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Preparation method for tetramethyl-bi(N1-methylene-1, 2-ethylenediamine) siloxane

A technology of dimethylethoxysilyl methylene and disiloxane, which is applied in the field of preparation of tetramethyl-disiloxane, and achieves the effect of simple operation and low cost

Inactive Publication Date: 2012-02-15
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] About tetramethyl-di(N 1 The preparation of -methylene-1,2-ethylenediamine) disiloxane has not been reported

Method used

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  • Preparation method for tetramethyl-bi(N1-methylene-1, 2-ethylenediamine) siloxane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Add 17.6 g (0.1 mol) N-(dimethylethoxysilomethylene)-1,2-ethylenediamine into a three-necked flask equipped with reflux condenser and dropping funnel, and add 1.44 dropwise with stirring g (0.08 mol) H 2 O, continue to react for 1 h after the addition is complete. After cooling, vacuum distillation (vacuum degree 3.9 KPa), collect the boiling point of 159~160 ℃ fractions, obtain tetramethyl-bis(N 1 -Methylene-1,2-ethylenediamine) disiloxane【 1 H NMR (400 MHz, CDCl 3 ): 2.72(t, J=5.6Hz, 4H), 2.61(t, J=6.0Hz, 4H), 1.99(s, 4H), 1.10(s, 6H), 0.06(s, 12H); 13 C NMR (400 MHz, CDCl 3 ): 57.16, 41.45, 41.26, 0.16; MS(M+1): 278.9. ], the yield is 97.2%, and the purity is 99.1%.

Embodiment 2

[0016] Add 17.6 g (0.1 mol) N-(dimethylethoxysilylene)-1,2-ethylenediamine into a three-necked flask equipped with a reflux condenser and dropping funnel, and add 1.08 dropwise with stirring g (0.06 mol) H 2 O, continue to react for 1 h after the addition is complete. After cooling, vacuum distillation (vacuum degree 3.9 KPa), collect the boiling point of 159~160 ℃ fractions, obtain tetramethyl-bis(N 1 -Methylene-1,2-ethylenediamine) disiloxane, with a yield of 97.3% and a purity of 99.3%.

Embodiment 3

[0018] Add 35.2 g (0.2 mol) N-(dimethylethoxysilylene)-1,2-ethylenediamine into a three-necked flask equipped with a reflux condenser and a dropping funnel, and add 2.16 dropwise with stirring g (0.12 mol) H 2 O, continue to react for 1 h after the addition is complete. After cooling, vacuum distillation (vacuum degree 3.9 KPa), collect the boiling point of 159~160 ℃ fractions, obtain tetramethyl-bis(N 1 -Methylene-1,2-ethylenediamine) disiloxane, the yield is 97.8%, and the purity is 99.2%.

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Abstract

The invention discloses a preparation method for tetramethyl-bi(N1-methylene-1, 2-ethylenediamine) siloxane, which comprises the following steps that N-(dimethylethoxysilane methylene)-1,2-ethylenediamine is used as raw materials, water is directly dripped at a room temperature for carrying out hydrolysis to prepare the tetramethyl-bi(N1-methylene-1, 2-ethylenediamine) siloxane, the reaction is continuously carried out for 1h after the dripping completion, the reduced pressure distillation is carried out after the cooling, the vacuum degree is 3.9KPa, fraction with the boiling point being 159 to 160 DEG C is collected, the tetramethyl-bi(N1-methylene-1, 2-ethylenediamine) siloxane is obtained, the mole ratio of the tetramethyl-bi(N1-methylene-1, 2-ethylenediamine) siloxane to the water is 1 / 0.6 to 0.8, the yield is 97 to 99 percent, and the purity is higher than 99 percent. The preparation method has the advantages that the heating is not needed, the preparation of target products can be completed through self heat release, the efficiency is high, the energy and the time are saved, the cost is low, the operation is simple, and the preparation method is suitable for industrial production.

Description

Technical field [0001] The present invention relates to a tetramethyl-bis(N 1 -Methylene-1,2-ethylenediamine) disiloxane is prepared by using N-(dimethylethoxysilylene)-1,2-ethylenediamine as raw material, at room temperature Directly add water to hydrolyze to prepare tetramethyl-bis(N 1 -Methylene-1,2-ethylenediamine) disiloxane method. Background technique [0002] Silicone products have both organic and inorganic properties, and have excellent high and low temperature resistance, UV and infrared radiation resistance, oxidation degradation resistance, electrical insulation, good elasticity, flame retardant, hydrophobic, non-toxic, odorless, and corrosion resistance With a series of excellent properties such as physiological inertia, silicone is called "industrial monosodium glutamate" and is widely used in electronics and electrical, light industry and textiles, cosmetics, plastics, paints, coatings, agricultural chemicals, petroleum, medicine, automobiles, machinery Various i...

Claims

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Application Information

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IPC IPC(8): C07F7/10
Inventor 余典徐朝哲方海燕康君辉余明新范宏茅开表
Owner ZHEJIANG UNIV