CN103668520A - Antibacterial regenerated cellulose fiber and preparation method thereof - Google Patents
Antibacterial regenerated cellulose fiber and preparation method thereof Download PDFInfo
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- CN103668520A CN103668520A CN201310648661.0A CN201310648661A CN103668520A CN 103668520 A CN103668520 A CN 103668520A CN 201310648661 A CN201310648661 A CN 201310648661A CN 103668520 A CN103668520 A CN 103668520A
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Abstract
The invention discloses an antibacterial regenerated cellulose fiber and a preparation method thereof, and the antibacterial cellulose fiber contains 0.5 ~ 10wt% of chitosan quaternary ammonium salt, the preparation method comprises the following steps: (1) preparing the chitosan quaternary ammonium salt with deionized water and sodium hydroxide into an antibacterial solution; (2) using cellulose pulp as a raw material to prepare spinning viscose; (3) adding the antibacterial solution to a viscose solution of any step from the yellowing step to before spinning, with the adding amount of the chitosan quaternary ammonium salt being 0.5 ~ 10% of the weight of alpha cellulose in the viscose solution, to obtain an antibacterial spinning viscose solution; and (4) obtaining the antibacterial regenerated cellulose fiber by coagulating bath spinning and drawing molding of the antibacterial spinning viscose solution, and then refining and drying. The antibacterial regenerated cellulose fiber simultaneously has biodegradability, biocompatibility, safety and antibacterial property and other excellent properties, and has better moisture absorption and moisture preservation, crease resistance and softness.
Description
Technical field
The present invention relates to functional fiber cellulose fiber, be specifically related to a kind of antibacterial regenerated celulose fibre and technology of preparing thereof that chitosan derivatives is antiseptic of take.
Background technology
Shitosan is the alkaline polysaccharide of the unique existence of occurring in nature, has the premium properties such as biodegradability, biocompatibility, security and antibiotic property.Due to the anti-microbial property that shitosan has, it obtains a wide range of applications at aspects such as wound suture, processing vegetable seeds, disinfectant, hand cleanser.Shitosan is obtained to quaternary chitosan derivatives material by modification, is one of important research direction improving chitosan anti-bacteria, is also the hot fields of anti-mattress investigation of materials.
Wherein, chitosan quaternary ammonium salt is a kind of important chitosan derivatives, has the features such as nontoxic, antibacterial and bacteriostatic activity is good, thereby is widely used in the technical fields such as preparation of environmental protection, food processing, drug loading, controlled release and antibacterial bacteriostatic material.The special molecular structure that shitosan and quaternary ammonium salt thereof have can be used for improving moisture absorbability and moisture retentivity, antistatic behaviour, antibiotic property, wrinkle resistance, the flexibility of fabric, and dyeability.
Although chitosan quaternary ammonium salt can give textiles many premium properties, in the application of field of textiles, be mainly to use it as after-finishing of textile products agent, during use, mostly adopt traditional rear finishing technique, make the function of giving fabric can not get lasting maintenance.The chitosan quaternary ammonium salt antibiotic finishing method of patent documentation CN201310119583.5 jean cloth as has been publicly, CN200910200566.8 water-soluble chitosan quaternary ammonium salt antibiotic finishing agent and preparation thereof and application, CN201310119582.0 jean cloth antibacterial finishing process chitosan quaternary ammonium salt dressing liquid is all the technology that adopt chitosan quaternary ammonium salt pair fabric to carry out rear arrangement in these documents.Therefore, the various premium properties that have according to shitosan and derivative thereof, improve the process technology of the textiles of chitosan quaternary ammonium salt pair variety classes and material, will greatly promote its application development at field of textiles.
Viscose is as regenerated celulose fibre, it is good that its goods have sucting wet air permeability, feature comfortable and easy to wear, in prior art, feature based on cellulose viscose manufacturing technique length, complex process, in recent years, along with the appearance of various functional viscose fibers, various antibacterial viscose fibers also arise at the historic moment, wherein also have use shitosan to viscose modification prepare the research report of antibacterial viscose fiber.Example is the manufacture method of patent documentation CN201010200183.3 hydroxyethyl chitosan modified viscose fiber as has been publicly, CN200610015705.6 hydroxyethyl chitosan modified viscose fiber and manufacture method thereof, all to use hydroxyethyl chitosan to carry out modification to cellulose fibre, due to after shitosan directly adds in viscose solution, viscose solution there will be gelatin phenomenon, affect spinning spinnability, therefore in prior art, all to carry out the alkalization of chitosan derivatives, the process treatment process that yellow etc. are complicated, therefore not only exist technological process long, equipment investment is large, the problem of complex process, and the anti-microbial property of the antibacterial viscose fiber preparing is barely satisfactory, even do not reach the antibacterial index of national regulation, cause the industrialization of chitosan anti-bacteria cellulose fibre to be restricted.
Summary of the invention
First technical problem to be solved by this invention is: for the poor problem of antibacterial regenerated celulose fibre anti-microbial property of the prior art, provide a kind of chitosan quaternary ammonium salt that uses as the antibacterial regenerated celulose fibre of antibacterial modified dose, the bacteriostatic activity of this anti-bacterial fibre cellulose fiber and bactericidal activity are all stipulated over GB.
Second technical problem to be solved by this invention is: long for the antibacterial regenerated celulose fibre technological process of production in prior art, equipment investment is large, complex process, and the poor problem of antibacterial regenerated celulose fibre antibiotic property of preparation, provides that a kind of technological process is short, technique is simple, the preparation method of the bacteriostatic activity of the anti-bacterial fibre cellulose fiber of preparation and the high antibacterial regenerated celulose fibre of bactericidal activity.
For solving above-mentioned first technical problem, technical scheme of the present invention is:
A kind of antibacterial regenerated celulose fibre, the chitosan quaternary ammonium salt that contains 0.5～10wt% in described antibacterial regenerated celulose fibre, substitution value >=80% of described chitosan quaternary ammonium salt, bacteriostatic activity value >=2.5 of described antibacterial regenerated celulose fibre, bactericidal activity value >=1.0.
As a kind of preferred, described chitosan quaternary ammonium salt is hydroxypropyl alkyl ammomium chloride shitosan.
As further preferred, described chitosan quaternary ammonium salt comprises at least one in HACC, hydroxypropyl alkyl-dimethyl ammonium chloride shitosan.
As further preferred, described chitosan quaternary ammonium salt is HACC.
For solving above-mentioned second technical problem, technical scheme of the present invention is:
A preparation method for antibacterial regenerated celulose fibre, comprises the following steps:
(1) deionized water, NaOH for chitosan quaternary ammonium salt are made into antiseptic solution, in described antiseptic solution, the mass concentration of chitosan quaternary ammonium salt is 1～10%, and the mass concentration of NaOH is 5～15%.
(2) adopting cellulose pulp is raw material, through comprising that dipping, squeezing, pulverizing, experienced, yellow step make cellulose sulfonate, and then make spinning viscose through dissolving, deaeration and filtration step.
(3) antiseptic solution step (1) being prepared adds yellow step in step (2) to the viscose solution in arbitrary step before spinning, the addition of described chitosan quaternary ammonium salt be in viscose solution chemical cellulose weight 0.5～10%, obtain antibacterial spinning viscose solution.
(4) by described antibacterial spinning viscose solution through coagulating bath spinning, draw forming, then through refining, dry and to obtain described antibacterial regenerated celulose fibre.
As a kind of improvement, in step (3), add and in the viscose solution before described antiseptic solution, contain chemical cellulose 8.5～10wt%, NaOH 4～5wt%, the viscosity of viscose solution is the viscosity that 30～60s(falling ball method is measured), add in the antibacterial spinning viscose solution after described antiseptic solution and contain chemical cellulose 7～9.5wt%, NaOH 4.5～7wt%, the viscosity of antibacterial spinning viscose solution is 30～55s.
As a kind of preferred, the temperature of described coagulating bath is 40～60 ℃, sulfur acid 90～130g/l, zinc sulfate and/or aluminum sulfate 5～15g/l, sodium sulphate 270～350g/l in described coagulating bath.
As a kind of preferred, the total stretch ratio of described drawing-off is 30～200%.
As a kind of preferred, described chitosan quaternary ammonium salt is hydroxypropyl alkyl ammomium chloride shitosan, substitution value >=80% of described chitosan quaternary ammonium salt.
As further preferred, described chitosan quaternary ammonium salt comprises at least one in HACC, hydroxypropyl alkyl-dimethyl ammonium chloride shitosan.
As further preferred, described chitosan quaternary ammonium salt is HACC.
Owing to having adopted technique scheme, the invention has the beneficial effects as follows:
Antibacterial regenerated celulose fibre of the present invention, adopt chitosan quaternary ammonium salt as chitosan antimicrobial agent, the antibiotic property mechanism of chitosan quaternary ammonium salt is, primary amine groups on shitosan and chitosan oligosaccharide C2 becomes the unique alkalescence sugar of occurring in nature, and being nearly all acidity, bacterium surface make shitosan and chitosan oligosaccharide there is biocidal property, and quaternary ammonium group CATION is passed through electrostatic force, the effects such as hydrophobic binding between hydrogen bond and protein molecule, adsorb electronegative bacterial body, be gathered on cell membrane, can form polyelectrolyte polymer, at cell peripheral, form and do not there is infiltrative top layer, stop nutriment to see through cell membrane and make bacterium can not carry out metabolism, generating chamber's inhibition effect, can cause bacterial growth suppressed and dead.The good bacteriostasis property having due to chitosan quaternary ammonium salt self, with the good blended characteristic with spinning viscose, the antibacterial regenerated celulose fibre that the present invention makes has the premium properties such as biodegradability, biocompatibility, security and antibiotic property simultaneously, antibacterial functions is lasting, human body is had no side effect, and gives the premium properties such as the better moisture-absorbing moisture-keeping of viscose, wrinkle resistance, flexibility simultaneously.The antibacterial regenerated celulose fibre that the present invention prepares all has good bacteriostasis to gram-positive bacteria and Gram-negative bacteria, and total bacteriostasis rate reaches more than 95%.
In prior art, due to after shitosan and derivative thereof add in viscose solution, can cause viscose glue to occur gelatin phenomenon, thereby affect spinning spinnability, and affect fungistatic effect, therefore those skilled in the art generally believe, before co-blended spinning, the derivative of shitosan or shitosan first should be alkalized, after yellow, obtain the xanthogenate solution of shitosan or chitosan derivatives, and then with spinning viscose blend after spinning, the spinning spinnability of guarantee process stabilizing.But this process not only exists complex process, production procedure long, the problem such as equipment investment is large, and use carbon disulfide during yellow, also there is work and problem of environmental pollution.And the inventor is devoted for years in the research of cellulose fibre and functional fiber cellulose fiber, through the research and analysis of cellulose and chitosan structure are found, cellulose and shitosan have closely similar molecular structure, with hydroxypropyl alkyl ammomium chloride shitosan difference be only hydroxypropyl alkyl ammomium chloride and the hydroxyl of C2 on glucose ring, structural similitude, makes the two should have good compatibility.Therefore, after through lot of experiments checking, the present invention has broken that those skilled in the art think must be first by after the derivative xanthic acid esterification of shitosan or shitosan with the technical conceive of viscose solution blend, but chitosan quaternary ammonium salt is dissolved in sodium hydroxide solution, then directly and spinning after viscose solution blend, not only simplified production stage, reduced equipment investment, work and environmental pollution have been alleviated, and adopting chitosan quaternary ammonium salt as bactericide, the antibacterial cellulose fibre antibacterial effect preparing is more excellent.
Spinning spinnability in viscose preparation, especially the spinning spinnability of functional viscose fiber, owing to having sneaked into functional materials in viscose solution, therefore when spinning, the performance indications of viscose solution, the matching of viscose solution and coagulating bath is all the deciding factor that determines spinning spinnability and functional fiber quality, the applicant determines by lot of experiment validation, in viscose solution before adding antiseptic solution, contain chemical cellulose 8.5～10wt%, NaOH 4～5wt%, the viscosity of viscose solution is the viscosity that 30～60s(falling ball method is measured), add in the antibacterial spinning viscose solution after antiseptic solution and contain chemical cellulose 7～9.5wt%, NaOH 4.5～7wt%, the viscosity of antibacterial spinning viscose solution is 30～55s, employing is suitable for the viscose solution of spinning moulding, it is the further safeguard measure of the performance indications of the spinning spinnability that guaranteed and finished product anti-bacterial fibre cellulose fiber.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.
Embodiment 1
An antibacterial regenerated celulose fibre, the chitosan quaternary ammonium salt that contains 1.5wt% in described antibacterial regenerated celulose fibre, the substitution value of described chitosan quaternary ammonium salt is 85%, the bacteriostatic activity value 3.2 of described antibacterial regenerated celulose fibre, bactericidal activity value 1.55.
Embodiment 2
A kind of antibacterial regenerated celulose fibre, the HACC that contains 3.5wt% in described antibacterial regenerated celulose fibre, the substitution value of described HACC is 94, the bacteriostatic activity value 4.2 of described antibacterial regenerated celulose fibre, bactericidal activity value 2.58.
Embodiment 3
A kind of antibacterial regenerated celulose fibre, the hydroxypropyl alkyl-dimethyl ammonium chloride shitosan that contains 7.5wt% in described antibacterial regenerated celulose fibre, the substitution value of described HACC is 92%, the bacteriostatic activity value 3.95 of described antibacterial regenerated celulose fibre, bactericidal activity value 1.9.
Embodiment 4
A preparation method for antibacterial regenerated celulose fibre, comprises the following steps:
(1) the hydroxypropyl alkyl ammomium chloride that is 88% by substitution value for shitosan deionized water, NaOH be made into antiseptic solution, in described antiseptic solution, the mass concentration of hydroxypropyl alkyl ammomium chloride shitosan is 3%, the mass concentration of NaOH is 8%.
(2) adopting cellulose pulp is raw material, through comprising that dipping, squeezing, pulverizing, experienced, yellow step make cellulose sulfonate, and then make spinning viscose through dissolving, deaeration and filtration step.
(3) antiseptic solution use step (1) being prepared is spun front injection and is added in the viscose solution before spinning, the addition of described hydroxypropyl alkyl ammomium chloride shitosan be in viscose solution chemical cellulose weight 1.5%, obtain antibacterial spinning viscose solution.
(4) by described antibacterial spinning viscose solution through coagulating bath spinning, draw forming, then through refining, dry and to obtain described antibacterial regenerated celulose fibre.
Embodiment 5
A preparation method for antibacterial regenerated celulose fibre, comprises the following steps:
(1) deionized water, the NaOH for HACC that by substitution value, are 90% are made into antiseptic solution, and in described antiseptic solution, the mass concentration of NaOH is 10%.
(2) adopting cellulose pulp is raw material, through comprising that dipping, squeezing, pulverizing, experienced, yellow step make cellulose sulfonate, and then make spinning viscose through dissolving, deaeration and filtration step.
(3) antiseptic solution step (1) being prepared adds in step (2) in yellow step in cellulose yellow acid fat, then dissolve and obtain viscose solution, the addition of described HACC be in viscose solution chemical cellulose weight 2.5%, obtain antibacterial spinning viscose solution; Add and in the viscose solution before described antiseptic solution, contain chemical cellulose 8.5wt%, NaOH 4wt%, the viscosity of viscose solution is the viscosity that 45s(falling ball method is measured), add in the antibacterial spinning viscose solution after described antiseptic solution and contain chemical cellulose 7wt%, NaOH 4.5wt%, the viscosity of antibacterial spinning viscose solution is 43s.
(4) by described antibacterial spinning viscose solution through coagulating bath spinning, draw forming, then through refining, dry and to obtain described antibacterial regenerated celulose fibre.
Embodiment 6
A preparation method for antibacterial regenerated celulose fibre, comprises the following steps:
(1) deionized water, the NaOH for HACC that by substitution value, are 92% are made into antiseptic solution, and in described antiseptic solution, the mass concentration of HACC is 5%, and the mass concentration of NaOH is 15%.
(2) adopting cellulose pulp is raw material, through comprising that dipping, squeezing, pulverizing, experienced, yellow step make cellulose sulfonate, and then make spinning viscose through dissolving, deaeration and filtration step.
(3) antiseptic solution step (1) being prepared adds in the viscose solution in the middle dissolving step of step (2), the addition of described HACC be in viscose solution chemical cellulose weight 7.0%, obtain antibacterial spinning viscose solution; Add and in the viscose solution before described antiseptic solution, contain chemical cellulose 9.2wt%, NaOH 4.5wt%, the viscosity of viscose solution is the viscosity that 50s(falling ball method is measured), add in the antibacterial spinning viscose solution after described antiseptic solution and contain chemical cellulose 8.7wt%, NaOH 5.6wt%, the viscosity of antibacterial spinning viscose solution is 47s.
(4) by described antibacterial spinning viscose solution through coagulating bath spinning, draw forming, then through refining, oven dry, obtain described antibacterial regenerated celulose fibre, the temperature of described coagulating bath is 51 ℃, sulfur acid 100g/l, zinc sulfate 9.5g/l, sodium sulphate 290g/l in described coagulating bath, the total stretch ratio of described drawing-off is 50%.
Embodiment 7
A preparation method for antibacterial regenerated celulose fibre, comprises the following steps:
(1) the hydroxypropyl alkyl-dimethyl ammonium chloride that is 95% by substitution value for shitosan deionized water, NaOH be made into antiseptic solution, in described antiseptic solution, the mass concentration of hydroxypropyl alkyl-dimethyl ammonium chloride shitosan is 2.5%, and the mass concentration of NaOH is 12%.
(2) adopting cellulose pulp is raw material, through comprising that dipping, squeezing, pulverizing, experienced, yellow step make cellulose sulfonate, and then make spinning viscose through dissolving, deaeration and filtration step.
(3) antiseptic solution step (1) being prepared adds in the viscose solution in the middle maturation step of step (2), the addition of described hydroxypropyl alkyl-dimethyl ammonium chloride shitosan be in viscose solution chemical cellulose weight 5.0%, obtain antibacterial spinning viscose solution; Add and in the viscose solution before described antiseptic solution, contain chemical cellulose 9.5wt%, NaOH 5wt%, the viscosity of viscose solution is the viscosity that 55s(falling ball method is measured), add in the antibacterial spinning viscose solution after described antiseptic solution and contain chemical cellulose 9.2wt%, NaOH 6.5wt%, the viscosity of antibacterial spinning viscose solution is 53s.
(4) by described antibacterial spinning viscose solution through coagulating bath spinning, draw forming, then through refining, oven dry, obtain described antibacterial regenerated celulose fibre, the temperature of described coagulating bath is 55 ℃, sulfur acid 125g/l, aluminum sulfate 12g/l, sodium sulphate 320g/l in described coagulating bath, the total stretch ratio of described drawing-off is 120%.
Comparative example 1
Comparative example 1 is that with the difference of embodiment 6 antiseptic using is hydroxyethyl chitosan, and all the other are all identical.
Comparative example 2
Comparative example 2 is with the difference of embodiment 6: step (1) is when preparing antiseptic solution, adopt alkalization, the yellow technique of HACC to prepare: 1. alkalization: deionized water, dissolution of sodium hydroxide for HACC are become to alkalizing solution, in described alkalizing solution, the mass concentration of HACC is 5%, and the mass concentration of NaOH is 15%; 2. xanthic acid esterification reaction: the alkalizing solution of gained HACC in is 1. placed in to capping still, the carbon disulfide that adds HACC quality 45%, keeping reaction temperature is 15 ℃, yellow is reacted 4 hours, obtains the antiseptic solution of HACC xanthate.
Comparative example 3
Comparative example 3 is with the difference of comparative example 2: the antiseptic of use is hydroxyethyl chitosan, and all the other are all identical.
Anti-microbial property and the mechanical performance index situation of the anti-bacterial fibre that embodiment 4-7 and comparative example 1-3 prepare see the following form.While detecting anti-microbial property, testing bacterial classification is: staphylococcus aureus ATCC6538, and by the test of JIS L1902-2008 textile fabrics antibacterial activity, inoculation bacterial concentration (CFU/ml) 1.6 * 10
5, incubation time 18h, bacteria concentration mensuration-colony counting method.
As can be seen from the above table, constant in process, only convert under the prerequisite of antiseptic, the chitosan quaternary ammonium salt that the present invention selects has better antibacterial effect than hydroxyethyl chitosan, under the identical prerequisite of antiseptic, use direct blending of the present invention and use first by chitosan derivatives after alkalization, yellow again with viscose solution blend, anti-microbial property the indifference of the anti-bacterial fibre cellulose fiber that it is prepared.
Claims (10)
1. an antibacterial regenerated celulose fibre, it is characterized in that the chitosan quaternary ammonium salt that contains 0.5～10wt% in described antibacterial regenerated celulose fibre, substitution value >=80% of described chitosan quaternary ammonium salt, bacteriostatic activity value >=2.5 of described antibacterial regenerated celulose fibre, bactericidal activity value >=1.0.
2. antibacterial regenerated celulose fibre as claimed in claim 1, is characterized in that: described chitosan quaternary ammonium salt is hydroxypropyl alkyl ammomium chloride shitosan.
3. antibacterial regenerated celulose fibre as claimed in claim 2, is characterized in that: described chitosan quaternary ammonium salt comprises at least one in HACC, hydroxypropyl alkyl-dimethyl ammonium chloride shitosan.
4. antibacterial regenerated celulose fibre as claimed in claim 3, is characterized in that: described chitosan quaternary ammonium salt is HACC.
5. a preparation method for antibacterial regenerated celulose fibre, is characterized in that comprising the following steps:
(1) deionized water, NaOH for chitosan quaternary ammonium salt are made into antiseptic solution, in described antiseptic solution, the mass concentration of NaOH is 5～15%;
(2) adopting cellulose pulp is raw material, through comprising that dipping, squeezing, pulverizing, experienced, yellow step make cellulose sulfonate, and then make spinning viscose through dissolving, deaeration and filtration step;
(3) antiseptic solution step (1) being prepared adds yellow step in step (2) to the viscose solution in arbitrary step before spinning, the addition of described chitosan quaternary ammonium salt be in viscose solution chemical cellulose weight 0.5～10%, obtain antibacterial spinning viscose solution;
(4) by described antibacterial spinning viscose solution through coagulating bath spinning, draw forming, then through refining, dry and to obtain described antibacterial regenerated celulose fibre.
6. the preparation method of antibacterial regenerated celulose fibre as claimed in claim 5, it is characterized in that: in step (3), add and in the viscose solution before described antiseptic solution, contain chemical cellulose 8.5～10wt%, NaOH 4～5wt%, the viscosity of viscose solution is 30～60s, add in the antibacterial spinning viscose solution after described antiseptic solution and contain chemical cellulose 7～9.5wt%, NaOH 4.5～7wt%, the viscosity of antibacterial spinning viscose solution is 30～55s.
7. the preparation method of antibacterial regenerated celulose fibre as claimed in claim 5, it is characterized in that: the temperature of described coagulating bath is 40～60 ℃ sulfur acid 90～130g/l, zinc sulfate and/or aluminum sulfate 5～15g/l, sodium sulphate 270～350g/l in described coagulating bath.
8. the preparation method of antibacterial regenerated celulose fibre as claimed in claim 5, is characterized in that: the total stretch ratio of described drawing-off is 30～200%.
9. the preparation method of the antibacterial regenerated celulose fibre as described in claim as arbitrary in claim 5 to 8, is characterized in that: described chitosan quaternary ammonium salt is hydroxypropyl alkyl ammomium chloride shitosan, substitution value >=80% of described chitosan quaternary ammonium salt.
10. the preparation method of antibacterial regenerated celulose fibre as claimed in claim 9, is characterized in that: described chitosan quaternary ammonium salt comprises at least one in HACC, hydroxypropyl alkyl-dimethyl ammonium chloride shitosan.
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| CN108866665B (en) * | 2018-07-19 | 2020-11-24 | 恒天纤维集团有限公司 | Antibacterial cellulose composite fiber and preparation method thereof |
| CN110172741A (en) * | 2019-02-26 | 2019-08-27 | 东华大学 | A kind of preparation method of functional fiber element fiber |
| CN109943977A (en) * | 2019-03-26 | 2019-06-28 | 泰州億达彩印包装有限公司 | A kind of nanofiber antimicrobial preservative film |
| CN111450304A (en) * | 2020-03-17 | 2020-07-28 | 青岛博益特生物材料股份有限公司 | Positively charged biological fiber hemostatic and bacteriostatic material and preparation method and application thereof |
| CN113151925A (en) * | 2021-04-07 | 2021-07-23 | 罗莱生活科技股份有限公司 | Polyquaternary ammonium salt/aloe antibacterial fiber, preparation method thereof and application thereof in antibacterial towels |
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