Preparation method of aminopolyether modified polysiloxane deforming agent

A technology of polysiloxane defoamer and amino polyether, which is applied in the field of defoamers, can solve the problems of poor polarity and poor water solubility, and achieve the effect of mild conditions, strong hydrophilicity and good stability

Inactive Publication Date: 2013-07-24
JIANGNAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, polyether modified polysiloxane defoamers hav...

Method used

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  • Preparation method of aminopolyether modified polysiloxane deforming agent
  • Preparation method of aminopolyether modified polysiloxane deforming agent
  • Preparation method of aminopolyether modified polysiloxane deforming agent

Examples

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preparation example Construction

[0015] In the preparation steps of the epoxy-modified silicone oil described in the present invention, in order to promote the reaction to be as thorough as possible, it is necessary to control several key factors such as the feed ratio of the reactants, the order of feed, and the reaction temperature: (1) Reaction Ratio of materials: In order to make the hydrogen-containing silicone oil react as completely as possible, it is necessary to control the amount of allyl glycidyl ether to be slightly excessive compared with the hydrogen-containing silicone oil, so that the hydrogen-containing silicone oil can be fully reacted, thereby increasing the shrinkage of the allyl glycidyl ether. Grafting rate of glycerol ether; (2) Feeding sequence: When preparing epoxy-modified silicone oil, it is necessary to preheat allyl glycidyl ether and chloroplatinic acid catalyst first, and then use the mixed solution of hydrogen-containing silicone oil and toluene to Constant pressure dropping fun...

Embodiment 1

[0035] Embodiment 1: A kind of preparation method of amino polyether modified polysiloxane defoamer, comprises the following process steps:

[0036] (1) Weigh 20g of terminal hydrogen-containing silicone oil (the mass of H atoms in the Si-H bond in the hydrogen-containing silicone oil accounts for 0.2478% of the mass of the hydrogen-containing silicone oil), dissolve the hydrogen-containing silicone oil in 25ml of toluene, and obtain the toluene of the hydrogen-containing silicone oil solution; weigh 6.788g (0.05947mol) allyl glycidyl ether and 0.1049g platinum catalyst, the amount of platinum catalyst added is 30ppm of the total mass of hydrogen-containing silicone oil and allyl glycidyl ether; Add the platinum catalyst into the container and mix it. After heating up to 60°C under the condition of nitrogen protection and reflux condensation, start to drop the toluene solution containing hydrogen silicone oil at a rate of 2 drops / second; continue to heat up to 90°C, under nitro...

Embodiment 2

[0042] Embodiment two: a kind of preparation method of amino polyether modified polysiloxane defoamer, comprises the following process steps:

[0043] (1) Weigh 3 g of epoxy-modified silicone oil (epoxy group is 0.005691 mol) obtained in Example 1 with an epoxy value of 0.1897 mol / 100 g;

[0044] (2) Add epoxy-modified silicone oil and 6.7270g of M-1000 (amine group content: 0.005691mol) into the container, measure 10ml of ethanol into the container as a solvent, stir and mix evenly; under the conditions of nitrogen protection and reflux condensation Carry out reaction, reaction temperature is 95 ℃, and reaction time is 12 hours; After reaction finishes, remove ethanol on rotary evaporator, and the temperature of rotary evaporator is 55 ℃, and pressure is-0.08MPa, and processing time is 22 minutes; Drying at 55° C. and vacuum degree of -0.09 MPa for 12 hours gave a light yellow amino polyether modified polysiloxane defoamer.

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Abstract

The invention relates to a preparation method of an aminopolyether modified polysiloxane deforming agent. The preparation method comprises the following steps of: (1) adding allyl glycidyl ether and a platinum catalyst to a container, stirring and heating under the conditions of nitrogen protection and reflux condensing; after heating to a certain temperature, dropwise adding a toluene solution containing hydrogen silicon oil; at the end of reaction, removing a solvent and low-boiling-point substances on a rotary evaporator and drying to obtain epoxy modified silicon oil; and (2) adding the epoxy modified silicon oil obtained in the step (1) and an ethanol solution of polyether amine to the container, heating and stirring, reacting under the conditions of nitrogen protection and reflux condensing; at the end of the reaction, removing ethanol on the rotary evaporator and drying to obtain the aminopolyether modified polysiloxane product. According to the preparation method, hydrosilylation/ring opening amination is used, simultaneously amino groups and polyether chain segments are introduced to a polysiloxane skeleton, the obtained deforming agent has good water solubility and stability, no additives and compounding are not added, and the aminopolyether modified polysiloxane deforming agent has good defoaming and foam inhibition performances at normal temperature.

Description

technical field [0001] The invention relates to a defoamer used in industries such as food, paint and printing ink, in particular to a preparation method of an amino polyether modified polysiloxane defoamer. Background technique [0002] With the increase of industrial production scale and environmental governance, a wide variety of defoamers have emerged. Among them, polydimethylsiloxane (methyl silicone oil) defoamer is favored by people for its low surface tension, chemical inertness, fast defoaming speed, long foam suppression time, no physiological toxicity, and wide application. However, it has disadvantages such as not being resistant to high temperature and strong alkali, poor dispersion in water, and needing emulsification. Although polyether defoamers are resistant to high temperature and strong alkali, their defoaming speed is not ideal. So in recent years there has been research on polyether-modified polysiloxane defoamers, which combine the advantages of tradi...

Claims

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Application Information

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IPC IPC(8): C08G81/00C08G77/38C08G77/388B01D19/04
Inventor 张松林张冬辉范慧军施英丁玉强张文泉尤卫民
Owner JIANGNAN UNIV
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