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Preparation method of polyether modified siloxane

A technology of polyether modification and siloxane, applied in chemical instruments and methods, silicon organic compounds, dissolution, etc., can solve problems such as high risk, pollute the environment, affect workers' health, etc., reduce side reactions, and be easy to operate and the effect of controlling and shortening the induction period

Inactive Publication Date: 2011-10-26
南通德益化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This not only pollutes the environment, affects the health of workers, and reduces the yield of a single kettle, but also these solvents are flammable and highly dangerous

Method used

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  • Preparation method of polyether modified siloxane
  • Preparation method of polyether modified siloxane
  • Preparation method of polyether modified siloxane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Put 550g of allyl-terminated polyoxyethylene ether and 5ml of speier catalyst into a 1000ml four-necked flask equipped with a stirrer and a thermometer. 2 Start stirring under protection, slowly increase the temperature to 90°C, activate at this temperature for 1 hour, and then continuously add 220g heptamethyltrisiloxane dropwise to the system, control the reaction temperature between 100-110°C, and add dropwise After the completion of the reaction for 3-4 hours, continuous sampling is performed for infrared analysis. After the reaction is completed, the catalyst is first adsorbed with activated carbon, and then the by-products are removed by vacuum distillation. Compared with the conventional reaction, the reaction time is shortened by nearly 1 hour. After testing, the result shows that the product content is more than 95%, and the side reactions are greatly reduced, which effectively improves the reaction efficiency.

Embodiment 2

[0024] Add 575g of allyl-terminated polyoxyethylene ether and 5ml of speier catalyst into a 1000ml four-necked flask equipped with a stirrer and a thermometer. 2 Start stirring under protection, slowly increase the temperature to 90°C, activate at this temperature for 1 hour, and then continuously add 220g heptamethyltrisiloxane dropwise to the system, control the reaction temperature between 100-110°C, and add dropwise After the completion of the reaction for 3-4 hours, continuous sampling is performed for infrared analysis. After the reaction is completed, the catalyst is first adsorbed with activated carbon, and then the by-products are removed by vacuum distillation. Compared with the conventional reaction, the reaction time is shortened by nearly 1 hour. After testing, the result shows that the product content is above 96%, and the side reactions are greatly reduced, which effectively improves the reaction efficiency.

Embodiment 3

[0026] Put 620g of allyl-terminated polyoxyethylene ether and 5ml speier catalyst into a 1000ml four-necked flask equipped with a stirrer and a thermometer. 2 Start stirring under protection, slowly increase the temperature to 90°C, activate at this temperature for 1 hour, and then continuously add 220g heptamethyltrisiloxane dropwise to the system, control the reaction temperature between 100-110°C, and add dropwise After the completion of the reaction for 3-4 hours, continuous sampling is performed for infrared analysis. After the reaction is completed, the catalyst is first adsorbed with activated carbon, and then the by-products are removed by vacuum distillation. Compared with the conventional reaction, the reaction time is shortened by nearly 1 hour. After testing, the result shows that the product content is more than 95%, and the side reactions are greatly reduced, which effectively improves the reaction efficiency.

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Abstract

The invention discloses a synthesis of organosilicon surfactant (polyether modified siloxane), comprising a solvent-free reaction of terminal allyl polyoxyethylene ether (molecular weight: 456-500) with heptamethyl trisiloxane by using chloroplatinic acid (speier catalyst) as catalyst. The catalyst used in the invention has high reactive activity for catalyzing organosilicon, and active hydrogen has high conversion rate, the use of benzene organic solvent is prevented, so that the preparation process is nontoxic and no pollution. The prepared polyether modified siloxane is clear and transparent, and has good wetability and spreadability.

Description

Technical field [0001] The invention relates to a method for preparing polyether-modified siloxane, in particular to a method for preparing polyether-modified siloxane by using hydrosilylation reaction. Background technique [0002] Silicone surfactants have the unique advantages of low surface tension, good wetting and spreading, large emulsification, good compatibility, and have foaming, foam stabilization and foam suppression effects, and no toxic side effects. They are now widely used In the agricultural chemicals, coatings, and textile industries. Through polyether graft modification, the prepared polyether modified siloxane can self-emulsify in water system, has good stability and strong surface expansion ability. [0003] Organosilicon surfactants are generally prepared by the hydrosilylation reaction, and there are certain deficiencies in the production process. In order to prevent the crosslinking of Si-H bonds in industrial production, it is generally necessary to add a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/08B01F17/54C09K23/54
Inventor 章小红贾庆山马海兵王莉
Owner 南通德益化工有限公司
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