Preparation method of supercritical-carbon-dioxide thickening agent

A carbon dioxide and supercritical technology, applied in the field of preparation of anhydrous fracturing fluid and supercritical carbon dioxide thickener, can solve the problems of reservoir damage, affecting fracturing stimulation, reducing reservoir permeability, etc. The effect of improving dissolution

Active Publication Date: 2017-10-17
SOUTHWEST PETROLEUM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using conventional mining methods is easy to form water lock in the reservoir, and the permeability of the reservoir is reduced, which will cause damage to the reservoir and affect the effect of fracturing to increase production

Method used

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  • Preparation method of supercritical-carbon-dioxide thickening agent
  • Preparation method of supercritical-carbon-dioxide thickening agent
  • Preparation method of supercritical-carbon-dioxide thickening agent

Examples

Experimental program
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Embodiment 1

[0019] (1) Preparation of tert-butyl hydroxyethyl carbamate: Add 25ml of deionized water into the three-neck flask, then add 0.02mol ethanolamine, stir to dissolve completely, and then add 0.021mol di Di-tert-butyl carbonate, react at a constant temperature of 35 °C for 4 hours, add 30 mL of ethyl acetate to the solution for extraction, collect the upper organic phase, add anhydrous Na 2 SO 4 Dry, filter, and distill under reduced pressure to obtain the intermediate product (1) tert-butyl hydroxyethyl carbamate.

[0020] (2) Preparation of tert-butyl perfluorooctanoic acid ethyl carbamate: add tert-butyl hydroxyethyl carbamate and perfluorooctanoyl chloride to the three-neck flask, the molar ratio of tert-butyl hydroxyethyl carbamate perfluoro to octanoyl chloride 1:1.1, condensed and refluxed, heated to 75 ° C for 12 hours, added anhydrous ether, then added 5% NaOH solution, the solution was layered, extracted to obtain an organic phase, washed with distilled water several t...

Embodiment 2

[0024] (1) Preparation of tert-butyl hydroxyethyl carbamate: Add 25ml of deionized water into the three-necked flask, then add 0.02mol ethanolamine, stir to dissolve completely, and then add 0.023mol di Di-tert-butyl carbonate, react at a constant temperature of 35 °C for 4 hours, add 30 mL of ethyl acetate to the solution for extraction, collect the upper organic phase, add anhydrous Na 2 SO 4 Dry, filter, and distill under reduced pressure to obtain the intermediate product (1) tert-butyl hydroxyethyl carbamate.

[0025] (2) Preparation of tert-butyl perfluorooctanoic acid ethyl carbamate: add tert-butyl hydroxyethyl carbamate and perfluorooctanoyl chloride to the three-neck flask, the molar ratio of tert-butyl hydroxyethyl carbamate perfluoro to octanoyl chloride 1:1.2, condensed and refluxed, heated to 75°C and reacted for 12 hours, after adding anhydrous ether, then added 5% NaOH solution, the solution was layered, extracted to obtain an organic phase, washed with distil...

Embodiment 3

[0029] (1) Preparation of tert-butyl hydroxyethyl carbamate: Add 25ml of deionized water to the three-necked flask, then add 0.02mol ethanolamine, stir to dissolve completely, and then add 0.022mol di Di-tert-butyl carbonate, react at a constant temperature of 35 °C for 4 hours, add 30 mL of ethyl acetate to the solution for extraction, collect the upper organic phase, add anhydrous Na 2 SO4 Dry, filter, and distill under reduced pressure to obtain the intermediate product (1) tert-butyl hydroxyethyl carbamate.

[0030] (2) Preparation of tert-butyl perfluorooctanoic acid ethyl carbamate: add tert-butyl hydroxyethyl carbamate and perfluorooctanoyl chloride to the three-neck flask, the molar ratio of tert-butyl hydroxyethyl carbamate perfluoro to octanoyl chloride 1:1.1, condensed and refluxed, heated to 75 ° C for 12 hours, added anhydrous ether, then added 5% NaOH solution, the solution was layered, extracted to obtain an organic phase, washed with distilled water several tim...

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Abstract

The invention relates to a preparation method of a supercritical-carbon-dioxide thickening agent used for unconventional oil and gas reservoir development and aims to solve the problem that a conventional recovery method harms oil and gas reservoirs. According to the technical scheme, the method includes: adding deionized water into a bottle, adding ethanolamine, dropwise adding di-tert-butyl dicarbonate at 35 DEG C, performing reaction at 35 DEG C for 4 hours, and distilling to obtain an intermediate product (1) hydroxyethyl tert-butyl carbamate; adding the intermediate product (1) into a three-necked bottle, heating to 75 DEG C, dropwise adding perfluorooctanoyl fluoride, and performing reaction at 75 DEG C for 12 hours to obtain an intermediate product (2) ethyl perfluorooctanoate tert-butyl carbamate; adding dichloromethane and trifluoroacetic acid into the bottle, adding the intermediate product (2), performing reaction at 25 DEG C for 2 hours, performing extraction and vacuum drying, and adding 1, 6-hexamethylene diisocyanate to perform reaction for 10 minutes to obtain a final product (1, 6-diethyl perfluorooctanoate carbamido) hexane. The thickening agent can increase the viscosity of supercritical carbon dioxide and can be used for fracturing reformation and chemical reservoir oil displacement.

Description

technical field [0001] The invention relates to a water-free fracturing fluid technology for developing unconventional oil and gas reservoirs without using water, in particular to a preparation method of a supercritical carbon dioxide thickener containing fluorine element, and belongs to the field of oilfield chemicals. Background technique [0002] With the continuous development of the economy, oil and natural gas, as an energy reserve, are becoming more and more important. In recent years, my country's oil and natural gas production and imports have increased year by year. In 2014, my country's crude oil imports were 310 million tons, an increase of 9.5% over the same period of the previous year, and natural gas imports were 53 billion cubic meters. An increase of 23.8% over the same period last year. Conventional oil and gas resources can no longer meet the growing demand for oil and gas. Therefore, the development and utilization of unconventional oil and gas resources...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C273/18C07C275/10C09K8/62
CPCC07C269/04C07C269/06C07C273/18C09K8/62C07C275/10C07C271/16Y02P20/54
Inventor 周明补军成赵金洲黄洲邹佳汐陈意萍
Owner SOUTHWEST PETROLEUM UNIV
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