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Preparation method of monoamino polyoxyethylene ether

A technology of monoamine polyoxyethylene ether and polyoxyethylene ether, which is applied in the field of preparation of monoamine polyoxyethylene ether, can solve the problems of affecting yield, high cost, potential safety hazards and the like, and achieves simplified reaction steps and operations Process, the reaction process is mild, the effect of improving the utilization rate

Pending Publication Date: 2019-11-22
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the catalytic reductive amination method has a simple and mature process route, and the product has a high conversion rate and primary amine selectivity, it requires high temperature (above 200°C) and high pressure (10-15MPa) reaction conditions, which affects the color of the product, and the process affects the equipment. The requirements are high, the equipment investment is large, the cost is high, there are certain safety hazards, and the preparation process of the catalyst is quite complicated, the catalytic efficiency of the catalyst is low, it is easy to be broken and deactivated, and the yield is affected

Method used

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  • Preparation method of monoamino polyoxyethylene ether
  • Preparation method of monoamino polyoxyethylene ether
  • Preparation method of monoamino polyoxyethylene ether

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Embodiment 1, the preparation of amino-terminated carbinol polyoxyethylene (10) ether

[0033] (1) Preparation of 2-(Boc amino)ethanol polyoxyethylene (10) ether: inhale 1mol in the glass-lined reactor, the N-(tert-butoxycarbonyl)ethanolamine that quality is 161g, and inhale 4.8g catalyst SnO2-PtO2-Al2O3, after pumping, close the vacuum valve. replace N2 Secondary, vacuum degree ≥-0.098MPa, displacement pressure ≥0.02MPa. replace N 2 After completion, slowly raise the temperature, control the temperature at 105±2°C, and dehydrate for 1.0h. After the dehydration is completed, raise the temperature to above 120°C and add 10mol of EO with a mass of 440g, control the reaction temperature at 145-150°C, and the pressure ≤0.30Mpa. After the reaction is completed, the temperature is lowered to 100° C. for degassing, and the material is discharged to obtain the crude product of 2-(Boc amino)ethanol polyoxyethylene (10) ether.

[0034] (2) Preparation of terminal (Boc amino) ...

Embodiment 2

[0036] Example 2. The preparation method of amino-terminated carbinol polyoxyethylene ethers of different specifications refers to Example 1. The difference from Example 1 is that the number of EO added is different, and the amount of each added reagent also changes with the change of EO. , see Table-1 for details.

[0037] Table-1 Amino-terminated carbinol polyoxyethylene ethers of different specifications

[0038]

[0039] It can be seen from Table-1 that when the molar ratio of the initiator N-(tert-butoxycarbonyl)ethanolamine to EO is in the range of 1:1-1:20, the prepared monoamino polyoxyethylene ether The conversion rates are all greater than 96%, and as the molecular weight increases, the conversion rate decreases gradually. Therefore, this method is more suitable for the synthesis of low molecular weight monoamino polyoxyethylene ether products.

Embodiment 3

[0040] Embodiment three, the preparation of amino alcohol-terminated polyoxyethylene (10) ether

[0041] (1) Preparation of 2-(Boc amino)ethanol polyoxyethylene (10) ether: inhale 1mol in the glass-lined reactor, the N-(tert-butoxycarbonyl)ethanolamine that quality is 161g, and inhale 4.8g catalyst SnO2-PtO2-Al2O3, after pumping, close the vacuum valve. replace N 2 Secondary, vacuum degree ≥-0.098MPa, displacement pressure ≥0.02MPa. replace N 2 After completion, slowly raise the temperature, control the temperature at 105±2°C, and dehydrate for 1.0h. After the dehydration is completed, raise the temperature to above 120°C and add 10mol of EO with a mass of 440g, control the reaction temperature at 145-150°C, and the pressure ≤0.30Mpa. After the reaction is completed, the temperature is lowered to 100° C. for degassing, and the material is discharged to obtain the crude product of 2-(Boc amino)ethanol polyoxyethylene (10) ether.

[0042] (2) Preparation of terminal (Boc am...

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Abstract

The invention relates to the technical field of production of amine-terminated polyether, in particular to a preparation method of monoamino polyoxyethylene ether. The invention relates to the preparation method of monoamino polyoxyethylene ether. The method comprises the following steps: reacting N-(tert-butyloxycarbonyl) ethanolamine with a supported catalyst SnO2-PtO2-Al2O3 to obtain 2-(Boc amino) ethanol polyoxyethylene ether through a polymerization reaction, directly adding an end-capping reagent after the reaction is finished, allowing a by-product HCl in the reaction to directly reactwith a BOC group to generate isobutene, CO2 and amino-terminated polyether salt, and finally obtaining the product monoamino polyoxyethylene ether by adjusting the pH value.

Description

technical field [0001] The invention relates to the technical field of amino-terminated polyether production, in particular to a preparation method of monoamino polyoxyethylene ether. [0002] technical background [0003] Amine-terminated polyethers (Amine-Terminated Polyethers) are a class of compounds with a polyoxyalkylene structure as the main chain and terminal amine groups as active functional groups. Since the amino hydrogen at the end of the amino-terminated polyether has stronger reactivity than the hydroxyl hydrogen at the end of the polyether, it can react with a variety of compounds, which greatly broadens the application range of the amino-terminated polyether in the industrial field. According to the number of substituted hydrogen atoms in the amine groups, amino-terminated polyethers can be divided into primary amine-terminated polyethers and secondary amine-terminated polyethers. Common primary amine-terminated polyethers in the industry include polyepoxy Et...

Claims

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Application Information

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IPC IPC(8): C08G65/28C08G65/337
CPCC08G65/2624C08G65/2654C08G65/266C08G65/269C08G65/337
Inventor 宋明贵金一丰余江陈天园金凌熠
Owner ZHEJIANG HUANGMA TECH