CN102127841A - Production method of cellulose non-woven fabric with functions of mildew proofing, antibiosis and deodorization through wet-type meltbrown - Google Patents
Production method of cellulose non-woven fabric with functions of mildew proofing, antibiosis and deodorization through wet-type meltbrown Download PDFInfo
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Abstract
The invention provides a production method of a cellulose non-woven fabric with functions of mildew proofing, antibiosis and deodorization through wet-type meltbrown, comprising the following steps of: adding natural chitosan macromolecules subjected to functionalized modification and nanocrystallization into a size prepared from pulp and N-methylmorpholine N-oxide (short for NMMO) to be mixed and dissolved to form a dope; then spraying the dope from a spinning nozzle in a meltbrown way to form a non-woven fabric silk net, and carrying out water mist solidification and regeneration; and finally, washing with water, rolling with a squirt cut, drying, rolling and carrying out other procedures to obtain a natural cellulose non-woven fabric with functions of mildew proofing, antibiosis and deodorization and a continuous filament form. The cellulose non-woven fabric with functions of mildew proofing, antibiosis and deodorization can be applied to wiping textiles, medical consumables, filtering materials, biotechnical materials, photoelectric wafers and the like with functions of mildew proofing, antibiosis and deodorization.
Description
[technical field]
The invention relates to a kind of melt and spray with wet type have mildew-resistant, the method for making of antibiotic and deodorization functions cellulose Nonwovens, especially refer to a kind of environmental protection processing procedure that has low manufacturing cost and can not cause environmental pollution, the Nonwovens finished product that it makes belongs to the long fiber kenel, and have mildew-resistant, antibiotic and deodorization functions, and then can be applied on the purposes such as textiles, medical and health, filtering material, biotechnology material and the wiping of photoelectricity wafer.
[background technology]
The present made Nonwovens of artificial synthetic fiber, it is high molecular polymerization raw material by fusion, with direct extrusion molding (spunlaid) through extruding extend to form continuous long fiber after, again it is stacked into net form and forms the Nonwovens finished product, can give Nonwovens because of long fiber and have rerum naturas such as air permeability and good and water absorption rate, so be widely used in large quantities such as on the fields such as amenities, wiping material, medical protection and filter material; And according to the statistics of U.S. Nonwovens TIA (INDA), the city of this artificial synthetic fiber's Nonwovens accounts for rate and has grown to 43.7% (first) in 2009 from 33.5% (second) in 1994, whole output also reaches annual 2.7 hundred ten thousand tons, and employed maximum raw material in its production, be polypropylene (PP) in regular turn, polyester (PET), polyethylene (PE) and nylon (Nylon), account for 96% of total use amount altogether, so when these a large amount of artificial synthetic fiber's Nonwovenss become discarded object after using, owing to can't be decomposed by natural environment, on the contrary environment be produced huge bad impact results.
Chitin, spherical chitosan are the straight chain shape high molecular polymers that is formed with β-1,4 bond by monomer N-acetyl grape amine candy and grape amine candy in addition; Chitin class material distributes very wide at occurring in nature, also contain suitable rich chitin in the shrimp and crab shells, and with regard to the viewpoint of food processing waste utilization, chitin and spherical chitosan quite are worth being developed.In addition, the output and the output value of the processing of shrimp crab, be Taiwan aquatic products processing product main projects for a long time, valuable compositions such as rich in proteins, astacin, chitin as not handled, very easily cause the burden of ecological environment in its discarded object, if can be with it utilization to make the product of high value, can not only solve the problem of discarded object, can increase economic value again, be to serve multiple.
Moreover; the crust of shrimp crab class can obtain 20～30% chitin class material approximately behind suitable purifying; if wish to get the spherical chitosan of multiple different degree of acetylation; only need the go acetyl processing of chitin through the high temperature thermokalite just can be obtained; and chitin/spherical chitosan has Biodegradable and bio-compatibility; except that environment is not had the injury, have more effects such as excellent mildew-resistant, antibiotic and deodorization functions.
Therefore, make as how natural fabric raw material and low-cost processing procedure have excellent mildew-resistant, the Nonwovens product of the long fiber kenel of antibiotic and deodorization functions, just become important business anxious to be broken through.
[summary of the invention]
Main purpose of the present invention is to provide a kind of melting and spraying with wet type to have mildew-resistant, the method for making of antibiotic and deodorization functions cellulose Nonwovens, be to add through the natural spherical chitosan macromolecule (chitosan) of functionalized modification and nanometer with wood pulp (pulp) and oxidation methyl agate beautiful jade (N-methylmorpholine N-oxide, abbreviation NMMO) in the slurries that are deployed into, make its phase mixed dissolution become mucus (dope), in the mode of melting and spraying (meltbrown) this mucus is formed the Nonwovens silk screen from spinning a mouthful ejection again, solidify regeneration through water smoke, after washing, liquid drugs injection rolls, dry and batch supervisor after, can make continuous long fiber silk kenel and have mildew-resistant, the native cellulose Nonwovens of antibiotic and deodorization functions; Because this processing procedure weak point makes manufacturing cost reduce, and because of using avirulent oxidation methyl agate beautiful jade also can fully recycle as solvent, and becoming not the environmental protection processing procedure that can pollute environment, this native cellulose Nonwovens of making still can be possessed original mildew-resistant, antibiotic and deodorization functions through washing 10 times simultaneously.
Another object of the present invention is to provide a kind of melting and spraying to have mildew-resistant with wet type, the method for making of antibiotic and deodorization functions cellulose Nonwovens, has a mildew-resistant according to this method is obtained, the native cellulose Nonwovens of antibiotic and deodorization functions, can be applicable to textiles, the health care material, filter material, on the purposes such as biotechnology material and the wiping of photoelectricity wafer, and can reduce human body, farming fishery livestock or article are by the probability of infected by microbes, and the generation that reduces the generation stink, and because of belonging to the continuous fiber kenel, except that having rerum naturas such as good gas permeability identical and water absorption rate with artificial synthetic fiber's Nonwovens, when becoming discarded object after it uses, can be in environment natural decomposition, and can not damage environment.
Technical scheme of the present invention is: a kind of melt and spray with wet type have mildew-resistant, the method for making of antibiotic and deodorization functions cellulose Nonwovens, it is characterized in that: step comprises:
A. be raw material with wood pulp (pulp); Select the wood pulp cellulose of alpha-cellulose content at the long and short fiber more than 85% for use, its cellulosic degree of polymerization (degree of polymerization is called for short DP) is between 500～1200;
B. add oxidation methyl agate beautiful jade solvent (N-methylmorpholine N-oxide is called for short NMMO) in wood pulp, and dissolving is deployed into the slurries of wood pulp and oxidation methyl agate beautiful jade;
C. will add in the slurries that above-mentioned wood pulp and oxidation methyl agate beautiful jade be deployed into through the natural spherical chitosan macromolecule (chitosan) of functionalized modification and nanometer, and make it mix formation mucus (dope) mutually; It is to utilize horizontal paste mixer, with this wood pulp cellulose, oxidation methyl agate beautiful jade solvent and through functionalized modification after the natural spherical chitosan of nanometer is inserted, carrying out high speed with 60 ℃～80 ℃ low temperature blends, utilize the vacuum film evaporimeter with 80 ℃～120 ℃ heating again, the mixed moisture content of evaporation dissolving is got rid of to 5～13% in 5 minutes, can form mucus (dope)
D. in the mode of melting and spraying (meltbrown) mucus is formed cellulose tow from spinning a mouthful ejection; And
E. spray water smoke and make cellulose tow solidify regeneration, more in regular turn through washing, liquid drugs injection rolls, dry and batch supervisor, promptly make continuous long fiber silk kenel and have the native cellulose Nonwovens of mildew-resistant, antibiotic and deodorization functions.
Wherein, natural spherical chitosan is to be raw material with discarded shrimp and crab shells among this step c, makes its separation and purification after peracid, alkali treatment, and the degree of deacetylation of its obtained spherical chitosan (degree of deacetylation) is between 50%～99%.
Wherein, the concentration of oxidation methyl agate beautiful jade solvent is 50%～75% among this step b.
Wherein, this native cellulose Nonwovens is to be continuous filament among the step e, and the fibre number of this native cellulose fibre Nonwovens is 1～15um, and the basic weight of this native cellulose Nonwovens is 10g/m2～300g/m2.
Wherein, the molecular weight of this spherical chitosan is 10,000～520,000 among the step c.
Wherein, the content that this spherical chitosan accounts for cellulose fibre among the step c is 0.1wt%～7.0wt%.
Wherein, the content of cellulose of this mucus is 6wt%～15wt% among the step c, and this mucus viscosity is 300～3000 (poise), and this mucus printing opacity index is 1.470～1.495, and this mucus melt index is 400～1000.
Wherein, the coiling speed of this continuous long fiber silk kenel native cellulose Nonwovens is 2～200 meters of per minutes among the step e.
Wherein, this acid, the used acid of alkali treatment are hydrochloric acid (HCl) or sulfuric acid (H2SO4).
Wherein, this acid, the used alkali of alkali treatment are to be NaOH (NaOH) or potassium hydroxide (KOH).
The present invention is a kind of melt and spray with wet type have mildew-resistant, the method for making of antibiotic and deodorization functions cellulose Nonwovens, its advantage and effect are: because this processing procedure weak point makes manufacturing cost reduce, and because of using avirulent oxidation methyl agate beautiful jade also can fully recycle as solvent, and becoming not the environmental protection processing procedure that can pollute environment, this native cellulose Nonwovens of making still can be possessed original mildew-resistant, antibiotic and deodorization functions through washing 10 times simultaneously.Has a mildew-resistant according to this method is obtained, the native cellulose Nonwovens of antibiotic and deodorization functions, can be applicable to textiles, the health care material, filter material, on the purposes such as biotechnology material and the wiping of photoelectricity wafer, and can reduce human body, farming fishery livestock or article are by the probability of infected by microbes, and the generation that reduces the generation stink, and because of belonging to the continuous fiber kenel, except that having rerum naturas such as good gas permeability identical and water absorption rate with artificial synthetic fiber's Nonwovens, when becoming discarded object after it uses, can be in environment natural decomposition, and can not damage environment.
[description of drawings]
Fig. 1 is a manufacturing process calcspar of the present invention.
Fig. 2 is the oxidation methyl agate beautiful jade solvent used herein chemical structural drawing of (N-methylmorpholine N-oxide is called for short NMMO).
Fig. 3 is spherical chitosan (chitosan) chemical structural drawing that the present invention uses.
Fig. 4 melts and sprays the Nonwovens illustrative view among the present invention.
Fig. 5 is a manufacturing process schematic diagram of the present invention.
Concrete label is as follows among the figure:
1-gear pump 2-mould
3-spins mouth pipe D-mucus
The H-hot-air
[specific embodiment]
Below in conjunction with drawings and Examples, technical scheme of the present invention is described further.
See also Fig. 1 to shown in Figure 5, the present invention melt and spray with wet type have mildew-resistant, the method for making of antibiotic and deodorization functions cellulose Nonwovens, its step comprises:
A. be raw material with wood pulp (pulp); Select the wood pulp cellulose of alpha-cellulose content at the long and short fiber more than 85% for use, its cellulosic degree of polymerization (degree of polymerization is called for short DP) is between 500～1200;
B. add oxidation methyl agate beautiful jade solvent (N-methylmorpholine N-oxide is called for short NMMO, and its chemical constitution as shown in Figure 2) in wood pulp, and dissolving is deployed into the slurries of wood pulp and oxidation methyl agate beautiful jade;
C. will add in the slurries that above-mentioned wood pulp and oxidation methyl agate beautiful jade be deployed into through the natural spherical chitosan macromolecule (chitosan, its chemical constitution as shown in Figure 3) of functionalized modification and nanometer, and make it mix formation mucus (dope) mutually; It is to utilize horizontal paste mixer, with this wood pulp cellulose, oxidation methyl agate beautiful jade solvent and through functionalized modification after the natural spherical chitosan of nanometer is inserted, carrying out high speed with 60 ℃～80 ℃ low temperature blends, utilize the vacuum film evaporimeter with 80 ℃～120 ℃ heating again, the mixed moisture content of evaporation dissolving is got rid of to 5～13% in 5 minutes, can form mucus (dope)
D. in the mode of melting and spraying (meltbrown) mucus is formed cellulose tow from spinning a mouthful ejection; As shown in Figure 4, this mucus D is squeezed into by gear pump 1 and spins in mouthful mould 2, enter again and spin the spinning in the mouth pipe 3 of mouthful mould 2, by hot-air H continue to pour into spin mouthful mould 2 after, and, force mucus D from spin mouth pipe 3, to be melted and sprayed and squeeze out the outside cellulose tow that forms from spinning the air-flow effect of discharging around the mouth pipe 3;
E. spray water smoke and make cellulose tow solidify regeneration, more in regular turn through washing, liquid drugs injection rolls, dry and batch supervisor (as shown in Figure 5), promptly make continuous long fiber silk kenel and have the native cellulose Nonwovens of mildew-resistant, antibiotic and deodorization functions.
Wherein, the concentration of the oxidation methyl agate beautiful jade solvent of step b is 50%～75% and is the avirulence solvent, after in water-washing process, being washed out, can be recovered after more after filtration, decolouring and decompression concentrate and distill and re-use, low and the rate of recovery of its proportion of goods damageds can reach more than 99.5%, not only can reduce manufacturing cost, also can not cause the pollution of environment, meet the standard of environmental protection processing procedure fully.
Wherein, natural spherical chitosan macromolecule is a raw material with discarded shrimp and crab shells mainly among the step c; earlier give separation and purification and become chitin (chitin) through peracid, alkali treatment; form spherical chitosan (chitosan) via removing N-acetyl group (N-acetyl group) after the hot alkali treatment again; at last by control NaOH concentration, heating-up temperature and time; and this spherical chitosan is imposed deacetylated (deacetylation), make its degree of deacetylation between 50%～99%.
The content of cellulose of this mucus is 6wt%～15wt% among the step c again, and the viscosity of its mucus is 300～3000 (poise), and the printing opacity index of mucus be 1.470～1.495 and the melt index of mucus be 400～1000.
The functionalized modification of this natural spherical chitosan and the mode of nanometer among other the step c, be earlier with molecular weight control system technology, during the high molecular spherical chitosan is degraded into, the low molecular weight spherical chitosan, again with the quarternary ammonium salt technology should in, the low molecular weight spherical chitosan carries out preliminary littleization upgrading, can finish its functionalized modification and nanometer with sol-gel process more at last, it possesses the good biological compatibility and biologically active promotes effect.
Wherein, its coiling speed is 2～200 meters of per minutes among the step e.
Being further proof characteristics of the present invention and enforcement effect, is to finish every test examples also to illustrate as the back:
Embodiment one (being sample number into spectrum 1～12 of the present invention):
Get the degree of polymerization and be the spherical chitosan macromolecule (chitosan) that adds degree of deacetylation 87% and 95% in 650 the wood pulp cellulose and behind functionalized modification, account for content 0.1wt%～5.0wt% in the fiber with nanometer; in the slurries of the deployed ratio of solvent oxidation methyl agate beautiful jade; utilize the unnecessary moisture content of vacuum film evaporator evaporation then; with 80 ℃～120 ℃ heating; get rid of moisture to 5%～13% in 5 minutes; cellulose dissolution can be become mucus (dope), mucus is formed table as shown in Table 1.Again this mucus is delivered to the machine of melting and spraying and is melted and sprayed with metering pump, form a Nonwovens silk screen, solidify regeneration with water smoke through spinning a mouthful ejection, again through washing, liquid drugs injection roll, dry and batch, promptly finish in the table one sample 1 to each mucus composition table of sample 12.
Each sample mucus of table one is formed table
| Sample | Cellulosic degree of polymerization | Spherical chitosan adding proportion (wt%) | De-acetyl chitin degree (%) | Content of cellulose (%) | Solvent (%) | Water content (%) | Mucus viscosity (poise) | Mucus printing opacity index | The mucus melt index |
| 1 | 650 | 0.1 | 87 | 7.6 | 813 | 11.1 | 840 | 1.489 | 870 |
| 2 | 650 | 0.5 | 87 | 7.5 | 81.9 | 10.6 | 980 | 1.482 | 820 |
| 3 | 650 | 1.0 | 87 | 8.1 | 81.2 | 10.7 | 1240 | 1.486 | 810 |
| 4 | 650 | 3.0 | 87 | 7.5 | 82.0 | 10.5 | 860 | 1.481 | 850 |
| 5 | 650 | 5.0 | 87 | 7.2 | 81.8 | 11.0 | 960 | 1.485 | 830 |
| 6 | 650 | 7.0 | 87 | 7.9 | 80.9 | 11.2 | 1160 | 1.486 | 740 |
| 7 | 650 | 0.1 | 95 | 7.5 | 81.6 | 10.9 | 980 | 1.482 | 820 |
| 8 | 650 | 0.5 | 95 | 8.1 | 81.5 | 10.4 | 1240 | 1.486 | 810 |
| 9 | 650 | 1.0 | 95 | 7.5 | 81.7 | 10.8 | 860 | 1.481 | 850 |
| 10 | 650 | 3.0 | 95 | 7.2 | 82.3 | 10.5 | 730 | 1.489 | 870 |
| 11 | 650 | 5.0 | 95 | 7.8 | 82.0 | 10.2 | 1080 | 1.488 | 820 |
| 12 | 650 | 7.0 | 95 | 8.1 | 81.8 | 10.1 | 1240 | 1.486 | 810 |
Embodiment two (being sample number into spectrum 13～24 of the present invention):
Get the degree of polymerization and be the spherical chitosan macromolecule (chitosan) that adds degree of deacetylation 87% and 95% in 1050 the wood pulp cellulose and behind functionalized modification, account for content 0.1wt%～5.0wt% in the fiber with nanometer; in the slurries of the deployed ratio of solvent oxidation methyl agate beautiful jade; utilize the unnecessary moisture content of vacuum film evaporator evaporation then; with 80 ℃～120 ℃ heating; get rid of moisture to 5%～13% in 5 minutes; cellulose dissolution can be become mucus (dope), mucus is formed table as shown in Table 2.Again this mucus is delivered to the machine of melting and spraying and is melted and sprayed with metering pump, melt and spray Nonwovens and regenerate through coagulating bath, again through washing, liquid drugs injection roll, dry and batch, promptly finish in the table two sample 13 to each mucus composition table of sample 24.
Each sample mucus of table two is formed table
| Sample | Cellulosic degree of polymerization | Spherical chitosan adds than ice-cold (wt%) | De-acetyl chitin degree (%) | Content of cellulose (%) | Solvent (%) | Water content (%) | Mucus viscosity (poise) | Mucus printing opacity index | Viscosity flow index MI |
| 13 | 1050 | 0.1 | 87 | 7.8 | 81.8 | 10.4 | 1080 | 1.488 | 720 |
| 14 | 1050 | 0.5 | 87 | 7.5 | 81.1 | 11.4 | 980 | 1.482 | 720 |
| 15 | 1050 | 1.0 | 87 | 7.1 | 82.1 | 10.8 | 830 | 1.489 | 790 |
| 16 | 1050 | 3.0 | 87 | 7.2 | 82.0 | 10.8 | 930 | 1.489 | 770 |
| 17 | 1050 | 5.0 | 87 | 7.9 | 81.0 | 11.1 | 1240 | 1.481 | 650 |
| 18 | 1050 | 7.0 | 87 | 7.2 | 82.2 | 10.6 | 1560 | 1.480 | 620 |
| 19 | 1050 | 0.1 | 95 | 1.9 | 80.2 | 11.9 | 1420 | 1.482 | 600 |
| 20 | 1050 | 0.5 | 95 | 8.0 | 81.5 | 10.5 | 1450 | 1.476 | 640 |
| 21 | 1050 | 1.0 | 95 | 8.1 | 82.1 | 10.8 | 1510 | 1.479 | 680 |
| 22 | 1050 | 3.0 | 95 | 7.9 | 80.2 | 11.9 | 1560 | 1.480 | 620 |
| 23 | 1050 | 5.0 | 95 | 7.5 | 82.0 | 10.5 | 1120 | 1.482 | 640 |
| 24 | 1050 | 7.0 | 95 | 7.2 | 82.1 | 10.7 | 1080 | 1.476 | 660 |
Embodiment three (assessment of antimildew function):
The assessment of antimildew function adopts Staphylococcus aureus subsp.Aureus 10451 for the test bacterial classification, earlier the bacterium number is cultured to 5～70E
+ 5(bacterium number/milliliter) gets the sample that test bacterium liquid 0.2ml evenly coats 0.2g, placing the sample bottle of adding a cover of sterilizing, and cultivates 18 hours down at 35 ℃.Add the BS that 20ml sterilized again, acutely shake 30 times, allow the test bacterial classification be scattered in the solution, get solution through suitable dilution, get 1ml and carry out agar broth cultivation, condition of culture be 35 ℃ following 48 hours, calculate the colony growth number then, release at last multiple and volume dimly and calculate and can extrapolate actual bacterium number on sample.More than experiment is done 6 times and is repeated, on average hold total bacteria count as calculated after, can judge the anti-mold effect of sample according to following formula:
A:, after test bacterium liquid is coated on the sample, cultivate the bacterium number of trying to achieve at once with the salt water sampling for not adding spherical chitosan in the sample.
B: for not adding spherical chitosan in the sample, test bacterium liquid is coated on the sample after the bacterium number of trying to achieve is cultivated in cultivation in 18 hours with the salt water sampling.
C: for adding spherical chitosan in the sample, test bacterium liquid is coated on the sample after the bacterium number of trying to achieve is cultivated in cultivation in 18 hours with the salt water sampling.
Judge increment at the sample more than 1.6 and have the effect of mildew-resistant according to testing standard, the assessment result of each sample as shown in Table 3.
The mould proof test result of each sample as shown in Table 3
Table three contains the antimildew function test of spherical chitosan cellulose Nonwovens
| Sample | Cellulosic degree of polymerization | Spherical chitosan adding proportion (wt%) | De-acetyl chitin degree (%) | Increment/ Decrement | Assessment result (having/do not have) |
| 1 | 650 | 0.1 | 87 | 1.25 | Do not have |
| 2 | 650 | 0.5 | 87 | 1.72 | Have |
| 3 | 650 | 1.0 | 87 | 2.28 | Have |
| 4 | 650 | 3.0 | 87 | 2.53 | Have |
| 5 | 650 | 5.0 | 87 | 2.75 | Have |
| 6 | 650 | 7.0 | 87 | 2.86 | Have |
| 7 | 650 | 0.1 | 95 | 1.48 | Do not have |
| 8 | 650 | 0.5 | 95 | 1.87 | Have |
| 9 | 650 | 1.0 | 95 | 2.33 | Have |
| 10 | 650 | 3.0 | 95 | 2.54 | Have |
| 11 | 650 | 5.0 | 95 | 2.80 | Have |
| 12 | 650 | 7.0 | 95 | 2.97 | Have |
| 13 | 1050 | 0.1 | 87 | 1.25 | Do not have |
| 14 | 1050 | 0.5 | 87 | 1.80 | Have |
| 15 | 1050 | 1.0 | 87 | 2.30 | Have |
| 16 | 1050 | 3.0 | 87 | 2.51 | Have |
| 17 | 1050 | 5.0 | 87 | 2.68 | Have |
| 18 | 1050 | 7.0 | 87 | 2.83 | Have |
| 19 | 1050 | 0.1 | 95 | 1.25 | Do not have |
| 20 | 1050 | 0.5 | 95 | 1.89 | Have |
| 21 | 1050 | 1.0 | 95 | 2.35 | Have |
| 22 | 1050 | 3.0 | 95 | 2.54 | Have |
| 23 | 1050 | 5.0 | 95 | 2.71 | Have |
| 24 | 1050 | 7.0 | 95 | 2.89 | Have |
Embodiment four (assessment of antibacterial functions):
The assessment of antibacterial functions adopts staphylococcus aureus (ATCC 6538P) and pneumobacillus (ATCC4352) to be the test bacterial classification.The derivative of spherical chitosan after by the chitin deacetylation is a kind of Nantural non-toxic, can suppresses bacterium and biological decomposable macromolecule.Because the positive electricity position on the spherical chitosan can combine with the negative electricity position on the protein, so can antimycotic and microorganism.Spherical chitosan is relevant with its molecular weight and functional group for the inhibition of bacterium and Mycophyta.Spherical chitosan can produce bond with aluminosilicate in Phospholipids, therefore limited moving of microorganism.The spherical chitosan oligomer can penetrate cells of microorganisms and suppress transcribing of RNA.The present invention's spherical chitosan is done the test of antibiotic property, test it and whether possess antibiotic property.
Table four and table five are for containing the result of the test of spherical chitosan cellulose Nonwovens antibacterial functions.This test method is a JIS L1902-1998 quantitative technique, and test strain is staphylococcus aureus (ATCC 6538P) and pneumobacillus (ATCC 4352).Wherein, plant bacteria concentration at 1.0 ± 0.3E
+ 5(bacterium number/milliliter) is interior represents experiment effectively, and Ma=is undressed, and sample washed away back bacterium number in 0 hour immediately, bacterium number after the cultivation in sample 18-24 hour that Mb=is undressed, and Mc=processing sample was cultivated back bacterium number in 18-24 hour; Bacterium growth activity value=logMb-logMa, bacterium growth activity value＞1.5 expression experiments are effective, antibacterial value=logMb-logMc, sterilizing value=logMa-logMc; According to the antibiotic standard of the new function evaluation consultation of Japanese fibre (JAFET), antibacterial value has fungistatic effect greater than 2.2 expression test sample books, and sterilizing value has bactericidal effect greater than 0 expression test sample book; 1.3E
+ 4Expression 13000, the rest may be inferred.
By table four and table five as can be known, via the present invention prepared go out contain spherical chitosan cellulose Nonwovens, itself has possessed quite good fungistatic effect and bactericidal effect for staphylococcus aureus and pneumobacillus.
The antibacterial tests result of each sample is shown in table four and table five
Table four contains the antibacterial functions test of spherical chitosan cellulose Nonwovens
| Sample | Cellulosic degree of polymerization | Spherical chitosan adding proportion (wt%) | De-acetyl chitin degree (%) | Antibacterial value | Sterilizing value | Result of the test (having/do not have) |
| 1 | 650 | 0.1 | 87 | ＞1.8 | ＞1.4 | Do not have |
| 2 | 650 | 0.5 | 87 | ＞5.0 | ＞3.2 | Have |
| 3 | 650 | 1.0 | 87 | ＞5.0 | ＞3.2 | Have |
| 4 | 650 | 3.0 | 87 | ＞5.0 | ＞3.2 | Have |
| 5 | 650 | 5.0 | 87 | ＞5.0 | ＞3.2 | Have |
| 6 | 650 | 7.0 | 87 | ＞5.0 | ＞3.2 | Have |
| 7 | 650 | 0.1 | 95 | ＞1.9 | ＞1.3 | Do not have |
| 8 | 650 | 0.5 | 95 | ＞5.0 | ＞3.2 | Have |
| 9 | 650 | 1.0 | 95 | ＞5.0 | ＞3.2 | Have |
| 10 | 650 | 3.0 | 95 | ＞5.0 | ＞3.2 | Have |
| 11 | 650 | 5.0 | 95 | ＞5.0 | ＞3.2 | Have |
| 12 | 650 | 7.0 | 95 | ＞5.0 | ＞3.2 | Have |
| 13 | 1050 | 0.1 | 87 | ＞1.8 | ＞1.4 | Do not have |
| 14 | 1050 | 0.5 | 87 | ＞5.0 | ＞3.2 | Have |
| 15 | 1050 | 1.0 | 87 | ＞5.0 | ＞3.2 | Have |
| 16 | 1050 | 3.0 | 87 | ＞5.0 | ＞3.2 | Have |
| 17 | 1050 | 5.0 | 87 | ＞5.0 | ＞3.2 | Have |
| 18 | 1050 | 7.0 | 87 | ＞5.0 | ＞3.2 | Have |
| 19 | 1050 | 0.1 | 95 | ＞1.9 | ＞1.2 | Do not have |
| 20 | 1050 | 0.5 | 95 | ＞5.0 | ＞3.2 | Have |
| 21 | 1050 | 1.0 | 95 | ＞5.0 | ＞3.2 | Have |
| 22 | 1050 | 3.0 | 95 | ＞5.0 | ＞3.2 | Have |
| 23 | 1050 | 5.0 | 95 | ＞5.0 | ＞3.2 | Have |
| 24 | 1050 | 7.0 | 95 | ＞5.0 | ＞3.2 | Have |
This test method is a JIS L1902-1998 quantitative technique, and test strain is staphylococcus aureus (ATCC6538P)
Table five contains the antibacterial functions test of spherical chitosan cellulose Nonwovens
| Sample | Cellulosic degree of polymerization | Spherical chitosan adding proportion (wt%) | De-acetyl chitin degree (%) | Antibacterial value | Sterilizing value | Result of the test (having/do not have) |
| 1 | 650 | 0.1 | 87 | ＞2.1 | ＞1.2 | Do not have |
| 2 | 650 | 0.5 | 87 | ＞6.3 | ＞3.2 | Have |
| 3 | 650 | 1.0 | 87 | ＞6.3 | ＞3.2 | Have |
| 4 | 650 | 3.0 | 87 | ＞6.3 | ＞3.2 | Have |
| 5 | 650 | 5.0 | 87 | ＞6.3 | ＞3.2 | Have |
| 6 | 650 | 7.0 | 87 | ＞6.3 | ＞3.2 | Have |
| 7 | 650 | 0.1 | 95 | ＞2.1 | ＞1.2 | Do not have |
| 8 | 650 | 0.5 | 95 | ＞6.3 | ＞3.2 | Have |
| 9 | 650 | 1.0 | 95 | ＞6.3 | ＞3.2 | Have |
| 10 | 650 | 3.0 | 95 | ＞6.3 | ＞3.2 | Have |
| 11 | 650 | 5.0 | 95 | ＞6.3 | ＞3.2 | Have |
| 12 | 650 | 7.0 | 95 | ＞6.3 | ＞3.2 | Have |
| 13 | 1050 | 0.1 | 87 | ＞2.1 | ＞1.1 | Do not have |
| 14 | 1050 | 0.5 | 87 | ＞6.3 | ＞3.2 | Have |
| 15 | 1050 | 1.0 | 87 | ＞6.3 | ＞3.2 | Have |
| 16 | 1050 | 3.0 | 87 | ＞6.3 | ＞3.2 | Have |
| 17 | 1050 | 5.0 | 87 | ＞6.3 | ＞3.2 | Have |
| 18 | 1050 | 7.0 | 87 | ＞6.3 | ＞3.2 | Have |
| 19 | 1050 | 0.1 | 95 | ＞2.1 | ＞1.2 | Do not have |
| 20 | 1050 | 0.5 | 95 | ＞6.3 | ＞3.2 | Have |
| 21 | 1050 | 1.0 | 95 | ＞6.3 | ＞3.2 | Have |
| 22 | 1050 | 3.0 | 95 | ＞6.3 | ＞3.2 | Have |
| 23 | 1050 | 5.0 | 95 | ＞6.3 | ＞3.2 | Have |
| 24 | 1050 | 7.0 | 95 | ＞6.3 | ＞3.2 | Have |
This test method is a JIS L1902-1998 quantitative technique, and test strain is pneumobacillus (ATCC 4352)
Embodiment five (assessment of deodorization functions):
The assessment of this deodorizing effect is the foundation of deodorizing to inhale the ammonia test, the following explanation of its method: with the airtight bottle certain density ammonia of packing into, the quantitative plain Nonwovens of chitin fiber that contains is put into bottle absorption 15 minutes, record the gas concentration that the cellulose Nonwovens that contains chitin is put into front and back with gas chromatograph (GC) again, this moment, deodorization was
The suction ammonia rate result of the test of each sample as shown in Table 6
Table six contains the deodorization functions test of spherical chitosan cellulose Nonwovens
| Sample | Cellulosic degree of polymerization | Spherical chitosan adding proportion (wt%) | De-acetyl chitin degree (%) | Inhale ammonia rate (%) | Result of the test (having/do not have) |
| 1 | 650 | 0.1 | 87 | 19.5 | Do not have |
| 2 | 650 | 0.5 | 87 | 66.4 | Have |
| 3 | 650 | 1.0 | 87 | 70.3 | Have |
| 4 | 650 | 3.0 | 87 | 80.5 | Have |
| 5 | 650 | 5.0 | 87 | 85.8 | Have |
| 6 | 650 | 7.0 | 87 | 86.9 | Have |
| 7 | 650 | 0.1 | 95 | 23.8 | Do not have |
| 8 | 650 | 0.5 | 95 | 67.2 | Have |
| 9 | 650 | 1.0 | 95 | 71.7 | Have |
| 10 | 650 | 3.0 | 95 | 83.1 | Have |
| 11 | 650 | 5.0 | 95 | 86.9 | Have |
| 12 | 650 | 7.0 | 95 | 88.3 | Have |
| 13 | 1050 | 0.1 | 87 | 20.7 | Do not have |
| 14 | 1050 | 0.5 | 87 | 66.6 | Have |
| 15 | 1050 | 1.0 | 87 | 70.3 | Have |
| 16 | 1050 | 3.0 | 87 | 81.0 | Have |
| 17 | 1050 | 5.0 | 87 | 84.1 | Have |
| 18 | 1050 | 7.0 | 87 | 86.2 | Have |
| 19 | 1050 | 0.1 | 95 | 23.8 | Do not have |
| 20 | 1050 | 0.5 | 95 | 65.8 | Have |
| 21 | 1050 | 1.0 | 95 | 72.5 | Have |
| 22 | 1050 | 3.0 | 95 | 83.1 | Have |
| 23 | 1050 | 5.0 | 95 | 86.9 | Have |
| 24 | 1050 | 7.0 | 95 | 88.3 | Have |
Embodiment six (mildew-resistant, antibiotic and deodorization functions assessment):
Each sample cleans 45 minutes 10 times in 70 ℃ hot water with the laundry paks of 5g/L, and each sample of gained is carried out mildew-resistant, antibacterial tests and the test of deodorizing rate, and the result of gained is shown in table seven, table eight and table nine.
Table seven contains spherical chitosan cellulose Nonwovens mildew-resistant function test after washing 10 times
| Sample | Cellulosic degree of polymerization | Spherical chitosan adding proportion (wt%) | De-acetyl chitin degree (%) | Increment/ Decrement | Assessment result (having/do not have) |
| 1 | 650 | 0.1 | 87 | 1.26 | Do not have |
| 2 | 650 | 0.5 | 87 | 1.68 | Have |
| 3 | 650 | 1.0 | 87 | 2.09 | Have |
| 4 | 650 | 3.0 | 87 | 2.31 | Have |
| 5 | 650 | 5.0 | 87 | 2.55 | Have |
| 6 | 650 | 7.0 | 87 | 2.49 | Have |
| 7 | 650 | 0.1 | 95 | 1.45 | Do not have |
| 8 | 650 | 0.5 | 95 | 1.71 | Have |
| 9 | 650 | 1.0 | 95 | 2.14 | Have |
| 10 | 650 | 3.0 | 95 | 2.32 | Have |
| 11 | 650 | 5.0 | 95 | 2.58 | Have |
| 12 | 650 | 7.0 | 95 | 2.72 | Have |
| 13 | 1050 | 0.1 | 87 | 1.26 | Do not have |
| 14 | 1050 | 0.5 | 87 | 1.66 | Have |
| 15 | 1050 | 1.0 | 87 | 2.07 | Have |
| 16 | 1050 | 3.0 | 87 | 2.11 | Have |
| 17 | 1050 | 5.0 | 87 | 2.42 | Have |
| 18 | 1050 | 7.0 | 87 | 2.58 | Have |
| 19 | 1050 | 0.1 | 95 | 1.27 | Do not have |
| 20 | 1050 | 0.5 | 95 | 1.72 | Have |
| 21 | 1050 | 1.0 | 95 | 2.16 | Have |
| 22 | 1050 | 3.0 | 95 | 2.34 | Have |
| 23 | 1050 | 5.0 | 95 | 2.48 | Have |
| 24 | 1050 | 7.0 | 95 | 2.56 | Have |
Table eight contains the antibacterial functions test after washing 10 times of spherical chitosan cellulose Nonwovens
| Sample | Cellulosic degree of polymerization | Spherical chitosan adding proportion (wt%) | De-acetyl chitin degree (%) | Antibacterial value | Sterilizing value | Result of the test (having/do not have) |
| 1 | 650 | 0.1 | 87 | ＞2.1 | ＞0.5 | Do not have |
| 2 | 650 | 0.5 | 87 | ＞3.3 | ＞1.6 | Have |
| 3 | 650 | 1.0 | 87 | ＞3.7 | ＞2.4 | Have |
| 4 | 650 | 3.0 | 87 | ＞4.3 | ＞2.3 | Have |
| 5 | 650 | 5.0 | 87 | ＞4.3 | ＞2.3 | Have |
| 6 | 650 | 7.0 | 87 | ＞4.3 | ＞2.3 | Have |
| 7 | 650 | 0.1 | 95 | ＞2.1 | ＞0.5 | Do not have |
| 8 | 650 | 0.5 | 95 | ＞3.3 | ＞1.6 | Have |
| 9 | 650 | 1.0 | 95 | ＞3.7 | ＞2.3 | Have |
| 10 | 650 | 3.0 | 95 | ＞4.3 | ＞2.3 | Have |
| 11 | 650 | 5.0 | 95 | ＞4.3 | ＞2.3 | Have |
| 12 | 650 | 7.0 | 95 | ＞4.3 | ＞2.3 | Have |
| 13 | 1050 | 0.1 | 87 | ＞2.1 | ＞0.5 | Do not have |
| 14 | 1050 | 0.5 | 87 | ＞3.3 | ＞1.6 | Have |
| 15 | 1050 | 1.0 | 87 | ＞3.7 | ＞2.4 | Have |
| 16 | 1050 | 3.0 | 87 | ＞4.3 | ＞2.3 | Have |
| 17 | 1050 | 5.0 | 87 | ＞4.3 | ＞2.3 | Have |
| 18 | 1050 | 7.0 | 87 | ＞4.3 | ＞2.3 | Have |
| 19 | 1050 | 0.1 | 95 | ＞2.1 | ＞0.5 | Do not have |
| 20 | 1050 | 0.5 | 95 | ＞3.3 | ＞1.6 | Have |
| 21 | 1050 | 1.0 | 95 | ＞3.7 | ＞2.4 | Have |
| 22 | 1050 | 3.0 | 95 | ＞4.3 | ＞2.3 | Have |
| 23 | 1050 | 5.0 | 95 | ＞4.3 | ＞2.3 | Have |
| 24 | 1050 | 7.0 | 95 | ＞4.3 | ＞2.3 | Have |
This test method is a JIS L1902-1998 quantitative technique, and test strain is pneumobacillus (ATCC 4352)
Table nine contains the deodorization functions test after washing 10 times of spherical chitosan cellulose Nonwovens
| Sample | Cellulosic degree of polymerization | Spherical chitosan adding proportion (wt%) | De-acetyl chitin degree (%) | Inhale ammonia rate (%) | Result of the test (having/do not have) |
| 1 | 650 | 0.1 | 87 | 17.7 | Do not have |
| 2 | 650 | 0.5 | 87 | 55.5 | Have |
| 3 | 650 | 1.0 | 87 | 68.8 | Have |
| 4 | 650 | 3.0 | 87 | 64.6 | Have |
| 5 | 650 | 5.0 | 87 | 76.6 | Have |
| 6 | 650 | 7.0 | 87 | 71.4 | Have |
| 7 | 650 | 0.1 | 95 | 36.5 | Do not have |
| 8 | 650 | 0.5 | 95 | 63.9 | Have |
| 9 | 650 | 1.0 | 95 | 57.7 | Have |
| 10 | 650 | 3.0 | 95 | 62.5 | Have |
| 11 | 650 | 5.0 | 95 | 69.6 | Have |
| 12 | 650 | 7.0 | 95 | 72.7 | Have |
| 13 | 1050 | 0.1 | 87 | 33.8 | Do not have |
| 14 | 1050 | 0.5 | 87 | 55.6 | Have |
| 15 | 1050 | 1.0 | 87 | 59.9 | Have |
| 16 | 1050 | 3.0 | 87 | 65.7 | Have |
| 17 | 1050 | 5.0 | 87 | 70.8 | Have |
| 18 | 1050 | 7.0 | 87 | 70.6 | Have |
| 19 | 1050 | 0.1 | 95 | 34.8 | Do not have |
| 20 | 1050 | 0.5 | 95 | 53.9 | Have |
| 21 | 1050 | 1.0 | 95 | 62.9 | Have |
| 22 | 1050 | 3.0 | 95 | 67.7 | Have |
| 23 | 1050 | 5.0 | 95 | 68.9 | Have |
| 24 | 1050 | 7.0 | 95 | 69.1 | Have |
Contain the plain Nonwovens mildew-resistant of chitin fiber and the antibacterial functions result of the test shows by table three, table four and table five, the nanometer spherical chitosan cellulose Nonwovens that contains of the present invention can reach mildew-resistant, antibiotic effect when the content of nanometer spherical chitosan reaches more than the 0.5wt%.Example by table three, table four and table five proves that the native cellulose Nonwovens that contains the nanometer spherical chitosan of the present invention can reach the effect of antimildew and antibacterial really.
Containing the plain Nonwovens deodorization functions of chitin fiber result of the test by table six shows, the nanometer spherical chitosan native cellulose Nonwovens that contains of the present invention has the good adsorption effect to ammonia, when the content of nanometer spherical chitosan reaches 0.5wt% when above, all can reach more than 50% the suction-operated of ammonia.
By table seven, table eight and table nine contain the mildew-resistant after washing 10 times of the plain Nonwovens of chitin fiber, antibiotic and deodorization functions result of the test shows, the nanometer spherical chitosan native cellulose Nonwovens that contains of the present invention is behind 10 times hot water and detergent treatment, before the mildew-resistant of Nonwovens and antibacterial functions effect were still kept and were washed originally about 90%, the result shows that the nanometer spherical chitosan native cellulose Nonwovens that contains of the present invention is one to have the mildew-resistant of long-acting type thus, the cellulose Nonwovens of antibiotic and deodorizing, its effect far surpass generally to be peddled with surface treatment on the market or adds the Nonwovens of antiseptic.
Claims (10)
- One kind melt and spray with wet type have mildew-resistant, the method for making of antibiotic and deodorization functions cellulose Nonwovens, it is characterized in that: step comprises:A. with the wood pulp raw material; Select the wood pulp cellulose of alpha-cellulose content at the long and short fiber more than 85% for use, its cellulosic degree of polymerization is between 500～1200;B. add oxidation methyl agate beautiful jade solvent in wood pulp, and dissolving is deployed into the slurries of wood pulp and oxidation methyl agate beautiful jade;C. will add through the natural spherical chitosan macromolecule of functionalized modification and nanometer in the slurries that above-mentioned wood pulp and oxidation methyl agate beautiful jade be deployed into, and make it mix the formation mucus mutually; It is to utilize horizontal paste mixer, with this wood pulp cellulose, oxidation methyl agate beautiful jade solvent and through functionalized modification after the natural spherical chitosan of nanometer is inserted, carrying out high speed with 60 ℃～80 ℃ low temperature blends, utilize the vacuum film evaporimeter with 80 ℃～120 ℃ heating again, the mixed moisture content of evaporation dissolving is got rid of to 5～13% in 5 minutes, can form mucus;D. in the mode of melting and spraying mucus is formed cellulose tow from spinning a mouthful ejection; AndE. spray water smoke and make cellulose tow solidify regeneration, more in regular turn through washing, liquid drugs injection rolls, dry and batch program, promptly make continuous long fiber silk kenel and have the native cellulose Nonwovens of mildew-resistant, antibiotic and deodorization functions.
- 2. method according to claim 1 is characterized in that: natural spherical chitosan is to be raw material with discarded shrimp and crab shells among this step c, makes its separation and purification after peracid, alkali treatment, and the degree of deacetylation of its obtained spherical chitosan is between 50%～99%.
- 3. method according to claim 1 is characterized in that: the concentration of oxidation methyl agate beautiful jade solvent is 50%～75% among this step b.
- 4. method according to claim 1 is characterized in that: this native cellulose Nonwovens is to be continuous filament among the step e, and the fibre number of this native cellulose fibre Nonwovens is 1～15um, and the basic weight of this native cellulose Nonwovens is 10g/m 2～300g/m 2
- 5. method according to claim 1 is characterized in that: the molecular weight of this spherical chitosan is 10,000～520,000 among the step c.
- 6. method according to claim 1 is characterized in that: to account for the content of cellulose fibre be 0.1wt%～7.0wt% to this spherical chitosan among the step c.
- 7. method according to claim 1 is characterized in that: the content of cellulose of this mucus is 6wt%～15wt% among the step c, and this mucus viscosity is 300～3000, and this mucus printing opacity index is 1.470～1.495, and this mucus melt index is 400～1000.
- 8. method according to claim 1 is characterized in that: the coiling speed of this continuous long fiber silk kenel native cellulose Nonwovens is 2～200 meters of per minutes among the step e.
- 9. method according to claim 2 is characterized in that: this acid, the used acid of alkali treatment are hydrochloric acid or sulfuric acid.
- 10. method according to claim 2 is characterized in that: this acid, the used alkali of alkali treatment are to be NaOH or potassium hydroxide.
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