Modified gelatin gradient film prepared from mixed glycidol and single-epoxy-terminated polysiloxane

A technology of polysiloxane and glycidol, which is applied in coatings, protein coatings, etc., can solve problems such as poor water resistance and corrosion resistance, strong plastic feeling, affecting film structure, film performance and film application, etc., to achieve weather resistance Excellent performance, low surface tension and superior performance

Active Publication Date: 2016-05-11
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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  • Modified gelatin gradient film prepared from mixed glycidol and single-epoxy-terminated polysiloxane
  • Modified gelatin gradient film prepared from mixed glycidol and single-epoxy-terminated polysiloxane
  • Modified gelatin gradient film prepared from mixed glycidol and single-epoxy-terminated polysiloxane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 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

[0029] The described method is consistent with that of Example 1, the only difference is that the temperature of the normal pressure oven is changed from 5°C to normal temperature.

[0030] Mix the white product and deionized water evenly at a mass ratio of 1:1, measure 0.5ml of the mixed solution, drop it on the gelatin substrate, and dry it at room temperature 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 81 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 115 ° C and 220 ° C, respectively, indicating that the modification The gelatin film has a microphase separation structure; scanning electron microscopy-energy dispersive spectroscopy analysis shows that...

Embodiment 3

[0032] The described method is consistent with Example 1, the only difference is that the temperature of the normal pressure oven is changed to 40°C.

[0033] Mix the white product and deionized water evenly at a mass ratio of 1:1, measure 0.5ml of the mixed solution, drop it on the gelatin substrate, and dry it in an oven at 40°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 increases to 100 o , indicating that the hydrophobicity of the modified gelatin film is improved; the differential calorimeter 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 127 ° C and 224 ° C, respectively, indicating that the modification The gelatin film has a microphase separation structure; scanning electron microscopy-energy dispersive spectroscopy analysis shows that the sili...

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Abstract

The invention relates to a modified gelatin gradient film prepared from mixed glycidol and single-epoxy-terminated polysiloxane. A method for preparing the modified gelatin gradient film includes dissolving surfactants in water to prepare aqueous solution; adding gelatin into the aqueous solution under the conditions of the temperatures of 40-60 DEG C and the pH (potential of hydrogen) of 8-11; stirring the gelatin and the aqueous solution for 4-8 h and then adding the single-epoxy-terminated polysiloxane into the gelatin and the aqueous solution continuously or in batches to obtain mixtures; carrying out reaction for 12-30 h and then adding glycidol into the mixtures; continuing to carry out reaction at the temperatures of 40-60 DEG C for 6-12 h to obtain milk white turbid liquid; adding ethyl alcohol into the milk white turbid liquid and uniformly mixing the ethyl alcohol with the milk white turbid liquid to obtain mixed liquid; dripping 0.5-0.8 ml of the measured mixed liquid on gelatin substrates; allowing the gelatin substrates to stand still for 12-18 h and then freezing the gelatin substrates by the aid of liquid nitrogen; drying the gelatin substrates by the aid of a freeze dryer to obtain the gradient film. The dosage of the gelatin is 1-10% of the mass of the aqueous solution. The dosage of the single-epoxy-terminated polysiloxane is 0.2-1.0 times the molar weight of the gelatin. The dosage of the glycidol is 0-1 times the mass of the single-epoxy-terminated polysiloxane. A volume ratio of the ethyl alcohol to reaction liquid is (3-5):1. The modified gelatin gradient film has the advantages that the concentration of components of the modified gelatin gradient film changes in longitudinal sections in a gradient manner, the modified gelatin gradient film is high in tensile strength and good in hydrophobic property and is soft, and the like.

Description

technical field [0001] The invention relates to a gradient film, in particular to preparing a modified gelatin gradient film by mixing glycidol and monoepoxy-terminated polysiloxane. 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 can...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09D189/00C09D7/12
CPCC09D7/65C09D189/00C08L83/04
Inventor 李天铎许静班青李静朱聪蓝林欣
Owner 山东山科美谷科技发展有限公司
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