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Preparation of mono-epoxy-terminated polysiloxane-modified gelatin gradient membrane by freeze-drying method

A technology of freeze-drying and polysiloxane, which is applied in the field of preparing single-epoxy-terminated polysiloxane modified gelatin gradient film by freeze-drying, which can solve the problem of poor water resistance and corrosion resistance, strong plastic feeling, and affecting film Structure, film performance and film application, etc., to achieve the effect of good weather resistance, low surface tension and superior performance

Active Publication Date: 2016-03-16
山东山科美谷科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Gelatin has become an important raw material for the preparation of protein films. Like other natural polymer materials, this type of protein material has problems such as strong plastic feeling, poor water resistance and corrosion resistance after forming a film.
Siloxane-modified gelatin can improve the water resistance and flexibility of gelatin film to a certain extent [201310012009.X], but the disordered distribution of siloxane components in the film directly affects the film structure, film performance and film application

Method used

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  • Preparation of mono-epoxy-terminated polysiloxane-modified gelatin gradient membrane by freeze-drying method
  • Preparation of mono-epoxy-terminated polysiloxane-modified gelatin gradient membrane by freeze-drying method
  • Preparation of mono-epoxy-terminated polysiloxane-modified gelatin gradient membrane by freeze-drying method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 0.3g of surfactant and 95g of deionized water into a three-neck reaction flask equipped with a thermometer socket, a sampling port, and a condenser socket, stir and heat to 50°C, and after the surfactant is completely dissolved, add 0.65mL of 2 mol / L sodium hydroxide, adjust the reaction pH to be 10.0, add 5g gelatin (accounting for 5% of the total solution mass), continue to stir until the gelatin is completely dissolved, and then add monoepoxy-terminated polysiloxane (Mw=500) continuously or in batches ), the consumption of single epoxy-terminated polysiloxane is 0.8 times of the primary amino molar weight in the gelatin molecule, the reaction starts, the primary amino content in the reaction system no longer changes in 24 hours, stops stirring and heating, obtains single Epoxy-terminated polysiloxane modified gelatin solution. The monoepoxy-terminated polysiloxane-modified gelatin solution is centrifuged at low temperature, and the white substance in the middle l...

Embodiment 2

[0031] The described method is consistent with Example 1, the only difference is that the temperature of the normal pressure oven is changed to 45°C.

[0032] Mix the white product and deionized water evenly according to the mass ratio of 1:1, add and then mix evenly according to the volume ratio of the mixed solution and ethanol at a ratio of 3:1, measure 0.5ml of the mixed solution and add it dropwise to the polytetrafluoroethylene On the substrate, dry in an oven at 45°C under normal pressure to obtain a modified gelatin film. The contact angle test shows that the contact angle of the raw gelatin film is 72 o , the contact angle of the modified gelatin film increased to 85 o , indicating that the hydrophobicity of the modified gelatin film is improved; the differential calorimetry thermal scanner test shows that the Tg of the raw gelatin film is 223 ° C, and the modified gelatin film has two Tgs, which are 179 ° C and 218 ° C, respectively, indicating that the modification...

Embodiment 3

[0034] The described method is consistent with Example 1, the only difference is that the temperature of the normal pressure oven is changed to 50°C.

[0035] Mix the white product and deionized water evenly according to the mass ratio of 1:1, add and then mix evenly according to the volume ratio of the mixed solution and ethanol at a ratio of 3:1, measure 0.5ml of the mixed solution and add it dropwise to the polytetrafluoroethylene On the substrate, dry it in a normal pressure oven at 50°C to obtain a modified gelatin film. The contact angle test shows that the contact angle of the raw gelatin film is 72 o , the contact angle of the modified gelatin film increased to 85 o , indicating that the hydrophobicity of the modified gelatin film is improved; the differential calorimetry thermal scanner test shows that the Tg of the raw gelatin film is 223 ° C, and the modified gelatin film has two Tgs, which are 165 ° C and 203 ° C, respectively, indicating that the modification Th...

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Abstract

The present invention relates to preparation of a mono-epoxy-terminated polysiloxane-modified gelatin gradient membrane by a freeze-drying method. Surfactant sodium alkyl sulfate is dissolved in water and formulated into an aqueous solution, the aqueous solution is stirred for 1-2h at 40-60 DEG C under the condition of pH of 8 to 11, gelatin is added, stirring is performed for 4-8h, and mono-epoxy-terminated polysiloxane with the molecular weight of 500 is added to obtain a mono-epoxy-terminated polysiloxane-modified gelatin solution. The mono-epoxy-terminated polysiloxane-modified gelatin solution is centrifuged at a low temperature, after layering, water is added into an intermediate layer for even mixing, ethanol is added, after even mixing, 0.5-0.8ml of the mixture is measured and dropwise added into a gelatin substrate, standing is performed for 12-18h, liquid nitrogen is used for freezing, and the freeze-drying method is used for drying to obtain the mono-epoxy-terminated polysiloxane-modified gelatin gradient membrane. The mono-epoxy-terminated polysiloxane-modified gelatin gradient membrane has the characteristics that component concentration change is gradient in longitudinal section, and the mono-epoxy-terminated polysiloxane-modified gelatin gradient membrane is high in tensile strength, good in hydrophobicity and soft, and so on.

Description

technical field [0001] The invention relates to a gradient film, in particular to a freeze-drying method for preparing a monoepoxy-terminated polysiloxane modified gelatin gradient film. This kind of gradient film has the characteristics of gradient change of component concentration in the longitudinal section, high tensile strength, good hydrophobicity and softness of the film, and is especially suitable as a finishing agent for leather bag leather, garment leather or car decoration leather. Background technique [0002] Gelatin is obtained from cheap tanning, pharmaceutical and food by-products or waste. It is a renewable resource, biodegradable, and has no pollution to the environment. Gelatin has become an important raw material for the preparation of protein films. Like other natural polymer materials, this type of protein material has problems such as strong plastic feeling, poor water resistance and corrosion resistance after film formation. Siloxane-modified gelatin...

Claims

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Application Information

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IPC IPC(8): C08J5/18C08G81/00
CPCC08G81/00C08J5/18C08J2387/00
Inventor 李天铎许静班青李静岳磊
Owner 山东山科美谷科技发展有限公司
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