Summary of the invention:
The object of this invention is to provide a kind of preparation method of Multifunction silk filtering material, the method by by silk modified for gel in conjunction with nonwoven fabric technology, make 3 D stereo filtering material, Multifunction silk filtering material prepared by the method has high adsorptivity and gas permeability, and antibacterial bacteriostatic, durable.
Object of the present invention is achieved through the following technical solutions:
A preparation method for Multifunction silk filtering material, comprises the following steps:
(1) silk that will give up is removed after impurity, and cutting gives up the length of silk to below 6cm, then comes unstuck with the sodium carbonate liquor of 0.08g/L, obtains the silk bundle come unstuck after washing drying;
(2) the silk bundle come unstuck step (1) obtained immerses in the mixed solution of TiO 2 sol and fibroin and soaks, and bath raio is 1:40, then impregnated in short gel, takes out after fibroin gel, obtains the silk bundle of gel;
(3), after the gel of the silk bundle removal excess surface of gel step (2) obtained, use warm-up mill cure under pressure, dry through water thorn, obtain Multifunction silk filtering material.
Preferred as technique scheme, the useless silk described in step (1) is the leftover bits and pieces of silk.
Preferred as technique scheme, in the mixed solution described in step (2), the mass fraction of fibroin is 10-15%, and the mass fraction of TiO 2 sol is 5-8%.
Preferred as technique scheme, the time of the immersion described in step (2) is 30-60min.
Preferred as technique scheme, the short gel described in step (2) is the mixture of carboxylic acid and polyethylene glycol, and the mol ratio of carboxylic acid and polyethylene glycol is 1:5.
Preferred as technique scheme, the volume of the short gel described in step (2) is 1/50 of the mixed solution of TiO 2 sol and fibroin.
Preferred as technique scheme, the temperature of the solidification described in step (3) is 30-50 DEG C, and after cure under pressure, the thickness of silk bundle is 1-3cm.
Preferred as technique scheme, the liquid drugs injection aperture of the water thorn described in step (3) is 0.15mm, and the density of liquid drugs injection is 16/cm.
Preferred as technique scheme, the temperature of the oven dry described in step (3) is 70-80 DEG C.
Preferred as technique scheme, the porosity of the Multifunction silk filtering material described in step (3) is 25-33%.
Compared with prior art, the present invention has the following advantages:
(1) main raw material of Multifunction silk filtering material that prepared by this method is silk, and by fibroin and TiO 2 sol process, the main material of filtering material is made to be still silk, therefore filtering material has the excellent properties of silk, possess high adsorptivity and permeability, and also have titanium dioxide in filtering material, therefore possess effect of antibacterial bacteriostatic.
(2) porous gel is applied to filtering material by this preparation method, and fibroin, after being heating and curing, can form the gel rubber material of porous, strengthens the adhesion of silk fiber, and by coated by titanium dioxide wherein, improves functional and durability.
(3) this preparation method finally adopts non-woven middle water thorn technology to reinforce, and is removed by the gel rubber material combined loosely, improves the cohesive force between silk, be prepared into 3 D stereo filtering material.
Detailed description of the invention:
In order to deepen the understanding of the present invention, below in conjunction with embodiment, the invention will be further described, and this embodiment only for explaining the present invention, does not form limiting the scope of the present invention.
Embodiment 1:
After the useless silk of below 6cm is removed impurity, come unstuck with the sodium carbonate liquor of 0.08g/L, after washing drying, obtain the silk bundle come unstuck.
By the silk bundle come unstuck, with bath raio 1:40, immerse in the mixed solution of TiO 2 sol and fibroin and soak 30min, wherein the mass fraction of fibroin is 15%, and the mass fraction of TiO 2 sol is 8%.Then silk bundle is taken out, be soaked in the short gel of carboxylic acid that mol ratio is 1:5 and polyethylene glycol, the consumption of short gel is 1/50 of the mixed liquor volume of TiO 2 sol and fibroin, takes out, obtain the silk bundle of Gel Treatment after fibroin gel.
After the silk bundle of Gel Treatment being removed the gel of excess surface, with warm-up mill pressurization, 30 DEG C are heating and curing, be 16/cm through density, aperture is after the process of 0.15mm water thorn, 70 DEG C of oven dry, obtaining thickness is 1cm, and porosity is the Multifunction silk filtering material of 25%.
Embodiment 2:
After the useless silk of below 6cm is removed impurity, come unstuck with the sodium carbonate liquor of 0.08g/L, after washing drying, obtain the silk bundle come unstuck.
By the silk come unstuck, with bath raio 1:40, immerse in the mixed solution of TiO 2 sol and fibroin and soak 60min, wherein the mass fraction of fibroin is 10%, and the mass fraction of TiO 2 sol is 5%.Then taken out by silk bundle, be soaked in carboxylic acid that mol ratio is 1:5 with the short gel of polyethylene glycol, the consumption urging gel is 1/50 of mixed liquor volume, takes out, obtain the silk bundle of Gel Treatment after fibroin gel.
After the silk of Gel Treatment being removed the gel of excess surface, with warm-up mill pressurization, 50 DEG C are heating and curing, be 16/cm through density, aperture is after the process of 0.15mm water thorn, 80 DEG C of oven dry, obtaining thickness is 3cm, and porosity is the Multifunction silk filtering material of 33%.
Embodiment 3:
After the useless silk of below 6cm is removed impurity, come unstuck with the sodium carbonate liquor of 0.08g/L, after washing drying, obtain the silk bundle come unstuck.
By the silk come unstuck, with bath raio 1:40, immerse in the mixed solution of TiO 2 sol and fibroin and soak 40min, wherein the mass fraction of fibroin is 12%, and the mass fraction of TiO 2 sol is 6%.Then taken out by silk bundle, be soaked in carboxylic acid that mol ratio is 1:5 with the short gel of polyethylene glycol, the consumption urging gel is 1/50 of mixed liquor volume, takes out, obtain the silk of Gel Treatment after fibroin gel.
After the silk bundle of Gel Treatment being removed the gel of excess surface, with warm-up mill pressurization, 40 DEG C are heating and curing, be 16/cm through density, aperture is after the process of 0.15mm water thorn, 75 DEG C of oven dry, obtaining thickness is 2cm, and porosity is the Multifunction silk filtering material of 30%.
Embodiment 4:
After the useless silk of below 6cm is removed impurity, come unstuck with the sodium carbonate liquor of 0.08g/L, after washing drying, obtain the silk bundle come unstuck.
By the silk come unstuck, with bath raio 1:40, immerse in the mixed solution of TiO 2 sol and fibroin and soak 50min, wherein the mass fraction of fibroin is 11%, and the mass fraction of TiO 2 sol is 7%.Then taken out by silk bundle, be soaked in carboxylic acid that mol ratio is 1:5 with the short gel of polyethylene glycol, the consumption urging gel is 1/50 of mixed liquor volume, takes out, obtain the silk of Gel Treatment after fibroin gel.
After the silk bundle of Gel Treatment being removed the gel of excess surface, with warm-up mill pressurization, 40 DEG C are heating and curing, be 16/cm through density, aperture is after the process of 0.15mm water thorn, 75 DEG C of oven dry, obtaining thickness is 1.5cm, and porosity is the Multifunction silk filtering material of 28%.
Embodiment 5:
After the useless silk of below 6cm is removed impurity, come unstuck with the sodium carbonate liquor of 0.08g/L, after washing drying, obtain the silk bundle come unstuck.
By the silk come unstuck, with bath raio 1:40, immerse in the mixed solution of TiO 2 sol and fibroin and soak 60min, wherein the mass fraction of fibroin is 15%, and the mass fraction of TiO 2 sol is 8%.Then taken out by silk bundle, be soaked in carboxylic acid that mol ratio is 1:5 with the short gel of polyethylene glycol, the consumption urging gel is 1/50 of mixed liquor volume, takes out, obtain the silk of Gel Treatment after fibroin gel.
After the silk bundle of Gel Treatment being removed the gel of excess surface, with warm-up mill pressurization, 35 DEG C are heating and curing, be 16/cm through density, aperture is after the process of 0.15mm water thorn, 73 DEG C of oven dry, obtaining thickness is 2.5cm, and porosity is the Multifunction silk filtering material of 30%.
Embodiment 6:
After the useless silk of below 6cm is removed impurity, come unstuck with the sodium carbonate liquor of 0.08g/L, after washing drying, obtain the silk bundle come unstuck.
By the silk come unstuck, with bath raio 1:40, immerse in the mixed solution of TiO 2 sol and fibroin and soak 30min, wherein the mass fraction of fibroin is 10%, and the mass fraction of TiO 2 sol is 5%.Then taken out by silk bundle, be soaked in carboxylic acid that mol ratio is 1:5 with the short gel of polyethylene glycol, the consumption urging gel is 1/50 of mixed liquor volume, takes out, obtain the silk of Gel Treatment after fibroin gel.
After the silk bundle of Gel Treatment being removed the gel of excess surface, with warm-up mill pressurization, 35 DEG C are heating and curing, be 16/cm through density, aperture is after the process of 0.15mm water thorn, 70-80 DEG C of oven dry, obtaining thickness is 2.5cm, and porosity is the Multifunction silk filtering material of 33%.
The adsorption rate of the Multifunction silk filtering material prepared by embodiment 1-6, air penetrability, antibiotic property and mechanical properties results are as shown in the table:
From above-mentioned data, the excellent performance of Multifunction silk filtering material prepared by this method, adsorptivity and gas permeability are all fine, and antibacterial bacteriostatic, and good mechanical property is durable for a long time.