CN104611913A - Preparation method of novel multifunctional silk filtering material - Google Patents

Preparation method of novel multifunctional silk filtering material Download PDF

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Publication number
CN104611913A
CN104611913A CN201510055874.1A CN201510055874A CN104611913A CN 104611913 A CN104611913 A CN 104611913A CN 201510055874 A CN201510055874 A CN 201510055874A CN 104611913 A CN104611913 A CN 104611913A
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silk
filtering material
multifunction
preparation
gel
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CN201510055874.1A
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CN104611913B (en
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陈永林
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Chongqing green edge leather products Co., Ltd.
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HUZHOU XINCHUANG SILK CO Ltd
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Abstract

The invention discloses a preparation method of a novel multifunctional silk filtering material. The method comprises the following steps: after silk is degummed, dipping the silk into a mixed solution of titanium dioxide sol and silk protein, soaking the silk in a gel promoter, taking out the silk, heating for curing the silk, and carrying out spun-laced drying on the silk, so that the novel multifunctional silk filtering material is obtained. The preparation method is simple, and combines a gel technology with a spun-laced nonwoven technology, and therefore, the method is suitable for mass production. The novel multifunctional silk filtering material prepared by using the method has high adsorbability and air permeability, and is antibacterial, bacteriostatic and durable.

Description

A kind of preparation method of Multifunction silk filtering material
Technical field:
The invention belongs to silk product technical field, particularly a kind of preparation method of Multifunction silk filtering material.
Background technology:
Current micro-nano granules thing dust has become the emphasis of urban atmospheric pollution thing control, and current high-effective dust-removing technology has bag type dust removing technology and electrostatic precipitator technology, but electrostatic precipitator technology is difficult to reach pollutant emission standard.The dust-proof filtering material used of pocket type mostly is that prepared by non-weaving cloth, also referred to as fiber filtering.Fiber filtering comprises non-woven filtrate and woven filtrate, non-woven filtrate is three-dimensional structure, possesses Graded Density, and woven filtrate limits by structural parameters, therefore non-woven filtrate possesses that filter efficiency is high, dust containing capacity is large, toxicity is low, cost is low, and the feature of easy other filter material compounds.
Take silk as the excellent performance of fiber filtering prepared by raw material, because the parallel distribution of the basic stratiform of the fibril of silk, short texture, and in fibrillar structure, there is a lot of micropore, therefore the porosity of the internal structure of the silk fiber fiber filtering that makes it prepare is high, permeability is good, and has research display silk to have extraordinary adsorption rate to the aldehyde material in cigarette, and finds much less than cellulose diacetate fibers of the change of silk temperature in adsorption process.
Chinese patent CN 101892608A (publication date 2010.11.24) discloses a kind of technique utilizing silk offcut to produce sterilization mask paper, break into fiber pulp after being sheared by silk, after adding chemical addition agent and photochemical catalyst, be prepared into sterilization mask paper.Chinese patent CN100588336C (publication date 2007.09.12) discloses cocoon fibre cigarette filter tip and preparation method thereof, is be filter core by silk fiber, and fibroin and alginate are sizing, and binding material is coated on the preparation of silk fiber surface.At present silk fiber mostly is directly as fibrous filter prepared by raw material that silk fiber is carried out arrangements processing is prepared into filtering material, it is functional relies on and characteristic of silk itself more, and therefore filtering material is functional not good enough.
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.

Claims (10)

1. a preparation method for Multifunction silk filtering material, is characterized in that, the method 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.
2. the preparation method of a kind of Multifunction silk filtering material as claimed in claim 1, it is characterized in that, the useless silk described in step (1) is the leftover bits and pieces of silk.
3. the preparation method of a kind of Multifunction silk filtering material as claimed in claim 1, it is characterized in that, 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%.
4. the preparation method of a kind of Multifunction silk filtering material as claimed in claim 1, is characterized in that, the time of the immersion described in step (2) is 30-60min.
5. the preparation method of a kind of Multifunction silk filtering material as claimed in claim 1, is characterized in that, 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.
6. the preparation method of a kind of Multifunction silk filtering material as claimed in claim 1, is characterized in that, the volume of the short gel described in step (2) is 1/50 of the mixed solution of TiO 2 sol and fibroin.
7. the preparation method of a kind of Multifunction silk filtering material as claimed in claim 1, it is characterized in that, 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.
8. the preparation method of a kind of Multifunction silk filtering material as claimed in claim 1, is characterized in that, 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.
9. the preparation method of a kind of Multifunction silk filtering material as claimed in claim 1, is characterized in that, the temperature of the oven dry described in step (3) is 70-80 DEG C.
10. the preparation method of a kind of Multifunction silk filtering material as claimed in claim 1, is characterized in that, the porosity of the Multifunction silk filtering material described in step (3) is 25-33%.
CN201510055874.1A 2015-02-03 2015-02-03 A kind of preparation method of Multifunctional silk filtering material Expired - Fee Related CN104611913B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108978032A (en) * 2018-08-01 2018-12-11 苏州汪永亨丝绸科技文化有限公司 A kind of production method of novel silk fabric
CN114515457A (en) * 2021-12-31 2022-05-20 杭州科百特过滤器材有限公司 Resin bonding and curing filter element and preparation method and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002363861A (en) * 2001-06-05 2002-12-18 Hiromoto Uejima Method for carrying out silk fibroin processing of fiber or fiber product
CN101498061A (en) * 2009-03-05 2009-08-05 浙江大学 Method for improving antibiosis of silk fibroin material
CN101619541A (en) * 2009-08-10 2010-01-06 浙江理工大学 Green-fabrics finishing method
CN104311848A (en) * 2014-09-25 2015-01-28 苏州印丝特纺织数码科技有限公司 Preparation method of regenerated fibroin-nano titanium oxide composite membrane

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002363861A (en) * 2001-06-05 2002-12-18 Hiromoto Uejima Method for carrying out silk fibroin processing of fiber or fiber product
CN101498061A (en) * 2009-03-05 2009-08-05 浙江大学 Method for improving antibiosis of silk fibroin material
CN101619541A (en) * 2009-08-10 2010-01-06 浙江理工大学 Green-fabrics finishing method
CN104311848A (en) * 2014-09-25 2015-01-28 苏州印丝特纺织数码科技有限公司 Preparation method of regenerated fibroin-nano titanium oxide composite membrane

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108978032A (en) * 2018-08-01 2018-12-11 苏州汪永亨丝绸科技文化有限公司 A kind of production method of novel silk fabric
CN114515457A (en) * 2021-12-31 2022-05-20 杭州科百特过滤器材有限公司 Resin bonding and curing filter element and preparation method and application thereof

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Inventor after: Chen Hongyu

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Address after: Guilin street 402660 Chongqing city Tongnan District Chunyang Road No. 274

Applicant after: Chongqing green edge leather products Co., Ltd.

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