Process for preparing alkylphenol formaldehyde oligomer sulfonate

A technology of sulfonate and alkylphenol, applied in the field of preparing alkylphenol formaldehyde oligomer sulfonate, can solve the problems of long reaction time, loss of crosslinking reaction, time-consuming and energy consumption, etc., to simplify post-processing method, the effect of improving catalytic activity and shortening the operating cycle

Inactive Publication Date: 2013-12-04
CHINA RES INST OF DAILY CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If sulfuric acid is used as a catalyst, because its dehydration is too strong, the condensation polymer will lose its active -OH group due to intramolecular dehydration, thus losing the ability of crosslinking reaction
In addition, inorganic acid catalysts such as hydrochloric acid and sulfuric acid all have the defects of corroding equipment and polluting the environment
[0009] 3. For organic acid catalysts such as oxalic acid, because of its weak acidity, the reaction between nonylphenol and formaldehyde is mild, takes a long time, and consumes a lot of energy
[0010] 4. For solid acid catalysts, the preparation process requires high-temperature calcination, which consumes time and energy
[0011] 5. The above reports are polycondensation first and then decompression to remove water. There are many process steps, large equipment investment, long reaction time and low yield.
The solvent and water are removed by vacuuming, the viscosity of the system increases, and post-processing is troublesome

Method used

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  • Process for preparing alkylphenol formaldehyde oligomer sulfonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Embodiment 1: in the reactor with thermometer, stirrer, condenser, add C 8 Linear alkyl phenol, catalyst linear dodecyl benzene sulfonic acid, the amount of catalyst is 0.1% of the mass of the alkyl phenol, after the stirring is turned on and heated to 30 ° C, 50% of the total injection mass of formaldehyde is added dropwise, and the stirring is continued. After warming up to a reaction temperature of 60° C., the remaining formaldehyde was added, and the molar ratio of alkylphenol to formaldehyde was 1:0.5, and the reaction was continued for 240 min at this reaction temperature. After the reaction, the reaction product was adjusted to pH 7.5 by adding an aqueous sodium hydroxide solution, and finally a yellow-brown colloidal substance, namely an alkylphenol formaldehyde oligomer, was obtained.

[0037] Add the alkylphenol formaldehyde oligomer to the reaction kettle with thermometer, stirrer and condenser, add isooctane to dissolve, turn on stirring and heat to 30℃, add...

Embodiment 2

[0038] Embodiment 2: in the reactor with thermometer, stirrer, condenser, add C 9Branched alkyl phenol, catalyst p-toluenesulfonic acid, the amount of catalyst is 10.0% of the mass of the alkyl phenol, after the stirring is turned on and heated to 50 ° C, 60% of the total injection mass of paraformaldehyde is added dropwise, and the temperature is continued to stir until the reaction is carried out. After the temperature is 120°C, the remaining paraformaldehyde is added, and the molar ratio of the alkylphenol to the formaldehyde in the paraformaldehyde is 1:5, and the reaction is continued for 30 minutes at this reaction temperature. After the reaction is completed, the pH of the reaction product is adjusted to be 6.5 by adding an aqueous sodium hydroxide solution, and finally a yellow-brown colloidal substance, namely an alkylphenol formaldehyde oligomer, is obtained.

[0039] Add the alkylphenol formaldehyde oligomer into the reaction kettle with thermometer, stirrer and con...

Embodiment 3

[0040] Embodiment 3: in the reactor with thermometer, stirrer, condenser, add C 12 Branched alkylphenol, catalyst isobutylnaphthalenesulfonic acid, the catalyst dosage is 5.0% of the mass of the alkylphenol, after turning on stirring and heating to 40 ° C, 80% of the total injection mass of formaldehyde is added dropwise, and stirring is continued to heat up until the reaction After the temperature is 80°C, the remaining formaldehyde is added, and the molar ratio of alkylphenol to formaldehyde is 1:1.5, and the reaction is continued for 90 minutes at this reaction temperature. After the reaction, the reaction product was adjusted to pH 7.3 by adding an aqueous sodium hydroxide solution to obtain a yellow-brown colloidal substance, namely an alkylphenol formaldehyde oligomer.

[0041] Add the alkylphenol formaldehyde oligomer to the reactor with thermometer, stirrer and condenser, add dichloromethane to dissolve, turn on stirring and heat to 50℃, then add an appropriate amount ...

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Abstract

The invention discloses a process for preparing alkylphenol formaldehyde oligomer sulfonate. The process comprises the following steps of: adding alkylphenol and a catalyst into a reaction kettle, heating with stirring, dripping a formaldehyde solution or paraformaldehyde, continuously stirring, and raising temperature to reaction temperature, adding residual formaldehyde solution or paraformaldehyde, continuously reacting, and after reaction is finished, adding a sodium hydroxide aqueous solution to adjust pH of a reaction product to be 6.5 to 8.0 to obtain alkylphenol formaldehyde oligomer; and adding the alkylphenol formaldehyde oligomer into the reaction kettle, adding a solvent to dissolve, opening a stirrer, stirring and heating to 30 to 80 DEG C, adding a sulfonating agent, continuously reacting for 30 to 90 minutes, neutralizing a sulfonating product by using alkali until pH is 7 to 8, and evaporating to remove the solvent to obtain the alkylphenol formaldehyde oligomer sulfonate. The process has the advantages that alkylphenol and formaldehyde are used as raw materials, the process is simple, and industrialization is easy to realize.

Description

technical field [0001] The invention relates to a process for preparing alkylphenol formaldehyde oligomer sulfonate by reacting alkylphenol with formaldehyde. Background technique [0002] Oligomeric surfactants are two or more common single-chain surfactant molecules that are linked together by chemical bonds with a spacer group at or near the hydrophilic group. Those with two, three, or four amphiphilic components in the molecule are called oligomeric surfactants such as dimeric, trimeric, and tetrameric, respectively. Compared with traditional surfactants, oligomeric surfactants have lower critical micelle concentration, richer aggregation behavior and better properties, especially in tertiary oil recovery. [0003] At present, the research on oligomeric surfactants at home and abroad mainly focuses on dimeric surfactants, and the research on trimeric, tetrameric, pentameric surfactants with a slightly higher degree of polymerization mainly focuses on cationic or nonioni...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C303/06C07C309/42
Inventor 牛金平张文星韩亚明刘晓臣韩向丽
Owner CHINA RES INST OF DAILY CHEM IND
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