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Method for synthesizing aliphatic alcohol sulfate

A technology of fatty alcohol sulfate and synthesis method, which is applied in the direction of sulfate ester preparation and organic chemistry, and can solve the problems of inability to use intermittent equipment, dark product color, and many side reactions, etc., and achieve good biodegradability and excellent quality , the effect of simple equipment

Inactive Publication Date: 2008-08-06
王伟松
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Using sulfuric acid and oleum as sulfating reagents has many side reactions, the product has deep color, poor quality, and serious equipment corrosion; using sulfur trioxide as the sulfating reagent, although the product quality is guaranteed, the required equipment is complicated and cannot be used. Batch equipment production; using chlorosulfonic acid as the sulfation reagent, although good quality products can be obtained by reaction, a large amount of hydrogen chloride gas is produced during the reaction process, and the equipment corrosion is very serious

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Example 1: Add 10 mol of lauryl alcohol, 12 mol of sulfamic acid, and 5 mol of urea into a reaction kettle, feed in nitrogen, heat to 115-125° C., and keep warm for 1.5 hours. Then the temperature was raised to 130-135°C, and the reaction was kept for 2.0 hours. After the heat preservation is completed, the temperature is lowered to 80-90°C, and 30% potassium hydroxide solution is added dropwise for neutralization. After neutralization, degas for 2.0 hours at 75-85°C and vacuum degree ≥ 0.090MPa. After degassing, add 169mol deionized water to dilute, and stir at 75-85°C for 2.0h. Cool to 60-70°C and discharge to obtain a light yellow transparent liquid with a content of 50%, which is potassium lauryl sulfate.

[0019] The chemical equation of sulfation reaction in the above-mentioned implementation is:

[0020] (H 2 N) 2 CO

[0021] C 12 h 25 OH+H 2 NSO 3 +KOH→C 12 h 25 OSO 3 K+NH 3 +H 2 o

Embodiment 2

[0022] Example 2: Add 10 mol of octadecyl alcohol, 18 mol of sulfamic acid, and 8 mol of urea into a reaction kettle, feed nitrogen, heat to 120-130° C., and keep warm for 1.5 hours. Then the temperature was raised to 135-140°C, and the temperature was kept for 2.0 hours. After the heat preservation is completed, the temperature is lowered to 80-90°C, and 40% sodium hydroxide solution is added dropwise for neutralization. After neutralization, degas for 2.0 hours at 75-85°C and vacuum degree ≥ 0.090MPa. After degassing, add 482mol deionized water to dilute, and stir at 75-85°C for 2.0h. Cool to 60-70 DEG C and discharge, and obtain a light yellow paste with a content of 30%, which is sodium stearyl sulfate.

Embodiment 3

[0023] Example 3: Add 10 mol of octanol, 11 mol of sulfamic acid, and 3 mol of urea into a reaction kettle, feed nitrogen, heat to 110-120° C., and keep warm for 1.5 hours. Then the temperature was raised to 125-130°C, and the temperature was kept for 2.0 hours. After the heat preservation is completed, the temperature is lowered to 80-90°C, and 50% potassium hydroxide solution is added dropwise for neutralization. After neutralization, degas for 2.0 hours at 75-85°C and vacuum degree ≥ 0.090MPa. After degassing, add 59mol deionized water to dilute, and stir at 75-85°C for 2.0h. Cool to 60-70°C and discharge to obtain a light yellow paste with a content of 70%, which is potassium octyl sulfate.

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PUM

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Abstract

A synthesis method of fatty alcohol sulfate belongs to the synthesis technical field of sulfate-type anion surface activator of organic chemistry. The invention uses fatty alcohol as raw material, which is characterized in that the invention uses sulfamic acid as sulfation agent and uses urea as catalyst to process sulfation reaction on fatty alaochol and sulfamic in the catalytic presence of urea and nitrogen gas protection, neutralizes via alkali solution, vacuums to remove generated ammonia gas and dilutes via water to prepare fatty alcohol sulfate, wherein the mol ratio of fatty alcohol and sulfamic acid is 1:1.0-2.0 and the mol ratio of fatty alcohol and catalyst urea is 1:0.2-1.0. The invention reasonably utilizes sulfamic as sulfation agent and urea as catalyst to process sulfation modification on fatty alcohol to synthesize fatty alcohol sulfate, with simple process, less side reaction, mild reaction condition and simple device, which is suitable for intermittent production with less device investment.

Description

technical field [0001] The invention relates to a synthesis method of fatty alcohol sulfate, which belongs to the technical field of synthesis of sulfate-type anionic surfactants in organic chemistry. Background technique [0002] Sulfation generally refers to the introduction of sulfate groups (-SO 3 H) Response. The new bond formed by the reaction is a C-O-S bond. In industrial production, sulfation reagents usually use sulfur trioxide, sulfuric acid, oleum, chlorosulfonic acid, etc. [0003] Using sulfuric acid and oleum as sulfating reagents has many side reactions, the product has deep color, poor quality, and serious equipment corrosion; using sulfur trioxide as the sulfating reagent, although the product quality is guaranteed, the required equipment is complicated and cannot be used. Batch type equipment production; using chlorosulfonic acid as the sulfation reagent, although products with better quality can be reacted, a large amount of hydrogen chloride gas is pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C305/04C07C303/24
Inventor 王伟松王新荣孟照平李福强
Owner 王伟松
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