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Process for preparing fatty acid ester sulfonate

A technology for ester sulfonate and fatty acid, which is applied in the field of preparing fatty acid ester sulfonate, can solve the problems of thickening of liquid film, easy explosion and high viscosity, and achieves strong low temperature washing ability, good hard water resistance and low temperature water solubility. good effect

Active Publication Date: 2014-03-26
中轻化工绍兴有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The fatty acid methyl ester sulfonate (MES) being developed at home and abroad is made of C 16 / C 18 It is prepared after sulfonation of fatty acid methyl ester, the hydrophilic group is located at the end of the hydrophobic group, the Krafft point is high, the low temperature water solubility is poor, the range of the gel region is wide and the viscosity is high, which brings certain advantages to the production and application of detergents. Difficulties, especially in the production process, the esterification / bleaching and methanol recovery processes are extremely prone to explosion. The above problems have always restricted the large-scale production and application of fatty acid methyl ester sulfonate (MES)
However, due to the high freezing point of fatty acids, it is easy to solidify in the liquid distributor of the falling film reactor, which affects the uniform distribution of materials, and the viscosity of fatty acid sulfonated products is high, which tends to thicken the liquid film at the lower part of the falling film reactor, and blockage in severe cases Reactor, the above situation is more serious when sulfonating fatty acids with carbon numbers higher than 16
[0005] So far, there is no domestic literature report on the esterification of α-sulfo fatty acids with fatty alcohols with an alkyl chain carbon number not less than 6. Fang Yun et al. only mentioned R=C in their patent (application number 200810021999.2). 6 -C 22 Alkyl α-sulfo fatty acid or its mixture is esterified with methanol (the molar ratio of the two = 1:7~40, the reaction is 2~10h under reflux)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1: n-hexanoic acid enters SO at 20°C 3 Gas jet sulfonation reactor, SO 3 / air (volume ratio 10%) mixed gas enters SO at 60°C 3 Gas injection sulfonation reactor, the gas velocity from the gas nozzle is 100m / s, n-hexanoic acid / SO 3 The feed molar ratio is 1:1.0, the reaction time of the two in the reactor body is 5 seconds, the sulfonated product and unreacted SO 3 / air mixture from SO 3 After the product outlet of the gas jet sulfonation reactor is discharged, the gas-liquid separation is carried out. After the liquid phase is cooled, the reaction is continued at 50°C for 60 minutes to obtain α-sulfocaproic acid, and the gas phase is SO 3 / air mixed gas, the mixed gas can be recycled.

[0027] Add α-sulfocaproic acid and cetyl alcohol in the esterification reactor, the mol ratio of the two is 1: 1.1, with the total mass of α-sulfo fatty acid and cetyl alcohol, add 300% heptane (boiling point 98.4°C), and reacted under reflux for 0.5h to obtain cetyl hexanoa...

Embodiment 2

[0029] C 1214 Mixed fatty acids enter SO at 40°C 3 Gas jet sulfonation reactor, SO 3 / air (volume ratio 15%) mixed gas enters SO at 65°C 3Gas injection sulfonation reactor, the gas velocity from the gas nozzle is 125m / s, C 1214 Mixed Fatty Acids / SO 3 The feed molar ratio is 1:1.2, the reaction time of the two in the reactor body is 6 seconds, the sulfonated product and unreacted SO 3 / air mixture from SO 3 After the product outlet of the gas jet sulfonation reactor is discharged, the gas-liquid separation is carried out. After the liquid phase is cooled, the reaction is continued at 180°C for 10 minutes to obtain α-sulfo C 1214 acid.

[0030] Add α-sulfo C in the esterification reaction kettle 1214 Acid and n-decyl alcohol, the molar ratio of the two is 1:1.2, with α-sulfo C 1214 Based on the total mass of acid and n-decyl alcohol, 200% n-hexane (boiling point 68.7° C.) was added in different proportions, and reacted for 2 h under reflux to obtain C 1214 Decyl sulfoni...

Embodiment 3

[0032] Hexadecanoic acid enters SO at 100°C 3 Gas jet sulfonation reactor, SO 3 / air (20% by volume) mixed gas enters SO at 80°C 3 Gas injection sulfonation reactor, the gas velocity from the gas nozzle is 225m / s, n-hexadecanic acid / SO 3 The feed molar ratio is 1:2.0, the reaction time of the two in the reactor body is 10 seconds, the sulfonated product and unreacted SO 3 / air mixture from SO 3 After the product outlet of the gas jet sulfonation reactor is discharged, the gas-liquid separation is carried out. After the liquid phase is cooled, the reaction is continued at 160° C. for 120 minutes to obtain α-sulfohexadecanoic acid.

[0033] Add α-sulfocetanoic acid and 2-ethylhexanol into the esterification reaction kettle, the molar ratio of the two is 1:1.1, without solvent, react at 30°C for 24h to obtain α-sulfocetanoic acid 2-Ethylhexanol ester. Add 80% ethanol / water solution by volume to the neutralization tank, add potassium hydroxide to prepare potassium hydroxide e...

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Abstract

The invention discloses a process for preparing fatty acid ester sulfonate, which comprises: introducing a mixed gas of SO3 and air into a SO3 gas jet-type sulfonation reactor, wherein the molar ratio of the fatty acid to the SO3 is kept at 1:1.0-2.0; reacting the fatty acid with the SO3 / air mixed gas in the SO3 gas jet-type sulfonation reactor, the product of sulfonation reaction and unreacted SO3 / air mixed gas are exhaust from product outlet of the SO3 gas jet-type sulfonation reactor, performing gas-liquid separation, cooling a liquid phase and continuing to react the liquid phase to obtain alpha-sulfo fatty acid; adding the alpha-sulfo fatty acid and an fatty alcohol which has an alkyl chain with 5 or more carbon atoms into an esterification kettle with a water distributor to perform esterification under a solvent or non-solvent condition to obtain an esterified product; and adding solution of alkaline alcohol and water in a neutralization kettle, adding the esterified product into the solution of the alkaline alcohol and water to perform an neutralization reaction, and evaporating the ethanol and the solvent added in esterification to obtain the fatty acid ester sulfonate. The process has the advantages of small equipment investment, convenient operation, simple process, easy control, water and energy conservation and high production safety.

Description

technical field [0001] The invention belongs to a process for preparing fatty acid ester sulfonate, in particular to a process for preparing fatty acid ester sulfonate through sulfur trioxide sulfonation, esterification with fatty alcohol, and neutralization. Background technique [0002] In recent years, the improvement of consumers' awareness of environmental protection and conservation, as well as the increase of environmental and economic pressures, have favorably promoted the development of washing products in the direction of low-temperature washing, concentration, liquefaction, environmental protection, energy saving, water saving, and high efficiency. Sodium alkylbenzene sulfonate (LAS), olefin sulfonate (AOS), fatty alcohol ether sodium sulfate (AES) and fatty acid methyl ester sulfonate (MES), which are currently used in domestic detergents, cannot Fully meet the above requirements, so it is necessary to develop functional surfactants with good low-temperature wate...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C303/32C07C309/17
Inventor 牛金平韩亚明韩向丽谷惠先
Owner 中轻化工绍兴有限公司
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