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A kind of catalyst based on non-volatile multifunctional poss-based tertiary amines and its preparation and application

A multi-functional, volatile technology, applied in the field of non-volatile catalysts and its preparation, can solve the problems of polyurethane material catalyst unpleasant smell, oxamine smell, etc., the method is simple and easy to achieve, the experimental efficiency is improved, and the processing process is simple Effect

Active Publication Date: 2022-03-18
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is to provide a non-volatile multifunctional POSS-based tertiary amine catalyst and its preparation and application, to overcome the traditional tertiary amine catalysts in the prior art and to easily emit small molecule products, which are very exciting. The shortcoming of bad amine odor, the technical problem that the commonly used polyurethane material catalyst produces unpleasant smell in the process of use, the present invention first synthesizes the cage with the terminal group of amino group by hydrolysis of γ-aminopropyltriethoxysilane Shaped polysilsesquioxane (octaamino POSS), and then reacted octaamino POSS with an alkyl chain with a halogen atom at one end by Hoffman alkylation reaction under reflux conditions to prepare a series of non-volatile Multifunctional POSS-based tertiary amine catalyst

Method used

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  • A kind of catalyst based on non-volatile multifunctional poss-based tertiary amines and its preparation and application
  • A kind of catalyst based on non-volatile multifunctional poss-based tertiary amines and its preparation and application
  • A kind of catalyst based on non-volatile multifunctional poss-based tertiary amines and its preparation and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] (1) Add 80g of deionized water, 40mL of n-propanol, 10mL of acetonitrile, and 2mL of tetraethylammonium hydroxide into a 250mL three-neck flask, add 50mL of γ-aminopropyltriethoxysilane under vigorous stirring, and heat up to 80°C After 24 hours of reaction, the solvent was removed by rotary evaporation, and then the product was recrystallized in tetrahydrofuran to obtain octaamino POSS. Synthetic route such as figure 1 shown.

[0040] (2) Take a 100mL round bottom flask, put POSS-NH 2(1.0g, 1.1mmol) was dissolved in 15mL of absolute ethanol solvent, then anhydrous potassium carbonate (1.2g, 9.0mmol) was added, stirred vigorously, and finally the temperature was raised to 60°C and dissolved in 10mL 1-Bromopropane (2.6g, 21.8mmol) in ethanol solvent was added dropwise in about 10min, refluxed for 12h, then cooled to room temperature, filtered to remove excess potassium carbonate, and then concentrated under reduced pressure to remove excess solvent to obtain the targe...

Embodiment 2

[0042] The preparation of octaamino POSS is the same as step (1) in Example 1.

[0043] Take a 100mL round bottom flask, put POSS-NH 2 (1.0g, 1.13mmol) was dissolved in 15mL of absolute ethanol solvent, then anhydrous potassium carbonate (1.3g, 9.1mmol) was added, stirred vigorously, and finally the temperature was raised to 80°C and dissolved in 10mL 1-Bromobutane (3.0g, 21mmol) in ethanol solvent was added dropwise in about 10min, refluxed for 12h, then cooled to room temperature, filtered to remove excess potassium carbonate, extracted 3 times with dichloromethane, then concentrated under reduced pressure Remove excess solvent to obtain the target product, named as A 2 . The yield was 85.52%. Infrared and NMR spectra are shown in image 3 b and Figure 4 b (Note: The substances from top to bottom in 3b are the obtained catalyst, 1-bromobutane, and octaamino POSS).

Embodiment 3

[0045] The preparation of octaamino POSS is the same as step (1) in Example 1.

[0046] Take a 100mL round bottom flask, put POSS-NH 2 (1.0g, 1.1mmol) was dissolved in 15mL of absolute ethanol solvent, then anhydrous potassium carbonate (1.3g, 9.1mmol) was added, stirred vigorously, and finally the temperature was raised to 80°C and dissolved in 10mL 1-Bromohexane (3.6g, 21.8mmol) in ethanol solvent was added dropwise in about 10min, refluxed for 12h, then cooled to room temperature, filtered to remove excess potassium carbonate, extracted 3 times with dichloromethane, and then decompressed Concentrate and remove excess solvent to obtain the target product, named as A 3 , and the yield was 87.27%. Infrared and NMR spectra are shown in image 3 c and Figure 4 c (Note: The substances from top to bottom in 3c are the obtained catalyst, 1-bromohexane, octaamino POSS).

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Abstract

The invention relates to a non-volatile multifunctional POSS-based tertiary amine catalyst and its preparation and application, the structure of which is shown in formula I. Preparation: Utilizing the Hofmann alkylation reaction, the haloalkanes with different alkyl chain lengths and octaamino POSS were synthesized by a one-pot method to synthesize multifunctional hybrid catalytic materials with different chain lengths. The method of the present invention is simple to operate and The reaction material is easy to obtain, the reaction is rapid, and the reaction conditions are mild. The non-volatile reactive multifunctional POSS-based tertiary amine catalyst has good application prospects in the preparation of low-odor polyurethane materials.

Description

technical field [0001] The invention belongs to the field of non-volatile catalysts and their preparation, in particular to a non-volatile multifunctional POSS-based tertiary amine catalyst and its preparation and application. Background technique [0002] Polyurethane material is a kind of multi-purpose synthetic resin with various product forms. The difference between polyurethane and other synthetic resins is that there are many kinds of raw materials, many formula combinations, and a wide range of product forms and application fields. In the process of synthesizing polyurethane, catalyst plays an important role. It is a bridge between the grafting reaction raw material and the reaction product. Polyurethane catalysts can increase the reaction rate, improve production efficiency, selectively promote positive reactions and suppress side reactions. In the production of many polyurethane products, catalyst is a commonly used auxiliary agent, although the dosage is small, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/388C08G77/04C08G77/26C08G18/18
CPCC08G77/388C08G77/045C08G77/26C08G18/1883
Inventor 徐洪耀刘义长赵岗光善仪
Owner DONGHUA UNIV