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Preparation method for high-temperature delay type organic zirconium cross-linking agent

A technology of zirconium crosslinking agent and high temperature stabilizer, applied in the field of fine chemical preparation technology, can solve problems such as poor temperature resistance, and achieve the effects of low formation damage rate, good development prospects and good filtration performance

Inactive Publication Date: 2011-05-04
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the disadvantages of poor heat resistance of existing crosslinking agents, and to provide a method for preparing an organic zirconium crosslinking agent with good temperature resistance, crosslinking performance and high temperature delay

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Example 1: 1) First, fully dissolve zirconium oxychloride in water and add it to the reactor, and heat the reactor to 80° C., then add lactic acid to the reactor, adjust the pH value to 6 with NaOH, at 80 ℃ constant temperature reaction for 5 hours to form A; wherein the mass ratio of zirconium oxychloride, water, and lactic acid is 1:8:2;

[0013] 2) adding triethanolamine, pyrrolidone and A to react, the reaction temperature is 80° C., and the reaction time is 1 hour to obtain B; wherein the mass ratio of triethanolamine, pyrrolidone and A is 15:1:40;

[0014] 3) Keep the temperature constant, add sorbitol to B, react for 0.5h, add KCl under high-speed stirring, and react at constant temperature for 1h to obtain a clear and transparent orange solution C; wherein the mass ratio of sorbitol, KCl and B is 5:1 : 40;

[0015] 4) Filter through a sieve to remove the KCl residue, and then the orange transparent high-temperature delayed organic zirconium crosslinking agent D...

Embodiment 2

[0016] Example 2: 1) First, fully dissolve zirconium tetrachloride in water and add it to the reactor, and heat the reactor to 83°C, then add acetic acid to the reactor, adjust the pH value to 5.5 with NaOH, at 83 ℃ constant temperature reaction for 4 hours to form A; wherein the mass ratio of zirconium tetrachloride, water, and acetic acid is 1:6:1.3;

[0017] 2) adding triethanolamine, pyrrolidone and A to react, the reaction temperature is 60° C., and the reaction time is 4 hours to obtain B; wherein the mass ratio of triethanolamine, pyrrolidone and A is 15:1:43;

[0018] 3) Keeping the temperature constant, add mannitol to B, react for 1h, add KCl under high-speed stirring, and react at constant temperature for 1.5h to obtain a clear and transparent orange solution C; the mass ratio of mannitol, KCl and B is 5:1 : 43;

[0019] 4) Filter through a sieve to remove the KCl residue, and then the orange transparent high-temperature delayed organic zirconium crosslinking agent...

Embodiment 3

[0020] Example 3: 1) First, fully dissolve zirconium oxychloride in water and add it to the reactor, and heat the reactor to 87°C, then add the mixture of lactic acid and acetic acid to the reactor, and adjust the pH value with NaOH To 6.5, react at a constant temperature of 87 ° C for 3 hours to form A; wherein the mass ratio of the mixed solution of zirconium oxychloride, water, lactic acid and acetic acid is 1:5:1;

[0021] 2) adding triethanolamine, pyrrolidone and A to react, the reaction temperature is 68°C, and the reaction time is 3 hours to obtain B; wherein the mass ratio of triethanolamine, pyrrolidone and A is 15:1:48;

[0022] 3) Keep the temperature constant, add sorbitol to B, react for 0.5h, add KCl under high-speed stirring, and react at constant temperature for 1h to obtain a clear and transparent orange solution C; wherein the mass ratio of sorbitol, KCl and B is 5:1 : 48;

[0023] 4) Filter through a sieve to remove the KCl residue, and then the orange tra...

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Abstract

The invention discloses a preparation method for a high-temperature delay type organic zirconium cross-linking agent. The preparation method comprises the following steps of: sufficiently dissolving inorganic zirconium salt in water and adding a proper amount of organic acid; under the catalytic action of NaOH, controlling the pH value of the system and raising the temperature and reacting to obtain organic acid-zirconium prepolymer; keeping the temperature constant, adding a ligand and a cross-linking shielding agent into the organic acid-zirconium-prepolymer to perform reaction; continuously keeping the temperature constant, adding polyalcohol and a high-temperature stabilizing agent, adjusting the pH value and reacting at constant temperature; removing the high-temperature stabilizing agent residue after reaction is finished so as to obtain the modified clarified transparent high-temperature delay type cross-linking agent. The aqueous fracturing fluid prepared by the invention has good shear resistance, good sand carrying property and wide application prospect, greatly enhances the heat resistance property, reduces the use cost and relieves damage to the stratum environment.

Description

technical field [0001] The invention belongs to the field of preparation technology of fine chemicals, and in particular relates to a preparation method of a high-temperature delayed organic zirconium crosslinking agent. Background technique [0002] With the deepening of exploration and development of oil and gas fields, the depth of a single well is constantly refreshed. The domestically developed organic boron crosslinking agents generally have a temperature resistance of no more than 130°C. In order to meet the high temperature resistance requirements of fracturing fluids in the deep reservoir stimulation process, the development of high-temperature delayed fracturing fluid systems is imminent. Many water-soluble polymers, such as biopolymers, various plant gum polysaccharides and their hydroxyalkyl, hydroxyalkylcarboxyalkyl derivatives, are cross-linked by multivalent metal ions in low-concentration aqueous solutions to form gels, It is widely used in oil and gas field...

Claims

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Application Information

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IPC IPC(8): C09K8/62
Inventor 李小瑞魏向博赵秀波赖小娟王磊马少云李刚辉
Owner SHAANXI UNIV OF SCI & TECH
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