Secondary terminating method for synthesizing methoxy-terminated polyether with high terminating rate

A technology of methoxy capping and capping rate, which is applied in the field of secondary capping method to synthesize high capping rate methoxy capped polyether, which can solve the problems of low capping rate, increased alkali dosage, unsuitable use, etc. , to achieve the effect of increasing the sealing rate and reducing the difficulty

Active Publication Date: 2010-06-02
NANJING WELL BIOCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

One is that the capping rate is not high, especially when the molecular weight of the polyether is greater than 1000, the capping rate is generally difficult to exceed 90%. Increasing the amount of alkali can also increase the capping rate, but the effect is not obvious. A large amount of salt increases the difficulty of post-processing; secondly, dimethyl sulfate is highly toxic and is a carcinogen, so it should not be used

Method used

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  • Secondary terminating method for synthesizing methoxy-terminated polyether with high terminating rate
  • Secondary terminating method for synthesizing methoxy-terminated polyether with high terminating rate
  • Secondary terminating method for synthesizing methoxy-terminated polyether with high terminating rate

Examples

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Effect test

Embodiment 1

[0041] Add 600g of polypropylene oxide-ethylene oxide mono-n-butanol ether with a molecular weight of 1210 into a 1L autoclave, gradually raise the temperature to 110°C~120°C through the jacket, and dehydrate under vacuum (0.095MPa~0.099MPa) 1 hour, then lower the temperature to 30°C, add 32g of sodium methoxide into the kettle, then raise the temperature to 110°C~120°C, demethanolize under 0.095MPa~0.099MPa vacuum for 1 hour, cool down to 70°C~80°C, and introduce 32g Chloromethane, control the pressure in the kettle to 0.2-0.4MPa, age for 5 hours, add 6.9g sodium hydride (50% active ingredient) after venting, degas for 1 hour under the same conditions as before, then press 8g of methyl chloride, The pressure is 0.2MPa. When the pressure in the kettle drops to 0.1MPa, the temperature is lowered to 30°C and the material is discharged. After the feed liquid is post-treated, 550g of methoxy-terminated polypropylene oxide-ethylene oxide mono-n-butanol ether is obtained. The value ...

Embodiment 2

[0043] Add 600g of polypropylene oxide-ethylene oxide mono-n-butanol ether with a molecular weight of 1112 into a 1L autoclave, gradually raise the temperature to 110°C~120°C with steam through the jacket, and dehydrate under vacuum (0.095MPa~0.099MPa) 1 hour, then lower the temperature to 30°C, add 25.9g of sodium hydroxide into the kettle, then raise the temperature to 110°C~120°C, dehydrate under 0.095MPa~0.099MPa vacuum for 1 hour, cool down to 70°C~80°C, pass 36g of methyl chloride, control the pressure in the kettle to 0.2-0.4MPa, age for 5 hours, add 7.51g of sodium hydride (50% active ingredient) after venting, degas for 1 hour under the same conditions as before, and then press 9g of methyl chloride into the kettle. The internal pressure is 0.2MPa. When the pressure in the kettle drops below 0.1MPa, the temperature is lowered to 30°C and the material is discharged. The material liquid is post-treated to obtain 547g of methoxy-terminated polypropylene oxide-ethylene oxi...

Embodiment 3

[0045]Add 600g of polypropylene oxide-ethylene oxide monoethanol ether with a molecular weight of 1305 into a 1L autoclave, gradually raise the temperature to 110°C~120°C through the jacket, and dehydrate under vacuum (0.095MPa~0.099MPa) for 1 hour , then lower the temperature to 30°C, add 30.9g of potassium hydroxide to the kettle, then raise the temperature to 110°C to 120°C, dehydrate under vacuum at 0.095MPa to 0.099MPa for 1 hour, cool down to 70°C to 80°C, and introduce 30g of chlorine Methane, control the pressure in the kettle to 0.2-0.4MPa, age for 5 hours, add 6.4g sodium hydride (50% active ingredient) after venting, degas for 1 hour under the same conditions as before, then press 7g of methyl chloride, the pressure in the kettle 0.2MPa, when the pressure in the kettle drops below 0.1MPa, the temperature is lowered to 30°C and the material is discharged, and the material liquid is post-treated to obtain 542g of methoxy-terminated polypropylene oxide-ethylene oxide mo...

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Abstract

The invention relates to a secondary terminating method for synthesizing methoxy-terminated polyether with high terminating rate, characterized in that terminating is continuously carried out twice in an autoclave. The method comprises the following steps: (1) adding single-hydroxy polyether and alkali to a reaction container; (2) stirring, increasing the temperature and reducing pressure to remove small molecular compounds; (3) leading chloromethane in to finish an etherification reaction under a certain pressure and temperature; (4) adding sodium hydride; (5) stirring, increasing the temperature and reducing pressure to remove hydrogen; (6) leading chloromethane in to finish the etherification reaction under a certain pressure and temperature; and (7) refining and post processing to obtain a qualified product. Polyether with high terminating rate higher than 99% is obtained after post processing the product. The invention overcomes the defects of a traditional process, obviously improves the terminating rate, lowers the post processing difficulty and avoids using carcinogens (such as dimethyl sulfate, and the like) by a traditional method.

Description

technical field [0001] The invention relates to a methyl end capping technology of saturated or unsaturated monohydroxyl polyether, which is a method for synthesizing high end capping rate methoxy end polyether by secondary end capping. Background technique [0002] Compared with ω-hydroxypolyether, alkoxy-terminated polyether has many special properties, such as low viscosity, small viscosity-temperature change, good chemical inertness, and not easy to absorb water. These special properties make alkoxy-terminated polyethers widely used in chemical fiber oil agents, low-foaming surfactants, air-conditioning compressor oils, and foam stabilizers for polyurethane foaming. However, after the hydroxyl polyether is capped with alkoxy groups, there are always a small amount of residual hydroxyl groups in the product. Due to the existence of hydroxyl groups, the product is easily oxidized during application, which affects the stability and service life of the product. In addition,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/338
Inventor 费红沈德渊贾建国
Owner NANJING WELL BIOCHEM
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