A kind of antibacterial gelatin leather finishing agent containing polysiloxane and quaternary ammonium salt and preparation method thereof

Abstract

The invention relates to an antibacterial gelatin leather finishing agent containing polysiloxane and a quaternary ammonium salt and a preparation method thereof. The gelatin is dissolved in water to prepare an aqueous solution with a concentration of 2 to 20%, and the gelatin is prepared at 40 to 70°C and the pH is Under the condition of 6~12, add epoxy quaternary ammonium salt in the 1st reaction bottle, obtain solution 1; Add surfactant in the 2nd reaction bottle, the consumption of surfactant is 2~20% of gelatin quality, Continue stirring while adding the epoxypolysiloxane containing Si-O-Si repeating units batchwise or continuously to obtain solution 2. Mix solution 1 and solution 2 in different proportions, weigh 15-20g and place it in a polytetrafluoroethylene mold, add 5-10mL of ethanol, tetrahydrofuran, methanol or a mixture of two or three solvents, and store at 40-80°C Dry in an oven at normal pressure to obtain a multifunctional gelatin leather finishing agent. The coating agent has the characteristics of antibacterial, adjustable hydrophilicity and hydrophobicity, soft film formation, and strong oxidation resistance.

Description

technical field

[0001] The invention relates to a gelatin leather finishing agent, in particular to an antibacterial gelatin leather finishing agent containing polysiloxane and quaternary ammonium salt and a preparation method thereof. The leather finishing agent has the characteristics of antibacterial, adjustable hydrophilicity and hydrophobicity, anti-oxidation, etc., and is especially suitable as a finishing agent for garment leather or decorative leather. Background technique

[0002] Protein finishes are important raw materials for the leather industry. The polypeptide main chain structure endows the protein coating agent with soft and natural luster, strong cohesive force and good hygienic properties such as air permeability and water vapor permeability. Gelatin is a hydrolyzed product of collagen protein, which has become an important raw material for the preparation of protein films. Like other natural polymer materials, after forming a film, this kind of protein m...

Examples

Embodiment 1

[0058] Add 12 grams of gelatin (accounting for 11.76% of the total mass) and 85 grams of deionized water into a 250ml three-neck reaction bottle equipped with a thermometer socket, a sampling port, and a condenser socket, stir and heat to 50°C. After the gelatin is completely dissolved, add 0.25mL of 3 mol / L sodium hydroxide, adjust the reaction pH to 10.0, add 8g of epoxy quaternary ammonium salt, after the reactants are not safely dissolved, continue to stir for 8 hours to prepare epoxy quaternary ammonium salt graft modified gelatin polymerization solution (Solution 1).

[0059] The infrared spectrogram of epoxy quaternary ammonium salt modified gelatin ( figure 2 ), the original 1643cm -1 The N~H absorption peak of the primary amino group disappears, and at the same time at 1475cm -1 -N(CH 3 ) 3 C-H new absorption peaks. One N-H absorption peak that appeared in the spectrum disappeared, and one ~N(CH 3 ) 3 The characteristic absorption peak of C-H on the top indica...

Embodiment 2

[0065] The described method is the same as that in Example 1, except that the mass of gelatin is changed to 3 grams (accounting for 2.83% of the total mass), the pH is changed to 6.0, and the mixture is heated and stirred to 40°C.

[0066] The viscosity of the obtained liquid is ~360 centipoise (50°C), and it is placed in a normal-pressure oven at 50°C for 6 hours to form a film with strong flexibility. The glass transition temperature (T g ) is 224℃, the T of gelatin film after modification g The temperature dropped to 196°C; the antibacterial rate of raw gelatin film against Escherichia coli was 18.3%, and that of the modified gelatin film increased to 86.2%, and the antibacterial rate increased significantly. 13 C NMR showed that the γ-C signal on the lysine and arginine molecules on the gelatin molecule in the glycidol-modified gelatin product disappeared, and new peaks appeared at 61 and 63ppm, which were - C Peaks of HOH- groups; new peaks appeared at 69 and 72ppm a...

Embodiment 3

[0070] The described method is consistent with that of Example 1, except that the mass of gelatin is changed to 16 grams (accounting for 15.09% of the total mass), the pH is changed to 12.0, and the mixture is heated and stirred to 40°C.

[0071] The viscosity of the obtained liquid is ~460 centipoise (50°C), and it is placed in a normal-pressure oven at 50°C for 6 hours to form a film with strong flexibility. The glass transition temperature (T g ) is 224℃, the T of gelatin film after modification g The antibacterial rate of raw gelatin film against Escherichia coli was 18.3%, and that of the modified gelatin film increased to 68.4%, and the antibacterial rate increased significantly. 13 C NMR showed that the γ-C signal on the lysine and arginine molecules on the gelatin molecule in the glycidol-modified gelatin product disappeared, and new peaks appeared at 61 and 63ppm, which were - C Peaks of HOH- groups; new peaks appeared at 69 and 72ppm as- C h 2 OH group peak;...

technical field

[0001] The invention relates to a gelatin leather finishing agent, in particular to an antibacterial gelatin leather finishing agent containing polysiloxane and quaternary ammonium salt and a preparation method thereof. The leather finishing agent has the characteristics of antibacterial, adjustable hydrophilicity and hydrophobicity, anti-oxidation, etc., and is especially suitable as a finishing agent for garment leather or decorative leather. Background technique

[0002] Protein finishes are important raw materials for the leather industry. The polypeptide main chain structure endows the protein coating agent with soft and natural luster, strong cohesive force and good hygienic properties such as air permeability and water vapor permeability. Gelatin is a hydrolyzed product of collagen protein, which has become an important raw material for the preparation of protein films. Like other natural polymer materials, after forming a film, this kind of protein m...

Examples

Embodiment 1

[0058] Add 12 grams of gelatin (accounting for 11.76% of the total mass) and 85 grams of deionized water into a 250ml three-neck reaction bottle equipped with a thermometer socket, a sampling port, and a condenser socket, stir and heat to 50°C. After the gelatin is completely dissolved, add 0.25mL of 3 mol / L sodium hydroxide, adjust the reaction pH to 10.0, add 8g of epoxy quaternary ammonium salt, after the reactants are not safely dissolved, continue to stir for 8 hours to prepare epoxy quaternary ammonium salt graft modified gelatin polymerization solution (Solution 1).

[0059] The infrared spectrogram of epoxy quaternary ammonium salt modified gelatin ( figure 2 ), the original 1643cm -1 The N~H absorption peak of the primary amino group disappears, and at the same time at 1475cm -1 -N(CH 3 ) 3 C-H new absorption peaks. One N-H absorption peak that appeared in the spectrum disappeared, and one ~N(CH 3 ) 3 The characteristic absorption peak of C-H on the top indica...

Embodiment 2

[0065] The described method is the same as that in Example 1, except that the mass of gelatin is changed to 3 grams (accounting for 2.83% of the total mass), the pH is changed to 6.0, and the mixture is heated and stirred to 40°C.

[0066] The viscosity of the obtained liquid is ~360 centipoise (50°C), and it is placed in a normal-pressure oven at 50°C for 6 hours to form a film with strong flexibility. The glass transition temperature (T g ) is 224℃, the T of gelatin film after modification g The temperature dropped to 196°C; the antibacterial rate of raw gelatin film against Escherichia coli was 18.3%, and that of the modified gelatin film increased to 86.2%, and the antibacterial rate increased significantly. 13 C NMR showed that the γ-C signal on the lysine and arginine molecules on the gelatin molecule in the glycidol-modified gelatin product disappeared, and new peaks appeared at 61 and 63ppm, which were - C Peaks of HOH- groups; new peaks appeared at 69 and 72ppm a...

Embodiment 3

[0070] The described method is consistent with that of Example 1, except that the mass of gelatin is changed to 16 grams (accounting for 15.09% of the total mass), the pH is changed to 12.0, and the mixture is heated and stirred to 40°C.

[0071] The viscosity of the obtained liquid is ~460 centipoise (50°C), and it is placed in a normal-pressure oven at 50°C for 6 hours to form a film with strong flexibility. The glass transition temperature (T g ) is 224℃, the T of gelatin film after modification g The antibacterial rate of raw gelatin film against Escherichia coli was 18.3%, and that of the modified gelatin film increased to 68.4%, and the antibacterial rate increased significantly. 13 C NMR showed that the γ-C signal on the lysine and arginine molecules on the gelatin molecule in the glycidol-modified gelatin product disappeared, and new peaks appeared at 61 and 63ppm, which were - C Peaks of HOH- groups; new peaks appeared at 69 and 72ppm as- C h 2 OH group peak;...

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