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MQ resin based organic silicon surfactant and preparation method thereof

A technology of surfactant and silicone, which is applied in the field of silicone resin or silicone surfactant to achieve long-term stability, high-efficiency emulsification, and a wide range of applications

Active Publication Date: 2019-05-31
宁波特粒科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, many patents disclose the synthesis of MQ resins (see patents CN104910382A, CN107915843A), but no attempt has been made to prepare silicone surfactants from MQ resins

Method used

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  • MQ resin based organic silicon surfactant and preparation method thereof
  • MQ resin based organic silicon surfactant and preparation method thereof
  • MQ resin based organic silicon surfactant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Utilize the inventive method to prepare hydrogen-containing MQ resin, (HR 2 SiO 1 / 2 ) m+n (R 3 SiO 1 / 2 ) p (SiO 2 ) q : Add 0.013 mol (1.75 g) of tetramethyldisiloxane (TMDS), 0.107 mol (17.4 g) of hexamethyldisiloxane into a 250 mL three-neck flask equipped with a reflux condenser, mechanical stirring and ice-water bath Oxygen (HMDS), 24.0 g deionized water, 12.0 g absolute ethanol, 16.0 g concentrated hydrochloric acid, vigorously stir and mix until transparent, add 0.4 mol (83.3 g) orthoethyl silicate (TEOS) with a constant liquid funnel, Control the dropping time to 1 h. After the ethyl orthosilicate was added, the stirring reaction was continued at room temperature for 1 h. After standing for stratification, pour off the upper liquid, wash the lower organic layer with water to neutrality, and then raise the temperature to 120 o C, Residual solvents and low molecular compounds were removed under 100 Pa vacuum conditions to obtain a colorless and transparent...

Embodiment 2~10

[0044] According to the exact same method as in Example 1, the hydrogen-containing MQ resins in Examples 2 to 10 were prepared by using different raw material combinations as shown in Table 1, and the hydrogen-containing MQ resins in Examples 2 to 10 were measured by gel permeation chromatography (GPC) at the same time. Weight-average molecular weight M of hydrogen-containing MQ resin w and molecular weight distribution M w / M n (See Table 1).

[0045] Table 1

[0046]

[0047] By comparing Examples 1 to 10 of the present invention, it is found that the obtained hydrogen-containing MQ resin can be regulated by controlling the molar ratio of tetramethyldisiloxane and hexamethyldisiloxane to the capping agent (tetramethyldisiloxane and hexamethyldisiloxane). In other words, the size of the MQ resin can be regulated. The higher the molar ratio, the larger the molecular weight and size of the obtained MQ resin. It is found that the molecular weight distribution of the MQ re...

Embodiment 11

[0049] Hydrosilylation reaction is used to graft hydrophilic / hydrophobic groups on the surface of hydrogen-containing MQ resins to prepare silicone surfactants based on MQ resins, (F 1 R 2 SiO 1 / 2 ) m (F 2 R 2 SiO 1 / 2 ) n (R 3 SiO 1 / 2 ) p (SiO 2 ) q : Add 2.0 g of hydrogen-containing MQ resin obtained in Example 1 to a 100 mL two-necked flask equipped with a reflux condenser, magnetic stirrer and rubber stopper, vent nitrogen, then vacuumize, and repeat three times to make the bottle full of nitrogen. Inject 50 mL of anhydrous toluene, 0.1 mL of xylene solution containing platinum(0)-1,3-diethylene-1,1,3,3-tetramethyldisiloxane catalyst, 0.011 mol (2.78 g) octadecene (C 18 h 36 ), 0.003 mol (1.49 g) polyethylene glycol monoallyl ether (HPAE, molecular weight 498), mix well. Heat to 120 o C was reacted for 12 h, and then low-molecular compounds were removed under 100 Pa vacuum condition to obtain a light yellow silicone surfactant based on MQ resin.

[0050] The...

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Abstract

The invention relates to an MQ resin based organic silicon surfactant and a preparation method thereof. The surfactant is in a core-shell structure with a Q portion namely a SiO2 core and an M portionnamely a shell layer containing hydrophobic and hydrophilic functional groups. The preparation method includes steps: 1) hydrogen-containing MQ resin synthesis; 2) hydrosilylation, to be more specific, grafting a double-bond-containing hydrophobic and / or hydrophilic compound on the MQ resin surface. Compared with a traditional organic silicon surfactant based on linear polydimethylsiloxane, the MQ resin based organic silicon surfactant has the advantage of excellent water resistance. Due to the special core-shell structure, advantages of a molecular surfactant and a solid particle stabilizerare combined, so that emulsifying effects and long-term stability of emulsion are improved. By control of grafting quantity of the surface hydrophobic and hydrophilic compound, amphipathicity of the surfactant can be systematically regulated. The novel surfactant can be used for stabilization of various oil-water emulsions and can serve as a foam stabilizer for polyurethane foam plastic.

Description

technical field [0001] The invention belongs to the field of organic silicon resin or organic silicon surfactant, and in particular relates to an organic silicon surfactant based on MQ resin and a preparation method thereof. Background technique [0002] Silicone surfactants were accepted by the industry as polyurethane foam stabilizers in the 1950s and entered the market, and then their structural designs became more and more diversified, and their application range continued to expand, becoming important chemicals related to the national economy and people's livelihood . [0003] Currently commercially available silicone surfactants refer to a class of substances that introduce one or more polar groups into the main chain of hydrophobic polydimethylsiloxane to make them hydrophilic. Commonly used polar groups are divided into nonionic, anionic, cationic and zwitterionic. Nonionic representatives include polyoxyethylene, polyoxyethylene and polyoxypropylene copolymers, su...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F283/12C08F283/06C08G77/12C08G77/06C08L75/04C08L51/08C08J9/00B01F17/54C09K23/54
Inventor 赵永亮朱晓敏
Owner 宁波特粒科技有限公司
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