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Method for composing ethoxy quinoline

An ethoxyquinoline, synthesis reaction technology, applied in the direction of organic chemistry, etc., can solve the problems of long reaction time, low conversion rate per pass, low conversion rate, etc., and achieve low cost of raw materials, high conversion rate per pass, and fast reaction speed. Effect

Inactive Publication Date: 2004-08-11
宜兴市天石饲料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The deficiency that this technology exists is conversion rate is low, below 90%, needs to use toluene as solvent and water-carrying agent, and reaction time is long (48-50 hours), because single-pass conversion rate is low, needs to wash with soda ash, caustic soda, hydrochloric acid, water Only after post-processing can meet the quality requirements of the subsequent process (distillation), not only the cost is high, but also the amount of waste water and waste gas is large, and the pollution is serious

Method used

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  • Method for composing ethoxy quinoline
  • Method for composing ethoxy quinoline
  • Method for composing ethoxy quinoline

Examples

Experimental program
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Effect test

Embodiment 1

[0015] Catalyst manufacture: TiCl 4 Dissolve in ice water, neutralize with dilute ammonia water to PH=9-10 under cooling, age the resulting precipitate for 10 hours, filter, wash the filter cake, and dry at 110°C for 24 hours to obtain Ti(OH)4; take Ti( OH)4 powder, with 0.5-1M H 2 SO 4 Soak for 20 minutes, filter, then soak in 0.5M ammonium molybdate solution for 60 minutes, evaporate to dryness at 110-120°C, add acidic amorphous silica gel and stir until it can be granulated, and shape it to 20-30 mesh by a granulator, 500 The catalyst was calcined at ℃ for 3 hours.

[0016] see figure 2 As shown in the process flow diagram, 1 mole of p-aminophenethyl ether is mixed with 2.07 moles of acetone material and placed in a vertical fixed-bed reactor, which is filled with 70% of the reactor volume H 2 SO 4 -MoO 3 -TiO 2 Solid superacid catalyst, at a temperature of about 150°C and a pressure of about 0.1Mpa, the cyclization reaction is about 30 hours, and the product after t...

Embodiment 2

[0018] The manufacture method of catalyst is with embodiment 1.

[0019] 1 mole of p-aminophenethyl ether is placed in a vertical fixed bed reactor with 2.1 moles of acetone, and the reactor is filled with 78% volume of H 2 SO 4 -MoO 3 -TiO 2 Solid superacid catalyst, at a temperature of about 160°C and a pressure of about 0.08Mpa, the cyclization reaction is about 35 hours, and the product after the cyclization reaction can be filtered and distilled to obtain the finished product, of which 10% of the previous fraction is re-distilled to obtain The finished product, the re-distilled 5% front cut is circulated into the fixed bed reactor for cyclization reaction.

Embodiment 3

[0021] The manufacture method of catalyst is with embodiment 1.

[0022] 1 mole of p-aminophenethyl ether is mixed with 2.2 moles of acetone material and placed in a vertical fixed-bed reactor filled with 65% volume of H 2 SO 4 -MoO 3 -TiO 2 Solid superacid catalyst, at a temperature of about 120°C and a pressure of about 0.15Mpa, the cyclization reaction is about 25 hours, and the product after the cyclization reaction can be filtered and distilled to obtain the finished product, of which 10% of the previous fraction is re-distilled to obtain The finished product, the re-distilled 5% front cut is circulated into the fixed bed reactor for cyclization reaction.

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Abstract

A process for synthesizing ethoxy quinoline from p-aminobenzoether and acetone features that in the synthesizing reaction, the super-strong solid acid H2SO4-MoO3-TiO2 is used as its catalyst for high reaction speed and high transform rate.

Description

technical field [0001] The invention relates to a method for synthesizing ethoxyquinoline. technical background [0002] Ethoxyquinoline is currently the cheapest and most efficient feed antioxidant used in the largest amount. It is synthesized by using p-aminophenethyl ether and acetone as raw materials, using p-benzenesulfonic acid as a catalyst, and using toluene as a solvent and water-carrying agent. See Figure 1 for the flowchart. The deficiency that this technology exists is conversion rate is low, below 90%, needs to use toluene as solvent and water-carrying agent, and reaction time is long (48-50 hours), because single-pass conversion rate is low, needs to wash with soda ash, caustic soda, hydrochloric acid, water Only after post-treatment can meet the quality requirements of the subsequent process (distillation), not only the cost is high, but also the amount of waste water and waste gas is large, and the pollution is serious. Contents of the invention [0003] ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D215/20
Inventor 赵传江
Owner 宜兴市天石饲料有限公司
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