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Process for preparing alkylphenol formaldehyde oligomer sulfonate

A technology for producing sulfonate and alkylsulfonic acid, which is applied in the preparation of sulfonic acid and organic chemistry, can solve the problems of long reaction time, time-consuming and energy-consuming, loss of cross-linking reaction, etc., and achieve simplified post-processing methods and shortened Operation cycle, the effect of improving catalytic activity

Inactive Publication Date: 2012-07-18
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: add C in the reactor with thermometer, stirrer, condenser tube 8 Linear alkylphenol, catalyst linear dodecylbenzene sulfonic acid, the amount of catalyst is 0.1% of the mass of alkylphenol, start stirring and after heating to 30°C, add dropwise 50% of the total injection mass of formaldehyde, and continue stirring After heating up to the reaction temperature of 60°C, the remaining formaldehyde was added, the molar ratio of alkylphenol to formaldehyde was 1:0.5, and the reaction was continued for 240 minutes at the reaction temperature. After the reaction, the pH of the reaction product was adjusted to 7.5 by adding an aqueous solution of sodium hydroxide, and finally a yellowish-brown colloidal substance, ie, an alkylphenol formaldehyde oligomer, was obtained.

[0037] Add alkylphenol formaldehyde oligomers into the reaction kettle with thermometer, agitator, and condenser, add isooctane to dissolve, start stirring and add appropriate amount of oleum when ...

Embodiment 2

[0038] Embodiment 2: add C in the reactor with thermometer, stirrer, condenser tube 9Branched-chain alkylphenol, catalyst p-toluenesulfonic acid, the amount of catalyst is 10.0% of the mass of alkylphenol, after starting stirring and heating to 50°C, add dropwise 60% of the total injection mass of paraformaldehyde, continue to stir and heat up to the reaction After the temperature was 120°C, the remaining paraformaldehyde was added, and the molar ratio of the alkylphenol to the formaldehyde in the paraformaldehyde was 1:5, and the reaction was continued for 30 minutes at the reaction temperature. After the reaction, the pH of the reaction product was adjusted to 6.5 by adding an aqueous solution of sodium hydroxide, and finally a yellow-brown colloidal substance was obtained, ie, an alkylphenol formaldehyde oligomer.

[0039] Add alkylphenol formaldehyde oligomers into a reaction kettle with a thermometer, agitator, and condenser, add cyclohexane to dissolve, start stirring an...

Embodiment 3

[0040] Embodiment 3: add C in the reactor with thermometer, stirrer, condensation pipe 12 Branched chain alkylphenol, catalyst isobutyl naphthalene sulfonic acid, the amount of catalyst is 5.0% of the mass of alkylphenol, start stirring and after heating to 40°C, add dropwise 80% of the total injection mass of formaldehyde, continue to stir and heat up to the reaction The remaining formaldehyde was added after the temperature was 80°C, the molar ratio of alkylphenol to formaldehyde was 1:1.5, and the reaction was continued for 90 minutes at the reaction temperature. After the reaction was completed, the pH of the reaction product was adjusted to 7.3 by adding an aqueous sodium hydroxide solution, and finally a yellow-brown colloidal substance, ie, an alkylphenol formaldehyde oligomer, was obtained.

[0041] Add alkylphenol formaldehyde oligomers into the reaction kettle with thermometer, stirrer, and condenser, add dichloromethane to dissolve, start stirring and heat to 50°C, ...

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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 and formaldehyde. Background technique [0002] Oligomeric surfactants are two or more common single-chain surfactant molecules that are chemically bonded together by a spacer group near or near a hydrophilic group. Those with 2, 3 or 4 amphiphilic components in the molecule are respectively called dimeric, trimeric, tetrameric and other oligomeric surfactants. 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, and pentameric surfactants with a slightly higher degree of polymerization mainly focuses on cationic or nonionic surfactants. How...

Claims

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Application Information

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Patent Type & Authority Applications(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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