.5% (volum...

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Abstract

The invention discloses a method for producing pinacolone by using a fluidized bed process. The method is characterized by comprising the following steps: preparing a mixed solution by using a soluble aluminum source, a soluble titanium source and a soluble cerium source according to the condition that the mole ratio of titanium to aluminum to cerium is 3:(1-1.5):(0.1-0.5), adding a precipitating agent to neutralize the mixed solution at the temperature of 60-70 DEG C and at a pH value of 7-9, washing a filter cake by water until the content of impurity ions is smaller than 0.1%, adding an adhesive into the filter cake and performing spray-drying for granulation; adding a catalyst of which the average grain size is 70-90 micrometers into a fluidized bed reactor and controlling the reaction conditions as follows: raw materials comprise trimethylacetic acid and acetic acid / acetone, the mole ratio of the trimethylacetic acid to the acetic acid / acetone is 1:1.2, the reaction temperature is 400-420 DEG C, the airspeed is 0.7-0.8h<-1>, and the yield of the product pinacolone is 48%-50%; and controlling the regeneration temperature of the catalyst in a regenerator at 500-550 DEG C, controlling the air flow speed at 30ml / min, and adding 3-5v% of methanol and water into the air to regenerate the catalyst so as to realize continuous production of pinacolone, wherein no waste catalyst is generated during production, moreover the procedures of the production process are shortened, the energy consumption is low and the production cost is low.

Description

technical field [0001] The invention relates to the production field of pinacolone, in particular to a method for producing pinacolone by a fluidized bed process. Background technique [0002] Pinacolone, also known as 3,3-dimethyl-2-butanone, methyl tert-butyl ketone, is an important raw material for the synthesis of pesticides and medicines. With the continuous development of high-efficiency, low-toxicity, systemic, and broad-spectrum pesticides in my country in recent years, the amount of pinacolone is increasing, especially in azole pesticides such as triadimefon, triadimenol, and specific azoles. At present, the production of pinacolone mostly adopts the "fixed bed" method. Such as CN200710065585.5 "a method for synthesizing 3,3-dimethyl-2-butanone", the patent uses alumina as a carrier and a catalyst with rare earth elements as active components to prepare pina by a fixed bed method Ketone production process. CN200710177196.1 "A synthetic method for pinacolone", the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/04C07C45/72
CPCY02P20/584
Inventor 陈永生于海斌孙春晖张健刘伟许岩王梦迪
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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