CN105177746A - Anti-bacterial Lyocell fiber and preparation method thereof - Google Patents
Anti-bacterial Lyocell fiber and preparation method thereof Download PDFInfo
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- CN105177746A CN105177746A CN201510665876.2A CN201510665876A CN105177746A CN 105177746 A CN105177746 A CN 105177746A CN 201510665876 A CN201510665876 A CN 201510665876A CN 105177746 A CN105177746 A CN 105177746A
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Abstract
The invention discloses anti-bacterial Lyocell fiber and a preparation method of the anti-bacterial Lyocell fiber. The anti-bacterial Lyocell fiber contains nano ZnO of which the mass content is 0.1 to 10 percent, wherein the fineness of the anti-bacterial Lyocell fiber is 1.1 to 4.3 dtex, the strength of the anti-bacterial Lyocell fiber is 1 to 5 cN/dtex, and the elongation at break of the anti-bacterial Lyocell fiber is 8 to 20 percent. A preparation method comprises the steps of uniformly mixing the nano ZnO subjected to surface modification treatment with NMMO (N-Methylmorpholine-N-Oixde) water solution of which the mass concentration is 70 to 87 percent to obtain ZnO-contained NMMO solution; then dissolving cellulose pulp; obtaining the anti-bacterial Lyocell fiber through spinning. The production technology is easy to control and is environment-friendly and pollution-free, industrial production is easy to realize, the nano ZnO is uniformly dispersed in a product, and the anti-bacterial performance of the product is good.
Description
Technical field
The present invention relates to functional fiber cellulose fiber technical field, be specifically related to a kind of Lyocell fiber with antibacterial functions.
Background technology
Cellulose be on the earth reserves at most, the widest natural high polymer of distribution, be the inexhaustible renewable resource of occurring in nature.Cellulose fibre has that intensity is high, dyeability good, spinning performance is good and the advantage such as industrial applications is wide, and therefore, the whole world is continuing to increase the market demand of cellulose fibre in recent years.Lyocell fiber be with renewable resources such as cotton linter, trees, bamboos for raw material, take NMMO as solvent, made by dry-jet wet-spinning, have natural fabric and the many excellent properties of synthetic fiber concurrently, and the cellulose fibre of production process environmental protection.
Lyocell fiber has that intensity is high, dyeability good, spinning performance is good and the advantage such as industrial applications is wide, and compared with viscose, performance is more outstanding, technological process is short and production technology green non-pollution.Therefore, the whole world is continuing to increase the market demand of Lyocell fiber in recent years.
Nano zine oxide (ZnO of ZnO particle diameter between 1-100nm) particle, it is a kind of novel high function fine inorganic product geared to the 21st century, show much special character, as non-migratory, fluorescence, piezoelectricity, absorption and scatters ultraviolet ability etc., utilize its marvellous performance in optical, electrical, magnetic, sensitivity etc., gas sensor, fluorophor, rheostat, UV-preventing material, image recording material, piezoelectric, piezo-resistance, effective catalyst, magnetic material and plastic sheeting etc. can be manufactured.
Nano-ZnO is added in fiber, fiber can be made to have antibacterial bacteriostatic, antiultraviolet, the series of characteristics such as the anti-enzyme of taste of dispelling.But because nano-ZnO has the features such as the large and specific surface energy of specific area is large, self easily reunites; On the other hand, surface of nanometer zinc oxide polarity is stronger, not easily dispersed in organic media, there is the technical problem being difficult to overcome in procedure of fibre production always, especially be difficult to be added in Lyocell fiber, not yet have in the market add nano-ZnO Lyocell fiber correlative study report, also and have no Related product come out.
Summary of the invention
First technical problem to be solved by this invention is: the deficiency existed for prior art, a kind of antibacterial Lyocell fiber containing nano-ZnO is provided, nano-ZnO is dispersed in the middle of Lyocell fiber, makes product have the performances such as good degerming antibacterial, uvioresistant.
Second technical problem to be solved by this invention is: the deficiency existed for prior art, there is provided one using nano-ZnO as antiseptic, add in NMMO solution, preparation has the method for the antibacterial Lyocell fiber of good degerming antibacterial and anti-ultraviolet property.
For solving above-mentioned first technical problem, technical scheme of the present invention is:
A kind of antibacterial Lyocell fiber, containing mass content in described antibacterial Lyocell fiber is the nano-ZnO of 0.1 ~ 10%, and the fiber number 1.1 ~ 4.3dtex of described antibacterial Lyocell fiber, intensity 1 ~ 5cN/dtex, elongation at break are 8 ~ 20%.
For solving above-mentioned second technical problem, technical scheme of the present invention is:
A preparation method for antibacterial Lyocell fiber, comprises the following steps:
(1) by nano-ZnO through surface modification treatment, with mass concentration be 70 ~ 87% NMMO aqueous solution even, mixing temperature is 60 ~ 115 DEG C, and the proportioning of described nano-ZnO and the described NMMO aqueous solution is 0.001 ~ 0.06:1.
(2) the NMMO solution premixed containing ZnO pretreated cellulose pulp and step (1) obtained, premixed temperature is 60 ~ 80 DEG C, and described cellulose pulp is 1:1 ~ 10 with the mixed dissolution proportioning of the NMMO solution containing ZnO.
(3) premixed of step (2) slurry congee is evacuated to-2 × 10 at 80 ~ 120 DEG C
4~-20 × 10
4pa Dehydration obtains spinning solution, and in described spinning solution, content of cellulose is 6 ~ 30wt%, NMMO content is 55 ~ 81wt%, and water content is 7 ~ 15wt%, and nano-ZnO content is 0.06 ~ 6wt%.
(4) by described spinning solution through coagulating bath spinning moulding, obtain described antibacterial Lyocell fiber.
As a kind of technical scheme of improvement, the surface modification treatment of described nano-ZnO comprises: nano-ZnO is milled to particle diameter 1 ~ 100nm, by at least one in silane coupler, phthalate coupling agent, organic silicon solution, after washing immersion 0.5 ~ 10h, dry 0.3 ~ 2h at 70 ~ 120 DEG C, be then again milled to particle diameter 1 ~ 100nm.
As the technical scheme that another kind improves, in step (2), the preliminary treatment of described cellulose pulp comprises after cellulose pulp pulverizing, first activate, and then squeezing obtains the cellulose pulp that moisture content is 30 ~ 70wt%.
As the technical scheme improved further, described activation adds cellulase and lignoenzyme in cellulose pulp after being pulverized, pH value be 5 ~ 6, temperature be 50 ~ 60 DEG C time enzymolysis, described enzymolysis time is 0.5 ~ 2h, and the complete rear adjust ph of enzymolysis is 10 ~ 12 to go out enzyme.
Owing to have employed technique scheme, the invention has the beneficial effects as follows:
Antibacterial Lyocell fiber of the present invention, containing mass content in described antibacterial Lyocell fiber is the nano-ZnO of 0.1 ~ 10%, fiber number 1.1 ~ the 4.3dtex of described antibacterial Lyocell fiber, intensity 1 ~ 5cN/dtex, elongation at break are 8 ~ 20%, because containing nano-ZnO, product not only has the performances such as good degerming antibacterial, uvioresistant, and physical and mechanical properties is excellent.
The preparation method of antibacterial Lyocell fiber of the present invention, by nano-ZnO after surface modification treatment, with mass concentration be 70 ~ 87% NMMO aqueous solution even, obtain the NMMO solution containing ZnO, then dissolving cellulos pulp, spinning prepares antibacterial Lyocell fiber, and production technology easily controls, in product, nano-ZnO is uniformly dispersed, and product anti-microbial property is good.
Due to nano-ZnO is milled to particle diameter 1 ~ 100nm, after silane coupler, phthalate coupling agent, organic silicon solution washing, immersion, drying, again particle diameter 1 ~ 100nm is milled to again, reduce surface polarity and the specific surface energy of nano-ZnO, solve the technical problem that in prior art, nano-ZnO self is easily reunited and should not be disperseed in organic media.
Detailed description of the invention
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
A kind of antibacterial Lyocell fiber, containing mass content in described antibacterial Lyocell fiber is the nano-ZnO of 2.3%, and fiber number 1.1dtex, the intensity 1.5cN/dtex of described antibacterial Lyocell fiber, elongation at break are 10.5%.
Embodiment 2
A kind of antibacterial Lyocell fiber, containing mass content in described antibacterial Lyocell fiber is the nano-ZnO of 4%, and fiber number 2.2dtex, the intensity 2.25cN/dtex of described antibacterial Lyocell fiber, elongation at break are 12.5%.
Embodiment 3
Nano-ZnO is carried out surface modification treatment, is first milled to particle diameter 1 ~ 20nm, after soaking 0.5h with silane coupler solution washing, dry 2h at 80 DEG C, be then again milled to particle diameter 1 ~ 20nm.
By the nano-ZnO through surface modification treatment, with mass concentration be 72% NMMO aqueous solution even, obtain the NMMO solution containing ZnO, mixing temperature is 65 DEG C, and the proportioning of described nano-ZnO and the described NMMO aqueous solution is 0.01:1.
By pretreated cellulose pulp and the NMMO solution premixed containing ZnO, premixed temperature is 65 DEG C, and described cellulose pulp is 1:1 with the mixed dissolution proportioning of the NMMO solution containing ZnO.
Above-mentioned premixed slurry congee is evacuated to-2 × 10 at 120 DEG C
4pa Dehydration obtains spinning solution, and in described spinning solution, content of cellulose is 27wt%, NMMO content is 64wt%, and water content is 8.1wt%, and nano-ZnO content is 0.9wt%.
By described spinning solution through coagulating bath spinning moulding, obtain the antibacterial Lyocell fiber that nano-ZnO content is 3%.
Embodiment 4
Nano-ZnO is carried out surface modification treatment, is first milled to particle diameter 5 ~ 10nm, after soaking 1h with organic silicon solution washing, dry 1h at 90 DEG C, be then again milled to particle diameter 5 ~ 10nm.
By the nano-ZnO through surface modification treatment, with mass concentration be 80% NMMO aqueous solution even, obtain the NMMO solution containing ZnO, mixing temperature is 95 DEG C, and the proportioning of described nano-ZnO and the described NMMO aqueous solution is 0.06:1.
After cellulose pulp is pulverized, first activate, cellulase and lignoenzyme is added in cellulose pulp after being pulverized, pH value be 5, temperature be 50 DEG C time enzymolysis, described enzymolysis time is 1h, the complete rear adjust ph of enzymolysis is 10 to go out enzyme, and then squeezing obtains the cellulose pulp that moisture content is 70wt%.
By above-mentioned pretreated cellulose pulp and the NMMO solution premixed containing ZnO, premixed temperature is 75 DEG C, and described cellulose pulp is 1:3 with the mixed dissolution proportioning of the NMMO solution containing ZnO.
Above-mentioned premixed slurry congee is evacuated to-5 × 10 at 100 DEG C
4pa Dehydration obtains spinning solution, and in described spinning solution, content of cellulose is 9.5wt%, NMMO content is 76wt%, and water content is 13.93wt%, and nano-ZnO content is 0.57wt%.
By described spinning solution through coagulating bath spinning moulding, obtaining nano-ZnO content is 5.5% antibacterial Lyocell fiber.
Embodiment 5
Nano-ZnO is carried out surface modification treatment, is first milled to particle diameter 2 ~ 30nm, after soaking 2h with the washing of phthalate coupling agent, dry 0.5h at 110 DEG C, be then again milled to particle diameter 2 ~ 30nm.
By the nano-ZnO through surface modification treatment, with mass concentration be 85% NMMO aqueous solution even, obtain the NMMO solution containing ZnO, mixing temperature is 100 DEG C, and the proportioning of described nano-ZnO and the described NMMO aqueous solution is 0.005:1.
After cellulose pulp is pulverized, first activate, cellulase and lignoenzyme is added in cellulose pulp after being pulverized, with formic acid adjust ph be 5.5, temperature be 55 DEG C time enzymolysis, described enzymolysis time is 0.5h, the complete rear NaOH adjust ph of enzymolysis is 10.5 to go out enzyme, and then squeezing obtains the cellulose pulp that moisture content is 45wt%.
By above-mentioned pretreated cellulose pulp and the NMMO solution premixed containing ZnO, premixed temperature is 80 DEG C, and described cellulose pulp is 1:7 with the mixed dissolution proportioning of the NMMO solution containing ZnO.
Above-mentioned premixed slurry congee is evacuated to-10 × 10 at 80 DEG C
4pa Dehydration obtains spinning solution, and in described spinning solution, content of cellulose is 6.1wt%, NMMO content is 80.2wt%, and water content is 13.19wt%, and nano-ZnO content is 0.51wt%.
By described spinning solution through coagulating bath spinning moulding, obtain the antibacterial Lyocell fiber that nano-ZnO content is 7.5%.
Experimental example 1
The antibacterial Lyocell fiber prepared by embodiment 1-5 accesses bacterial strain 1 (staphylococcusaureusATCC6538), bacterial strain 2 (EscherichiacoliATCC25922), bacterial strain 3 (PseudomonasaeruginosaATCC27853) respectively, keep the clearance detecting each bacterial strain after 2 hours under normal temperature, result is as table 1.
Table 1
| Project | Bacterial strain 1 clearance (%) | Bacterial strain 2 clearance (%) | Bacterial strain 3 clearance (%) |
| Embodiment 1 | 99.91 | 99.94 | 99.93 |
| Embodiment 2 | 99.98 | 99.92 | 99.93 |
| Embodiment 3 | 99.94 | 99.95 | 99.94 |
| Embodiment 4 | 99.97 | 99.95 | 99.96 |
| Embodiment 5 | 99.95 | 99.96 | 99.96 |
Claims (5)
1. an antibacterial Lyocell fiber, it is characterized in that: containing mass content in described antibacterial Lyocell fiber is the nano-ZnO of 0.1 ~ 10%, and the fiber number 1.1 ~ 4.3dtex of described antibacterial Lyocell fiber, intensity 1 ~ 5cN/dtex, elongation at break are 8 ~ 20%.
2. prepare the method for antibacterial Lyocell fiber as claimed in claim 1, it is characterized in that comprising the following steps:
(1) by nano-ZnO through surface modification treatment, with mass concentration be 70 ~ 87% NMMO aqueous solution even, mixing temperature is 60 ~ 115 DEG C, and the proportioning of described nano-ZnO and the described NMMO aqueous solution is 0.001 ~ 0.06:1;
(2) the NMMO solution premixed containing ZnO pretreated cellulose pulp and step (1) obtained, premixed temperature is 60 ~ 80 DEG C, and described cellulose pulp is 1:1 ~ 10 with the mixed dissolution proportioning of the NMMO solution containing ZnO;
(3) premixed slurry congee step (2) obtained is evacuated to-2 × 10 at 80 ~ 120 DEG C
4~-20 × 10
4pa, Dehydration obtains spinning solution, and in described spinning solution, content of cellulose is 6 ~ 30wt%, NMMO content is 55 ~ 81wt%, and water content is 7 ~ 15wt%, and nano-ZnO content is 0.06 ~ 6wt%;
(4) by described spinning solution through coagulating bath spinning moulding, obtain described antibacterial Lyocell fiber.
3. the preparation method of antibacterial Lyocell fiber as claimed in claim 2, it is characterized in that the surface modification treatment of described nano-ZnO comprises: nano-ZnO is milled to particle diameter 1 ~ 100nm, by at least one in silane coupler, phthalate coupling agent, organic silicon solution, after washing immersion 0.5 ~ 10h, dry 0.3 ~ 2h at 70 ~ 120 DEG C, be then again milled to particle diameter 1 ~ 100nm.
4. the preparation method of antibacterial Lyocell fiber as claimed in claim 2, it is characterized in that: in step (2), the preliminary treatment of described cellulose pulp comprises after cellulose pulp pulverizing, first activate, and then squeezing obtains the cellulose pulp that moisture content is 30 ~ 70wt%.
5. the preparation method of antibacterial Lyocell fiber as claimed in claim 4, it is characterized in that: described activation adds cellulase and lignoenzyme in cellulose pulp after being pulverized, pH value be 5 ~ 6, temperature be 50 ~ 60 DEG C time enzymolysis, described enzymolysis time is 0.5 ~ 2h, and the complete rear adjust ph of enzymolysis is 10 ~ 12 to go out enzyme.
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Cited By (5)
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| CN108842207A (en) * | 2018-07-19 | 2018-11-20 | 赛得利(九江)纤维有限公司 | A kind of preparation method of environment-friendly antibacterial cellulose fibre |
| CN110592694A (en) * | 2019-09-10 | 2019-12-20 | 博富科技股份有限公司 | Zinc oxide powder for antibacterial tencel and preparation method thereof |
| JP2020105686A (en) * | 2018-12-25 | 2020-07-09 | 南亞塑膠工業股▲分▼有限公司 | Deodorizing fibers |
| CN113136632A (en) * | 2021-06-04 | 2021-07-20 | 东华大学 | Preparation method of cellulose functional slurry |
| CN115161841A (en) * | 2022-08-15 | 2022-10-11 | 罗莱生活科技股份有限公司 | Zinc oxide modified fiber blended fabric and preparation method thereof |
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| CN103556235A (en) * | 2013-10-28 | 2014-02-05 | 山东英利实业有限公司 | Preparation technology of cellulose fiber spinning solution |
| CN103556248A (en) * | 2013-10-28 | 2014-02-05 | 山东英利实业有限公司 | Bamboo charcoal Lyocell fiber and preparation process thereof |
| CN104831398A (en) * | 2015-05-13 | 2015-08-12 | 吴江市震宇缝制设备有限公司 | Antibacterial texture sewing fiber and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103172989A (en) * | 2013-04-15 | 2013-06-26 | 杭州昌翔化纤新材料有限公司 | Environment-friendly antibacterial polyester material and preparation method thereof |
| CN103556235A (en) * | 2013-10-28 | 2014-02-05 | 山东英利实业有限公司 | Preparation technology of cellulose fiber spinning solution |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108842207A (en) * | 2018-07-19 | 2018-11-20 | 赛得利(九江)纤维有限公司 | A kind of preparation method of environment-friendly antibacterial cellulose fibre |
| JP2020105686A (en) * | 2018-12-25 | 2020-07-09 | 南亞塑膠工業股▲分▼有限公司 | Deodorizing fibers |
| CN110592694A (en) * | 2019-09-10 | 2019-12-20 | 博富科技股份有限公司 | Zinc oxide powder for antibacterial tencel and preparation method thereof |
| CN113136632A (en) * | 2021-06-04 | 2021-07-20 | 东华大学 | Preparation method of cellulose functional slurry |
| CN115161841A (en) * | 2022-08-15 | 2022-10-11 | 罗莱生活科技股份有限公司 | Zinc oxide modified fiber blended fabric and preparation method thereof |
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Application publication date: 20151223 |