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Alkynolalkoxy compound modified siloxanesurfactant and preparation method thereof

A technology of surfactant and compound, applied in the field of siloxane surfactant and its preparation, can solve the problems of leather surface effect, reduce dynamic surface tension, large dynamic surface tension gap, etc., and achieve good environmental and economic benefits , Improve foam problem, good compatibility effect

Inactive Publication Date: 2019-01-18
WUHAN OXIRAN SPECIALTY CHEM CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] U.S. Patent (application date: 1997-08-08, publication number: US5869727A) discloses a manufacturing process of polyether-modified silicone, which states that the grafted product - polyether-modified polysiloxane, can effectively The surface tension of the system can be reduced, so as to achieve the effect of wetting and leveling, but this kind of surfactant has a strong foam stabilizing function at the same time, but the air bubbles will have a serious impact on the surface effect of the leather; and, the United States The patent (application date: 1994-03-08, publication number: US5391697A) discloses that the static surface tension and dynamic surface tension of polyether-modified organosiloxane surfactants are very different. , its wettability decreased obviously; U.S. Patent (application date: 2001-12-18, publication number: US6455234B1), Japanese patent (application date: 1990-07-17, publication number: JP2636954B2) all reported acetylenic diols Ethoxylated surfactants can reduce dynamic surface tension and have low foaming characteristics. Under high-speed and dynamic construction conditions, they have good wetting properties and wide application range
However, these surfactants have high static surface tension values ​​which make it difficult to wet lower surface energy substrates

Method used

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  • Alkynolalkoxy compound modified siloxanesurfactant and preparation method thereof
  • Alkynolalkoxy compound modified siloxanesurfactant and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0036] The preparation process of the siloxane surfactant modified by the acetylenic alcohol alkoxy compound is as follows figure 1 Shown, the reaction raw materials 1,1,1,3,5,5,5--heptamethyltrisiloxane (HMTS) and butynediol ethoxy ether (BEO), through the hydrosilylation reaction method synthesis.

[0037] The specific operation is: feed the raw materials HMTS (Runhe Silicone) and BEO (Wuhan Aoke Special Chemicals) at a molar ratio of 1.13:1, and the catalyst H 2 PtC1 6 According to 100ppm (the amount is based on the mass of Pt / the total mass of acetylenic alcohol alkoxy compound and hydrogen-containing siloxane), the reaction inhibitor sodium carboxylate is added to a 250mL four-port container equipped with a mechanical stirring device, a condensing reflux device and a thermometer. In the round-bottomed flask, wherein the addition of the reaction inhibitor accounts for 0.05% of the total reactant mass percentage, then vacuumizes, and the vacuum degree is at 500mmHg, and t...

Embodiment 2

[0039] The raw materials HMTS (Runhe Silicone) and BEO (Wuhan Aoke Specialty Chemicals) were fed in a molar ratio of 1.13:1, and the catalyst H 2 PtC1 6 According to 50ppm (the amount is based on the total mass of Pt mass / alkynol alkoxy compound and hydrogen-containing siloxane), accounting for 0.05% reaction inhibitor sodium carboxylate in the mass percentage of the total reaction substances, add a mechanical stirring device , 250mL four-neck round-bottomed flask with a condensing reflux device and a thermometer, vacuumize, and the vacuum degree is at 700mmHg, and then under stirring conditions, after heating and reacting in an oil bath for 3.5 hours, the temperature is finally cooled and discharged to obtain the product acetylenic alcohol alkoxy compound Modified silicone surfactant (TBEO). It is measured that the hydrosilylation conversion rate is 85%, and the color is transparent and watery white.

Embodiment 3

[0041] The raw materials HMTS (Runhe Silicone) and BEO (Wuhan Aoke Specialty Chemicals) were fed in a molar ratio of 1.13:1, and the catalyst H 2 PtC1 6According to 200ppm (the amount is based on the total mass of Pt mass / alkynol alkoxy compound and hydrogen-containing siloxane), accounting for 0.05% reaction inhibitor sodium carboxylate in the mass percentage of the total reaction substance, add a mechanical stirring device , a 250mL four-necked round-bottomed flask with a condensing reflux device and a thermometer, vacuumize, and the vacuum degree is at 500mmHg, and then under stirring conditions, after heating and reacting in an oil bath for 3.5 hours, the temperature is finally cooled and discharged to obtain the product acetylenic alcohol alkoxy compound . The tested silicon hydrogen conversion rate is 88%. Color yellow.

[0042] In terms of silicon hydrogen conversion rate, increasing the amount of catalyst did not improve the conversion rate, and the color deepened. ...

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Abstract

The invention discloses an alkynolalkoxy compound modified siloxanesurfactant, a main chain of a molecular structure is a hydrogen-containing siloxane group losing a hydrogen atom, a side chain is analkynolalkoxy compound group through addition of alkynyl and one hydrogen, and the main chain and the side chain are connected through a Si-C chemical bond; a synthesis method comprises the followingsteps: an alkynolalkoxy compound and hydrogen-containing siloxane have a hydrosilylation reaction to obtain a product under a vacuum, solvent-free and catalyst conditions; and the molar ratio of the alkynolalkoxy compound to the hydrogen-containing siloxane is 1.15:1, the reaction temperature is 80 DEG C to 110 DEG C, the vacuum degree of the reaction is 200-750 mmHg, the reaction time is 3.5 h,and proper amount of reaction inhibitor is used. The surfactant has the advantages of low static and dynamic surface tension, low foam, high stability and the like; the preparation method is differentfrom the traditional preparation process, the use of a carboxylic acid or a salt of the carboxylic acid prevents the condition that the acetylene alcohol ether and / or hydroxyl of a copolymer form / forms acetal, the steps of processing the acetal and a solvent and dissolving out the solvent in the traditional process are omitted, the process is simplified, and the cost is lowered.

Description

technical field [0001] The invention relates to the technical field of surfactants, in particular to a siloxane surfactant modified by an alkynol alkoxy compound and a preparation method thereof. Background technique [0002] Polyether modified silicone surfactant is the most widely used silicone surfactant in industry. It has the characteristics of effectively reducing the interfacial tension of the oil-water interface that trisiloxane surfactants usually have, and has the characteristics of "super spreadability" on low-energy hydrophobic surfaces. Due to its thermal instability in application, weak emulsification ability to oil / water interface and more foam when using concentration. Therefore, the scope of application of polyether-modified siloxane surfactants is limited to a certain extent. In addition, the raw materials for the synthesis of polyethers come from non-renewable petroleum energy sources. [0003] Alkyne diol surfactants are a new class of multifunctional ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01F17/54B01F17/42C09K23/54C09K23/42
CPCC09K23/00
Inventor 刘敏任凡付远波王亮张静耿聪
Owner WUHAN OXIRAN SPECIALTY CHEM CO
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