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A kind of preparation method of crosslinking agent and crosslinking controllable high temperature resistant gel

A technology of cross-linking agent and trimethylol phenol, which is applied in the field of preparation of cross-linking agent and cross-linking controllable high-temperature resistant gel, which can solve the problems of uncontrollable cross-linking time, weak gel strength, and poor temperature resistance , to achieve control of cross-linking time, good water solubility and good cross-linking effect

Inactive Publication Date: 2016-06-22
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The invention provides a cross-linking agent and a composite cross-linking system gel to solve the problems of poor temperature resistance of the gel system, weak gel strength and uncontrollable cross-linking time in the prior art.

Method used

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  • A kind of preparation method of crosslinking agent and crosslinking controllable high temperature resistant gel
  • A kind of preparation method of crosslinking agent and crosslinking controllable high temperature resistant gel
  • A kind of preparation method of crosslinking agent and crosslinking controllable high temperature resistant gel

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] A 250ml three-neck flask equipped with a thermometer and mechanical stirring was placed in a water bath, and the temperature of the water bath was set at 65°C. Add 15.03g (0.16mol) of phenol, 40.02g (0.49mol) of 37% formaldehyde solution, and 0.054g of ethylenediamine into the flask, stir well and raise the temperature to 70°C. The reaction process is observed by TLC, and trimethylol is completely formed For base phenol, add 0.085g cetyltrimethylammonium chloride, 14.82g (0.16mol) epichlorohydrin, slowly add 16g 40% NaOH (0.16mol) aqueous solution dropwise, and raise the temperature to 90°C for 2 hours after the dropwise addition , naturally cooled to obtain 84.09 g of water-soluble, transparent light yellow crosslinking agent. Polyacrylamide (PAM) with a molecular weight of 7 million and a degree of hydrolysis of 25% was prepared with 3.5% saline to a concentration of 0.6wt% and 0.7wt%, and the obtained trimethylolphenol glycidyl ether was added to crosslink agents an...

Embodiment 2

[0042] The molecular weight is 7,000,000, the degree of hydrolysis is the PAM of 25%, is prepared as the concentration of 0.4wt% and 0.5wt% with the brine of mass fraction 3.5%, adds the obtained trimethylolphenol glycidyl ether cross-linking agent and cross-linking agent of example 1 joint accelerator. The degree of gel crosslinking was characterized by gel viscosity and GelStrengthCodes method. The viscometer is: NDJ-1B rotational viscometer, 4# rotor 6rpm, the measurement is at room temperature, and the maximum temperature resistance temperature is the highest temperature at which the gel does not appear water separation after 24h high temperature treatment.

[0043] Table 2

[0044]

[0045] It can be seen from Table 2 that when the PAM concentration is 0.4wt% and 0.5wt%, the gel strength after crosslinking can reach the low deformation and non-flowing glue H grade and the rigid glue I grade, and the temperature resistance temperature can be above 180°C. This is much ...

Embodiment 3

[0047] The molecular weight is 7,000,000, and the degree of hydrolysis is 25% PAM, is prepared as the concentration of 0.2wt% and 0.3wt% with the brine of mass fraction 3.5%, adds the obtained trimethylolphenol glycidyl ether cross-linking agent and cross-linking agent of example 1 joint accelerator. The degree of gel crosslinking was characterized by gel viscosity and GelStrengthCodes method. The viscometer is: NDJ-1B rotational viscometer, 4# rotor 6rpm, the measurement is at room temperature, and the maximum temperature resistance temperature is the highest temperature at which the gel does not appear water separation after 24h high temperature treatment.

[0048] table 3

[0049]

[0050] It can be seen from Table 3 that when the concentration of PAM is reduced to 0.2wt% and 0.3wt%, the gel strength after crosslinking can reach grade G of non-flowing medium-deformation glue and grade H of low-deformation glue, which have good strength and temperature resistance The te...

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Abstract

The invention discloses a crosslinking agent and a preparation method of a crosslinking controllable high-temperature-resistant gel. The crosslinking agent is prepared through the synthetic steps of sequentially adding phenol and a formaldehyde solution into a reaction kettle in a weight ratio of 1:(3.0-3.1), uniformly stirring the obtained mixture, adding an ethylenediamine catalyst into the reaction kettle, and heating the obtained mixture in an oil bath at a temperature of 65-70 DEG C; in the process of reaction, detecting and observing the mixture by using the TLC (Thin-Layer Chromatography), and when trimethylol phenol is completely generated, sequentially adding hexadecyl trimethyl ammonium chloride, epichlorohydrin and a NaOH solution into the reaction kettle; heating the obtained product to 90 DEG C, and reacting for 2 hours. The gel is prepared from the following components in percentage by mass: (1) 0.2-0.7% of polyacrylamide; (2) 0.2-0.6% of a crosslinking agent, namely trimethylolpropane triglycidyl ether; (3) 50-200 ppm of a polyamine crosslinking promoter; (4) the balance of water. According to the invention, the crosslinking agent, namely trimethylolpropane triglycidyl ether, and the polyamine crosslinking promoter are introduced into a gel system for the first time, and the crosslinking promoter can effectively adjust the crosslinking time and promote the gel for further crosslinking so as to increase the strength of the gel, so that a gel which is controllable in crosslinking time, high in strength and high in temperature resistance is obtained.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a crosslinking agent and a method for preparing a crosslinking controllable high temperature resistant gel. Background technique [0002] Heavy oil is also called heavy crude oil or high-viscosity crude oil (heavy oil in English), and its viscosity is generally higher than 100mPa.s at the oil reservoir temperature. It is estimated that the total amount of conventional oil resources in the world is 300 billion tons. In addition, there are more than 80 million tons of unconventional oil resources such as heavy oil, oil sands and oil shale. These will become important sources of oil in the 21st century. According to relevant reports, my country's heavy oil reserves rank seventh in the world, and nine large and medium oil-bearing basins and a large number of heavy oil reservoir blocks have been discovered so far. Therefore, the exploitation of heavy oil will become a major...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D301/28C07D303/26C08J3/24C08L33/26
CPCC07D301/28C07D303/26C08J3/24C08J2333/26C08K5/1515C08L2201/08C08L2201/54C08L33/26
Inventor 张晓云张思思武继辉吴伟陈文婷周同娜
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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