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High-temperature guanidine gum cross-linking agent and preparation method thereof

A technology of cross-linking agent and guar gum, which is applied in the field of high-temperature guar gum cross-linking agent and its preparation, to achieve the effects of excellent temperature resistance and shear resistance, small amount of residue of gel-breaking liquid and surface tension, and short gel-breaking time

Inactive Publication Date: 2017-04-26
CHONGQING UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are few domestic reports on organoboron-zirconium guanidine crosslinking agents that can withstand 180°C. The present invention intends to improve the ultra-high temperature resistance of organoboron-zirconium crosslinking agents by introducing ligands with high temperature resistance during synthesis.

Method used

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  • High-temperature guanidine gum cross-linking agent and preparation method thereof
  • High-temperature guanidine gum cross-linking agent and preparation method thereof
  • High-temperature guanidine gum cross-linking agent and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] The synthesis of embodiment 1 organoboron crosslinking agent (BOC)

[0056] Dissolve a certain amount of borax in the organic solvent according to the proportioning ratio (the solvent is a mixed solution of glycerol and water), add the basic catalyst NaOH, set the first reaction temperature, add the ligand polyhydric alcohol after the first reaction time, set The second reaction temperature, after the second reaction time, adjust the pH value to 7-8 to obtain a colorless and transparent solution, that is, an organoboron crosslinking agent (BOC).

[0057] The main factors affecting the synthesis of organoboron crosslinking agent are: the amount of sodium tetraborate, the amount of ligand, the amount of glycerol, and the second reaction temperature. In the case of constant experimental conditions, a single control variable was used to investigate the effects of different variables on the appearance and performance of organoboron crosslinking agents, and to determine the o...

Embodiment 2

[0081] The synthesis of embodiment 2 organic zirconium crosslinking agent (ZOC)

[0082] Dissolve a certain amount of zirconium oxychloride in an organic solvent according to the proportion, add an acidic catalyst, set the first reaction temperature, add the ligand polyhydric alcohol after the first reaction time, set the second reaction temperature, and the second reaction time ends Finally, adjust the pH value to 3-5 to obtain a light yellow transparent solution, which is the organic zirconium crosslinking agent (ZOC).

[0083] The four main factors affecting the synthesis of organic zirconium crosslinking agent are: the amount of zirconium oxychloride, the amount of ligand, the first reaction temperature and the reaction time. Orthogonal experiment to prepare organic zirconium crosslinking agent.

[0084] (1) The amount of zirconium oxychloride

[0085] Under the same experimental conditions, 70% solvent (glycerol: water (v:v) = 1:3), lactic acid-citric acid mixture (the ...

Embodiment 3

[0129] The synthesis of embodiment 3 organic boron zirconium crosslinking agent

[0130] Under the conditions of maintaining the concentration of the modified guar gum base solution at 0.7%, the pH value at 10-11, 0.6% sodium thiosulfate, and the cross-linking ratio of 100:0.6, the effect of different boron-zirconium ratios on the jelly was investigated. The influence of temperature resistance and shear resistance of glue. Anton Paar rheometer was used to measure its temperature resistance and shear resistance, and the shear rate was 170s -1 , the temperature is 160°C, observe the final viscosity of the jelly after continuous shearing for 30 minutes, and record the data for graph analysis, the results are as follows figure 1 shown. figure 1 For different BOC:ZOC values ​​at the same heating rate with the change of shear time and the influence of crosslinking time, according to the curve, the temperature resistance of the crosslinking agent decreases with the increase of BOC:...

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Abstract

The invention discloses a high-temperature guanidine gum cross-linking agent and a preparation method thereof. A preparation process of the guanidine gum cross-linking agent includes steps: preparing an organic boron cross-linking agent and an organic zirconium cross-linking agent, and well mixing according to a volume ratio of 0.15-0.2:1 to obtain an organic boron-zirconium cross-linking agent. The guanidine gum cross-linking agent is excellent in temperature resistance and shear resistance, gum viscosity measured by a HAAKE rheometer is still kept to be 100mPa.s or above after shearing of a cross-linking system for 2h at 180 DEG C and 170s<-1>, and ultrahigh-temperature-resistant guanidine gum cross-linking agent BZC and GHPG cross-linked gel is excellent in temperature resistance and shear resistance; the researched organic boron-zirconium cross-linking agent is capable of retarding cross linking for 1-4min; the cross-linking agent is excellent in gel breaking performance, short in gel breaking time and low in gel breaking liquid residue quantity and surface tension.

Description

technical field [0001] The invention relates to the petroleum field, in particular to a high-temperature guar gum crosslinking agent and a preparation method thereof. Background technique [0002] In the field of exploration, due to deep burial and low formation permeability of deep ultra-high temperature reservoirs, fracturing is the main development method to improve such reservoirs, and high temperature resistant guar gum fracturing fluid is one of the commonly used fracturing fluids. Commonly used crosslinking agents for high-temperature guar gum suitable for deep formation fracturing include borate, metal antimony, aluminum, titanium, zirconium, organic boron, and organic zirconium. Titanium and zirconium have better heat resistance effects, but titanium has certain toxicity and has Not suitable for environmental protection requirements. [0003] Regarding the research and development of crosslinking agents, as early as 1967, Chrisp studied the crosslinking effect of t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K8/68C09K8/90
CPCC09K8/685C09K8/887C09K8/905
Inventor 黄文章沈丽嵇承红向林李林邓磊
Owner CHONGQING UNIVERSITY OF SCIENCE AND TECHNOLOGY
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