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Method for preparing fluorocarbon alkyl imidazonline through fixed bed catalytic reaction

A fluorocarbon-based imidazoline and fixed-bed reactor technology, which is applied in organic chemistry and other fields, can solve problems such as greater influence on product purity, difficult separation of catalysts, solvent recovery environment, etc., and achieve high single-pot yield and short reaction time Short and three-waste pollution effect

Inactive Publication Date: 2015-08-05
SHAANXI YANCHANG PETROLEUM GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to overcome the problems such as long reaction time, difficult separation of catalyst, great influence on product purity, or easy foaming in the reaction process, solvent recovery and environmental pollution in the existing preparation method of fluorocarbon alkyl imidazoline, the present invention proposes A method for the preparation of fluorocarbon-alkyl imidazolines by fixed-bed catalytic reaction using activated alumina molecular sieve-loaded phosphotungstic acid as a catalyst

Method used

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  • Method for preparing fluorocarbon alkyl imidazonline through fixed bed catalytic reaction
  • Method for preparing fluorocarbon alkyl imidazonline through fixed bed catalytic reaction
  • Method for preparing fluorocarbon alkyl imidazonline through fixed bed catalytic reaction

Examples

Experimental program
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Effect test

Embodiment 1

[0013] In a 500ml stainless steel preheating kettle (E-1) equipped with a thermometer, agitator and pressure gauge, add 100g of diethylenetriamine, heat to 30°C, add 252g of perfluorovaleric acid and stir evenly, heat up to 130°C and keep warm For 30 minutes, use the fixed bed feed pump (P-1) to pump the preheated liquid into the fixed bed reactor (E-2) filled with 7g of catalyst. The catalyst is activated alumina supported phosphotungstic acid catalyst, The pump (P-2) pumps the effluent material from the fixed bed reactor (E-2) into the receiving tank (E-4), and the flow rate of the feed pump and the reflux pump (P-1, P-2) is 30ml / min, the fixed-bed reactor (E-2) is heated by a heat conduction oil tank (E-5), and the reaction temperature (T) is controlled at 150-160°C. The top of the fixed bed reactor (E-2) is equipped with a condenser (E-3) and a vacuum device (I-1), and the material is circulated to the fixed bed reactor (E-2) through the vacuum device (I-1). 0~-0.03MPa v...

Embodiment 2

[0019] In a 500ml stainless steel preheating kettle (E-1) equipped with a thermometer, agitator and pressure gauge, add 100g of diethylenetriamine, heat to 30°C, add 299g of perfluorohexanoic acid and stir evenly, heat up to 132°C and keep warm For 30 minutes, use the fixed bed feed pump (P-1) to pump the preheated liquid into the fixed bed reactor (E-2) filled with 8g of catalyst. The catalyst is activated alumina supported phosphotungstic acid catalyst, The pump (P-2) pumps the effluent material from the fixed bed reactor (E-2) into the receiving tank (E-4), and the flow rate of the feed pump and the reflux pump (P-1, P-2) is 30ml / min, the fixed bed reactor (E-2) is heated by heat conduction oil (E-5), and the reaction temperature (T) is controlled at 150-160°C. The top of the fixed bed reactor (E-2) is equipped with a condenser (E-3) and a vacuum device (I-1), and the material is circulated to the fixed bed reactor (E-2) through the vacuum device (I-1). 0~-0.03MPa vacuum ...

Embodiment 3

[0021] In a 500ml stainless steel preheating kettle (E-1) equipped with a thermometer, agitator and pressure gauge, add 100g of diethylenetriamine, heat to 34°C, add 349g of perfluoroheptanoic acid and stir evenly, heat up to 130°C and keep warm For 30 minutes, use the fixed bed feed pump (P-1) to pump the preheated liquid into the fixed bed reactor (E-2) filled with 9g of catalyst. The catalyst is activated alumina supported phosphotungstic acid catalyst, The pump (P-2) pumps the effluent material from the fixed bed reactor (E-2) into the receiving tank (E-4), and the flow rate of the feed pump and the reflux pump (P-1, P-2) is 30ml / min, the fixed bed reactor (E-2) is heated by heat conduction oil (E-5), and the reaction temperature (T) is controlled at 150-160°C. The top of the fixed bed reactor (E-2) is equipped with a condenser (E-3) and a vacuum device (I-1), and the material is circulated to the fixed bed reactor (E-2) through the vacuum device (I-1). 0~-0.03MPa vacuum...

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Abstract

The invention relates to a method for preparing fluorocarbon alkyl imidazonline through fixed bed catalytic reaction. The method comprises taking perfluoro-carboxylic acid and polyethylene-polyamine at a mole ratio of acid to amide being 1 to 1.02-1 to1.1; adding the polyethylene-polyamine into a preheater, heating the polyethylene-polyamine to 30-35 DEG C, adding the perfluoro-carboxylic acid under stirring, increasing the temperature to 110-150 DEG C and performing heat preservation for 30-40 minutes; circulating preheated liquid through a fixed bed feeding pump and a fixed bed reflux pump at a reaction temperature of 150-160 DEG C; providing a vacuum degree of 0-0.03 MPa for a fixed bed, pumping out produced water, and after 4-6 hours' reaction, testing whether the content of a product is greater than 96% through the ultraviolet spectrophotometry, if so, determining that the product is qualified, wherein the obtained product is N-aminoethyl (or diethyltoluenediamine)-fluorocarbon alkyl imidazonline. The method for preparing the fluorocarbon alkyl imidazonline through fixed bed catalytic reaction has the advantages of being simple in process, free from solvent, stable in operation and control, short in reaction time, high in single-reactor yield and purity, low in three-waste pollution, environmentally friendly and easy to industrialize.

Description

technical field [0001] The invention relates to a preparation method of a fluorocarbon surfactant, which is mainly used for preventing metal equipment from being corroded by a corrosive medium in the process of high-temperature oil and gas field exploitation and petroleum refining. Fluorocarbon surfactants also have foaming properties and can be used in the field of foam fire extinguishing agents and foaming acids for natural gas development. In particular, the present invention relates to a method for preparing N-aminoethyl (or diethyldiamine)-perfluoroalkyl imidazoline compound by using fixed-bed catalytic reaction. Background technique [0002] As the oil field continues to be exploited, the down pressure of the oil well decreases and the production decreases, so the production will be increased through water injection pressurization and acidizing operations. Such production increase measures lead to a substantial increase in crude oil water content and corrosive media. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/24
CPCC07D233/24
Inventor 陈晓东侯雯雯陈君黄瑾杨惠玲
Owner SHAANXI YANCHANG PETROLEUM GRP
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