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Process for producing an amino composition

A composition and amino technology, applied in amino compound purification/separation, condensation/addition reaction to prepare amino compounds, organic chemical methods, etc., can solve the problem of reduced commodity value, high device price, and reduced performance of epoxy resin cured products, etc. question

Active Publication Date: 2005-08-24
MITSUBISHI GAS CHEM CO INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Moreover, devices that require a high vacuum state like thin film distillation are expensive, so people are looking for a simple way to remove unreacted polyamines.
[0006] In addition, the amino composition is a low-viscosity transparent liquid immediately after preparation, and changes over time (increase in viscosity and / or formation of white solid) regardless of whether there is unreacted polyamine or not, which not only makes the commercial value remarkable It also reduces the performance of the derived epoxy resin cured product. Therefore, people are looking for a preparation method with excellent storage stability

Method used

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  • Process for producing an amino composition
  • Process for producing an amino composition

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0108] (Process 1)

[0109] In a 2-liter flask equipped with a stirring device, a thermometer, a nitrogen inlet tube, a dropping funnel, and a cooling tube, 817.2 g (6.0 mole ) and 2.9 g (0.13 mol) of lithium amide (manufactured by Merck Co., Ltd., reagent) were heated to 80° C. while stirring under a nitrogen stream. Thereafter, 625.2 g (6.0 mol) of styrene (manufactured by Wako Pure Chemical Industries, Ltd., reagent special grade) was continuously dripped over 2 hours while maintaining the temperature at 80°C. After the dropwise addition, keep it at 80°C for 30 minutes, then add 23.4g (1.3 moles) of distilled water equivalent to 10 times the molar amount of the added lithium amide, and 23.4g (1.3 moles) of distilled water equivalent to 10 times the weight of the added lithium amide as an alkali adsorption 2MgO 6 SiO 2 / xH 2 29 g of O (manufactured by Kyowa Chemical Industry Co., Ltd., キョ-ヮ-do 600s) was stirred for 1 hour, and the precipitate in the solution in the flask...

Embodiment 2

[0115] (Process 1)

[0116] In the same manner as in Example 1, 1453 g of a reaction solution containing an amino composition was obtained.

[0117] (Process 2)

[0118] 1453 g of the obtained solution was put into the same flask as in Example 1, and the inside of the apparatus was depressurized to 2.0 kPa and stirred, and then heated to 145°C. After reaching the predetermined temperature, 49 kPa steam was introduced into the apparatus, and an operation for removing unreacted polyamine was performed for 4 hours. Furthermore, the introduction of steam was stopped, and it was kept at a predetermined temperature and a reduced pressure for 30 minutes. Thus, amino composition B1175.4 g was obtained. Unreacted MXDA was 1.2% by weight. In addition, the mono-adduct was 53.0% by weight, the di-adduct was 41.6% by weight, the tri-adduct was 4.2% by weight, and the viscosity was 65 mPa·s. In addition, a storage stability test was performed on the obtained amino composition B. The r...

Embodiment 3

[0122] (Process 1)

[0123] In the same manner as in Example 1, 1453 g of a reaction solution containing an amino composition was obtained.

[0124] (Process 2)

[0125] 1453 g of the obtained solution was put into the same flask as in Example 1, and the inside of the apparatus was depressurized to 4.0 kPa and stirred, and then heated to 165°C. After reaching the predetermined temperature, 49 kPa steam was introduced into the apparatus, and an operation for removing unreacted polyamine was performed for 2.5 hours. Furthermore, the introduction of steam was stopped, and it was kept at a predetermined temperature and a reduced pressure for 30 minutes. Thus, 2.4 g of amino composition C118 was obtained. Unreacted MXDA was 1.9% by weight. In addition, the mono-adduct was 52.5% by weight, the di-adduct was 41.9% by weight, the tri-adduct was 3.7% by weight, and the viscosity was 66 mPa·s. In addition, a storage stability test was performed on the obtained amino composition C. ...

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Abstract

The present invention provides a process for producing an amino composition by addition reaction between a polyamine and an unsaturated hydrocarbon compound in the presence of a strongly basic alkali metal catalyst to obtain an amino composition containing not more than 2% by weight of unreacted polyamine and preferably not more than 10 ppm of alkali metal, which at least comprises the following steps: (A) a step of conducting addition reaction between a polyamine and an unsaturated hydrocarbon compound in the presence of a strongly basic alkali metal catalyst to obtain a reaction liquid containing an amino composition (addition reaction-step), (B) a step of removing unreacted polyamine from said reaction liquid containing an amino composition obtained by said addition reaction-step (A) in the form of a mixture of water and unreacted polyamine by steam stripping to obtain an amino composition wherein the content of unreacted polyamine is not more than 2% by weight (steam stripping-step).

Description

technical field [0001] The invention relates to a method for preparing an amino composition through the addition reaction of a polyamine and an unsaturated hydrocarbon compound. The amino composition in the invention has reactivity with epoxy resin or isocyanate, and is suitable for epoxy resin curing agent and polyurethane resin the field of chain extenders. technical background [0002] The amino composition obtained by the addition reaction of polyamine and unsaturated hydrocarbon compound is low viscosity, for example, the epoxy resin composition using the epoxy resin curing agent containing the amino composition can obtain good epoxy resin curing Physical performance, is a useful composition. [0003] The preparation method of this amino composition, that is, the preparation method of carrying out the addition reaction of polyamine and unsaturated hydrocarbon compound in the presence of a strongly basic alkali metal catalyst is a known method (refer to Japanese Patent ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/84C07B61/00C07C209/60C07C211/27C07C211/36C07C211/38
CPCC07C209/60C07C211/27
Inventor 桑原久征沼本勉越后雅敏小川俊
Owner MITSUBISHI GAS CHEM CO INC
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