Method for preparing phenolic resin pre-condensation polymer cross-linking agent

A technology of phenolic resin and precondensation, which is applied in the direction of chemical instruments and methods, drilling compositions, etc., can solve the problems of unfavorable environmental protection, great harm to operators, and restricted use, and achieve low toxicity, good temperature resistance, and traffic good connection performance

Active Publication Date: 2010-06-16
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, resin crosslinking agents are mostly used as monomers of phenols and aldehydes, and the pH value needs to be adjusted with sodium bicarbonate or oxalic acid during use. Large, not conducive to environmental protection, restricting its use

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Cooling water is passed through the reaction kettle, and 120kg of phenol, 120kg of hydroquinone and 60kg of sodium hydroxide solution with a mass concentration of 40% are added to the reaction kettle; the mixer is turned on, the cooling water valve is adjusted, and the cooling degree is adjusted. The temperature in the reaction kettle is not high at 50°C; when the temperature no longer rises and is controlled below 40°C, add 80kg of urotropine to dissolve, then slowly add 620kg of formaldehyde, and pay attention to control the temperature in the reactor not to exceed 50°C when adding; after all materials are added Stir and react for 20-30 minutes, and discharge when the temperature no longer rises and tends to drop. After discharging, continue to observe the temperature change of the product. If there is a phenomenon of temperature rise, it should be cooled with cooling water in time.

[0015] The key to the whole synthesis process is to control the temperature in the re...

Embodiment 2

[0020] The reaction kettle is fed with cooling water, and 100kg of melted phenol, 100kg of hydroquinone and 50kg of sodium hydroxide solution with a mass concentration of 40% are added to the reaction kettle; the mixer is turned on, the cooling water valve is adjusted, the cooling degree is adjusted, and the reaction kettle is controlled. The internal temperature is not higher than 50°C; when the temperature no longer rises and is controlled below 40°C, add 50kg of urotropine to dissolve, then slowly add 550kg of formaldehyde and 150kg of remaining water. Over 50°C; after adding all the materials, stir and react for 20-30 minutes, and discharge the material when the temperature is no longer rising and has a tendency to fall. After discharging, continue to observe the temperature change of the product. If the temperature rises, it should be cooled in time Water cooling treatment.

[0021] The product obtained by the above steps, due to the low raw material addition ratio, the e...

Embodiment 3

[0023] The reaction kettle is fed with cooling water, and 150kg of melted phenol, 150kg of hydroquinone and 50kg of sodium hydroxide solution with a mass concentration of 40% are added to the reaction kettle; the mixer is turned on, the cooling water valve is adjusted, and the cooling degree is adjusted. The temperature shall not be higher than 50°C; when the temperature does not rise any more, when the temperature is below 40°C, add 100kg of urotropine to dissolve, then slowly add 550kg of formaldehyde, and pay attention to control the temperature in the reactor not to exceed 50°C when adding; Stir and react for 20 to 30 minutes after completion, and discharge the product when the temperature is no longer rising and tends to drop. After discharging, continue to observe the temperature change of the product. If there is a phenomenon of temperature rise, it should be cooled with cooling water in time.

[0024] The product that makes by above-mentioned steps, because phenol and u...

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Abstract

The invention provides a method for preparing phenolic resin pre-condensation polymer cross-linking agent, which takes phenol, hydroquinone, methanol, urotropine, 40% of sodium hydroxide solution and water as raw materials and comprises the following steps: introducing cooling water into a reaction kettle; adding 10-15% of phenol, 15-10% of hydroquinone and 5-10% of sodium hydroxide solution withmass concentration of 40%; starting a stirrer, opening a cooling water valve, adjusting the cooling temperature to be not higher than 50 DEG C; adding 5-10% of urotropine when the cooling temperatureis controlled below 40 DEG C, dissolving, adding 65-55% of methanol slowly when the temperature is controlled to be not higher than 50 DEG C; stirring and reacting for 20-30min after all the raw materials are added, discharging when the fact that the temperature rises without any fallout trend is observed to obtain the phenolic resin pre-condensation polymer cross-linking agent which has the advantages of simple use, low toxicity, environment protection, adjustable gelation time and temperature of jelly thereby, and good temperature tolerance.

Description

Technical field: [0001] The invention relates to an oil field chemical agent, especially a preparation method for preparing polymer jelly delay crosslinking agent. Background technique: [0002] Polymer jelly is a viscoelastic body formed by the cross-linking reaction between polymers in solution and cross-linking agents. Polymer jelly is widely used in oilfield profile control, water shutoff and tertiary oil recovery. The commonly used polymer is partially hydrolyzed polyacrylamide (relative molecular mass 5×10 6 ~12×10 6 , degree of hydrolysis 10% to 25%), commonly used cross-linking agents are high-valent metal ions (such as Cr 3+ 、Zr 4+ 、Al 3+ 、Ti 4+ etc.), aldehydes (such as formaldehyde, acetaldehyde, glyoxal, etc.) and resins (such as phenolic resins), etc. Different cross-linking agents can form different jelly, such as chromium jelly, zirconium jelly, aluminum jelly, titanium jelly, aldehyde jelly and resin jelly. Among them, the high-valent metal ion cross-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/24C08L33/26C08L61/06C09K8/44
Inventor 戴彩丽赵福麟
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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