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Method for preparing 1,3-dioxane acetal type dianion surface active agent

A dioxane acetal and surfactant technology, applied in 1 field, can solve the problems of explosiveness, carcinogenicity, and limited industrial sources, etc., and achieve low price, weak human toxicity, and extensive industrial sources Effect

Inactive Publication Date: 2010-05-26
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Obviously, the sulfonated reagent 1,3-propane sultone used in the above-mentioned preparation method has limited industrial sources, is explosive, and has high price, especially potential carcinogenicity, so it is unfavorable for the realization of industrialization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Step 1: Add 6.84g (60mmol) n-heptanal, 8.70g (64mmol) pentaerythritol, 60mL N, N-dimethylformamide in a 100mL three-necked round bottom flask equipped with an electromagnetic stirrer, reflux condenser and thermometer (DMF) and 0.5g catalyst p-toluenesulfonic acid, refluxed for 20h. After the reaction was completed, cool, remove the solvent under reduced pressure to obtain a yellow solid, add 60ml of ethyl acetate, filter off the insoluble matter, and wash the filtrate twice with 2% sodium bicarbonate solution 100ml and distilled water 100ml respectively, add anhydrous sulfuric acid to the organic layer After magnesium drying for 3 h, ethyl acetate was removed to give a yellow solid. The yellow solid was washed with petroleum ether to obtain 11.20 g of 1,3-dioxane acetal as white needles, with a yield of 80.5%.

[0013] Step 2: Under nitrogen protection, add 40ml of anhydrous tetrahydrofuran and 0.43g (18mmol) NaH to the 100mL three-necked round-bottomed flask equipped ...

Embodiment 2

[0016] Step 1: Same as Example 1.

[0017] Step 2: Under nitrogen protection, add 40ml of anhydrous tetrahydrofuran and 0.38 (16mmol) NaH to a 100mL three-necked round-bottomed flask equipped with an electromagnetic stirrer, a reflux condenser and a thermometer. After stirring for 10 minutes, 1.74g (7.5 mmol) The white needles 1,3-dioxane acetal prepared in step 1 are dissolved in constant pressure dropping funnel with 10ml anhydrous tetrahydrofuran and slowly dripped into the round bottom flask, after reflux for 16h, cool to At room temperature, pipette 1.68ml (16mmol) of 1-chloro-3-bromopropane, slowly drop it into the flask, and reflux for 18h. After the reaction was completed, the solvent was removed, and 2.31 g of a white viscous product was obtained after recrystallization from ethanol, with a yield of 80.1%.

[0018] Step 3: Install a 100mL four-necked round bottom flask on an electromagnetic stirrer, and equipped with a reflux condenser and a thermometer. Add 0.77g (...

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Abstract

The invention relates to a method for preparing a 1,3-dioxane acetal type dianion surface active agent, which comprises the following steps of: reacting n-heptaldehyde with pentaerythritol to obtain 1,3-dioxane acetal and then reacting the 1,3-dioxane acetal with 1-chlorol-3-bromopropane; and reacting the obtained product with potassium iodide, sodium sulfite and catalyst tetrabutyl ammonium bromide in water to prepare the product. The used sulfonated reagent sodium sulfite has wide industrial source, low cost and low toxicity to the human body and provides the condition for realizing the industrialization of the product.

Description

technical field [0001] The invention relates to an acetal type decomposable surfactant, in particular to a preparation method of a 1,3-dioxane acetal type dianion surfactant. Background technique [0002] Surfactants have been widely used in many fields such as daily chemical, food, textile, medicine and petroleum based on their advantages of economy, practicability and excellent performance. At present, surfactants have been developed in the direction of green, multifunctional, specialized, and molecular design. Compared with traditional surfactants, acetal-type surfactants not only have greatly improved chemical and biodegradability, but also have a certain increase in surface activity. A direction for the development of "environmentally friendly" surfactants. The type containing 1,3-dioxane acetal is a kind of decomposable surfactant that has been studied more now, while the anionic surfactant containing 1,3-dioxane acetal at home and abroad There are relatively few st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01F17/32C09K23/32
Inventor 张昭翟文杰边建红
Owner SHANXI UNIV
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