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Method for compounding high-purity sulfuric acid esters

A technology of a sulfuric acid diester and a synthesis method, applied in the field of organic chemistry, can solve the problems of inability to truly meet the requirements of large-scale industrial production, large material loss, production failure, etc., and achieve easy industrial-scale production, low pollution, and simple production operations. Effect

Inactive Publication Date: 2015-09-30
CHENGDU BAISHIXING SCI & TECH IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method requires olefins to have a high purity, and the reaction is either carried out in a high-concentration liquid state at low temperature, or a large amount of gas needs to be passed through, resulting in a large material loss, and at the same time, higher requirements are placed on equipment and energy consumption.
Unable to truly meet the requirements of large-scale industrial production
[0007] When the R and R' groups are substituted organic functional groups, use the above method to synthesize higher-order sulfuric acid diesters. Since the multi-substituted alkenes have multiple reaction sites, the substituted alcohols will dehydrate to form alkenes isomers. Use sulfuric acid The method of production often obtains a mixture of sulfate esters, or high polymers, resulting in production failure

Method used

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  • Method for compounding high-purity sulfuric acid esters
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  • Method for compounding high-purity sulfuric acid esters

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Experimental program
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Effect test

Embodiment 1

[0030] Embodiment 1: the synthesis of diisobutyl sulfate

[0031] (1) Preparation of diisobutyl sulfite

[0032] In a dry 500 ml three-necked flask, add anhydrous isobutanol (200 g, 2.7 mol), cool to 0-10° C. with ice water, add thionyl chloride (107 g, 0.9 mol) dropwise under rapid stirring, After the dropwise addition was completed, the temperature was naturally raised to room temperature, and stirring was continued for 2 hours. Spot the plate to track the reaction. When it shows a single point, the reaction is over. The reaction time is 2 hours. Add 100 ml of saturated sodium bicarbonate aqueous solution to the reaction system, stir for 10 minutes, let stand to separate the layers, and wash the organic layer twice with water. (50ml×2) and dried to obtain a colorless oil (187g), yield 99%.

[0033] (2) Preparation of diisobutyl sulfate (potassium permanganate oxidation method)

[0034] The diisobutyl sulfite (187 grams) obtained above was dissolved in a mixed solvent of 3...

Embodiment 2

[0035] Embodiment 2: the synthesis of diisobutyl sulfate

[0036] (1) Preparation of diisobutyl sulfite

[0037] In a dry 500 ml three-necked flask, add anhydrous isobutanol (185 g, 2.5 mol), cool to 0-10 °C with ice water, add thionyl chloride (118 g, 1 mol) dropwise under rapid stirring, drop After the addition was completed, the temperature was naturally raised to room temperature, and stirring was continued for 2 hours. The dot plate tracks the reaction, and when it appears as a single dot, the reaction is complete. The reaction time was 20h, and 100 ml of saturated aqueous sodium bicarbonate solution was added to the reaction system, and after stirring for 10 minutes, the layers were left to stand, and the organic layer was washed twice with water (50 ml × 2), and dried to obtain a colorless oil ( 184 grams), yield 95%.

[0038] (2) Preparation of diisobutyl sulfate (hydrogen peroxide oxidation method)

[0039] The diisobutyl sulfite (184 grams) obtained above was dis...

Embodiment 3

[0040] Embodiment 3: the synthesis of diisobutyl sulfate

[0041] (1) Preparation of diisobutyl sulfite

[0042] In a dry 500 ml three-necked flask, add anhydrous isobutanol (163 g, 2.2 mol), cool to 0-10 ° C with ice water, add thionyl chloride (118 g, 1 mol) dropwise under rapid stirring, drop After the addition was completed, the temperature was naturally raised to room temperature, and stirring was continued for 2 hours. The dot plate tracks the reaction, and when it appears as a single dot, the reaction is complete. Reaction time is 10, in reaction system, add 100 milliliters of saturated sodium bicarbonate aqueous solutions, after stirring for 10 minutes, leave standstill layering, organic layer washes with water twice again (50 milliliters * 2), dry, obtain colorless oil ( 182 grams), yield 94%.

[0043] (2) Preparation of diisobutyl sulfate (oxone oxidation method)

[0044]The diisobutyl sulfite obtained above (182 g) was dissolved in 400 ml of tetrahydrofuran / wate...

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Abstract

The invention discloses a method for compounding high-purity sulfuric acid esters, wherein alcohol and thionyl chloride react to generate a midbody A, the midbody A is reacted in oxidizing agents to generates sulfuric acid esters. The method for compounding the high-purity sulfuric acid esters has the beneficial effects that the method for compounding the high-purity sulfuric acid esters use the alcohol, the thionyl chloride and the oxidizing agents as raw materials, wherein the alcohol, the thionyl chloride and the oxidizing agents are easy to obtain, and are low in cost. The method for compounding the high-purity sulfuric acid esters is high in selectivity, does not have side effect, is high in yield and strong in universality, and is suitable for all complex high grade sulfuric acid esters. The method for compounding the high-purity sulfuric acid esters is simple in production operation, is low in demands on process equipment, does not have corrosivity, does not need strict production conditions such as high pressure high temperature or high pressure low temperature and the like, is easy for industrial scale production and small in pollution to environment, and accords with environmental protection requirements of green production.

Description

technical field [0001] The invention belongs to the field of organic chemistry, in particular to a method for synthesizing high-purity sulfuric acid diester. Background technique [0002] Sulfuric acid esters such as structural formula (I) are organic ester derivatives of sulfuric acid, the general formula R-O-SO 2 -O-R', [0003] [0004] When R is an organic group and R' is a proton or no group (i.e., a sulfate at one end), the general formula represents a sulfuric acid monoester, such as the detergent sodium lauryl sulfate derived from lauryl alcohol and chlorosulfonic acid , and ethoxylated fatty alcohols such as sodium lauryl polyoxyethylene ether sulfate used in daily necessities. When R and R' are both organic groups, the general formula represents a sulfuric acid diester, usually a symmetrical sulfuric acid diester (that is, R=R'), and diethyl sulfate and dimethyl sulfate are common. [0005] Sulfate ester is an important class of organic chemical raw materials...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/24C07C305/08
Inventor 石常青
Owner CHENGDU BAISHIXING SCI & TECH IND
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