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A kind of aqueous fluorescent tracer and preparation method thereof

A fluorescent tracer, water-based technology, applied in the field of fluorescent tracers, can solve the problems of unfavorable large-scale popularization and application, poor adaptability and selectivity, large amount of chemical tracers, etc., to achieve easy monitoring and analysis, good thermal stability , low-cost effect

Active Publication Date: 2019-10-11
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The amount of chemical tracers is usually large, the cost is high, the detection error is large, and the adaptability and selectivity are poor, the test resolution is low, and there are environmental and safety problems. Such tracers are gradually being eliminated; Tracers require professional construction personnel and use special equipment for testing. The analysis and testing methods are complicated and expensive, which is not conducive to large-scale promotion and application.

Method used

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  • A kind of aqueous fluorescent tracer and preparation method thereof
  • A kind of aqueous fluorescent tracer and preparation method thereof
  • A kind of aqueous fluorescent tracer and preparation method thereof

Examples

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Embodiment 1

[0044] This embodiment provides a kind of aqueous fluorescent tracer, the preparation of this aqueous fluorescent tracer comprises the following process:

[0045] 1) Mix 10.5 parts of salicylaldehyde, 21 parts of diethyl malonate, 50 parts of absolute ethanol, 0.8 parts of hexahydropyridine and 0.01 part of glacial acetic acid, stir and reflux at 78°C for 2 hours;

[0046] 2) Cool to room temperature after reflux, add 6 parts of cold water (the temperature of cold water is 5-25°C) to the reaction product, suction filter after crystallization, and cool with 1 part of ice water, and then use 60% ethanol with a mass fraction of Solution washed 2 times;

[0047] 3) Recrystallize with an ethanol solution with a mass fraction of 25%, and obtain the first product after drying;

[0048] 4) After mixing 2.2 parts of the first product above, 2 parts of potassium hydroxide, 20 parts of absolute ethanol and 10 parts of water, heat to 78°C and reflux for about 1.5 hours; pour the reaction p...

Embodiment 2

[0055] This embodiment provides a kind of aqueous fluorescent tracer, the preparation of this aqueous fluorescent tracer comprises the following process:

[0056] 1) Stir and reflux 10.5 parts of salicylaldehyde, 21 parts of diethyl malonate, 50 parts of absolute ethanol, 0.8 parts of hexahydropyridine and 0.01 part of glacial acetic acid at 78°C for 2 hours;

[0057] 2) Cool to room temperature after reflux, add 6 parts of cold water (the temperature of cold water is 5-25°C) to the reaction product, suction filter after crystallization, and cool with 1 part of ice water, and then use a mass fraction of 50% Wash with ethanol solution 3 times;

[0058] 3) Recrystallize with an ethanol solution with a mass fraction of 20%, and obtain the first product after drying;

[0059] 4) After mixing 2.2 parts of the above-mentioned first product, 2 parts of potassium hydroxide, 20 parts of absolute ethanol and 10 parts of water, heat to 75 and reflux for about 1.5 hours; pour the reactio...

Embodiment 3

[0066] This embodiment provides a kind of aqueous fluorescent tracer, the preparation of this aqueous fluorescent tracer comprises the following process:

[0067] 1) After mixing 10.5 parts of salicylaldehyde, 21 parts of diethyl malonate, 50 parts of absolute ethanol, 0.8 parts of hexahydropyridine and 0.01 part of glacial acetic acid, stir and reflux at 78°C for 2 hours;

[0068] 2) Cool to room temperature after reflux, add 6 parts of cold water to the reaction product (the temperature of cold water is 5-25 ° C), suction filter after crystallization, and cool with 1 part of ice water, and then use 45% ethanol with a mass fraction Solution washed 4 times;

[0069] 3) Recrystallize with an ethanol solution with a mass fraction of 30%, and obtain the first product after drying;

[0070] 4) Heat 2.2 parts of the first product above, 2 parts of potassium hydroxide, 20 parts of absolute ethanol and 10 parts of water to reflux at 80°C for about 1 hour; pour the reaction product i...

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Abstract

The invention provides an aqueous fluorescent tracer and a preparation method thereof. The aqueous fluorescent tracer has a chemical structure shown in the description; and R in the chemical structureis -SO3Na, -(CH2)2NH(CH2)2SO3Na, -Ph-SO3Na, -Ph-COOC2H2SO3H or a group with the formula being shown in the description. The preparation method of the aqueous tracer comprises the following steps: carrying out a condensation reaction on salicylaldehyde and diethyl malonate with piperidine as a catalyst to obtain a first product; carrying out a hydrolysis reaction on the first product under an alkaline condition to obtain a second product; and reacting the second product with aminosulfonate to prepare the aqueous fluorescent tracer. The aqueous fluorescent tracer has the advantages of good water solubility, low cost, non-toxicity, good chemical and biological stability, good thermal stability, simplicity in analysis operation, small dosage, high sensitivity, and convenience in monitoring.

Description

technical field [0001] The invention relates to a water-based fluorescent tracer and a preparation method thereof, belonging to the technical field of fluorescent tracers. Background technique [0002] For a long time, the most commonly used tracers in oilfield development mainly include chemical tracers and isotope tracers. Although they are widely used in various oil fields, they also have disadvantages of varying degrees: [0003] The amount of chemical tracers is usually large, the cost is high, the detection error is large, and the adaptability and selectivity are poor, the test resolution is low, and there are environmental and safety problems. Such tracers are gradually being eliminated; Tracers require professional construction personnel and use special equipment for testing. The analysis and testing methods are complicated and expensive, which is not conducive to large-scale promotion and application. [0004] At present, fluorescence technology has been widely us...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D311/12G01N21/64
Inventor 刘洪林卢德唐郑德温胡先海李清宇陈建军刘曼莉窦红波陈俊华董大忠刘建武张晓伟潘文鼎于荣泽
Owner PETROCHINA CO LTD
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