CN1277977C - Crosslinked pupa chitosan viscose antibacterial azelon preparing method - Google Patents
Crosslinked pupa chitosan viscose antibacterial azelon preparing method Download PDFInfo
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- CN1277977C CN1277977C CN 200410081574 CN200410081574A CN1277977C CN 1277977 C CN1277977 C CN 1277977C CN 200410081574 CN200410081574 CN 200410081574 CN 200410081574 A CN200410081574 A CN 200410081574A CN 1277977 C CN1277977 C CN 1277977C
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Abstract
The present invention relates to a manufacturing method of crosslinking pupa chitosan viscose protein antibacterial fibers, particularly to a manufacturing method of base materials of antibacterial fabrics. In the manufacturing method, silkworm pupa chitosan and pupa viscose protein filaments are used as raw materials, and the silkworm pupa chitosan is decolorized and then dissolved in acidic medium; the decolorized silkworm pupa chitosan solution is mixed with the silkworm pupa viscose protein filaments, and is penetrated and adsorbed on the silkworm pupa viscose protein filaments by vacuum suction filtration; then, crosslinking agents are used for solid-liquid crosslinking for fixing the silkworm pupa chitosan and stabilizing the silkworm pupa isolated proteins in the viscose protein filaments, and thus, the crosslinking pupa chitosan viscose protein antibacterial fibers are prepared. The fibers prepared by the present invention can not only have the favorable property of the silkworm pupa viscose protein filaments, but also have the function of gram-positive bacteria, can reduce more than 93% of the dissolution rate of the silkworm pupa isolated proteins in the fibers, and can be widely used as the base materials of the antibacterial fabrics, so the present invention is a good method for manufacturing the crosslinking pupa chitosan viscose protein antibacterial fibers.
Description
One. technical field
The present invention relates to the material manufacturing method of textile industry, particularly the antibiotic fabric production method for base material.
Two. background technology
Antibiotic fabric is to have antibiotic, as to control functions such as mould, deodorization fabric.Antibiotic fabric can prevent that not only fabric from being stained by microorganism and variable color, mouldy, degraded embrittlement equivalent damage take place, and has the new function of health care.The antibiotic health care textiles will be the senior textiles of modern people's demand, so antibiotic fabric has tempting prospect and vast market.Antibiotic fabric can be widely used in makes underwear, coat, socks, shoes interlining, baby diaper, the bedding of hospital, hotel, family, the fabric articles for use that towel, bath towel, ornament, carpet, health department are used, the fighting uniform of military service etc., have great economic benefit and social benefit, antibiotic fabric is again the very strong fabric of practicality.The base material of antibiotic fabric is an anti-bacterial fibre.Shitosan has characteristics such as excellent broad spectrum antibacterial, excellent biological compatibility, nontoxic, nonirritant, no antigen, is the base material of anti-bacterial fibre.
Chinese patent ZL971078009.9 disclosed " a kind of method for manufacturing pupa protein viscose filament rayon " is to be raw material with pupa albumen, make the pupa protein solution earlier, the back with the blend of cellulose sulfonic acid solutions, reel off raw silk from cocoons and hydroformylation, obtain the pupa toranomer-protein silk, this pupa toranomer-protein silk has the flexibility as the silk, characteristics such as good hygroscopicity, drapability, wrinkle resistance and dyeability.Its fabric sheen is soft, and feel is smooth, moisture absorption, good permeability, but this pupa viscose does not have antibiotic property, is golden yellow, color is darker, protein instability, weak point such as go mouldy easily, particularly the silkworm separated protein of blend in viscose glue is water-soluble higher under alkali condition, therefore in the fabric that is made into this pupa viscose, concise under alkali condition, the process that dyes, its albumen easily runs off, form " color spot silk ", form " piebald lining " with its cloth that is made into; Silkworm separated protein is one of main nutriment of growth of microorganism needs, in wet environment, easily is that microorganism utilizes " going mouldy ", has a strong impact on the application prospect of pupa albumen silk.
Three. summary of the invention
The objective of the invention is weak point at the pupa toranomer-protein silk, a kind of crosslinked pupa chitosan viscose antibacterial azelon preparation method is provided, its fiber that produces has not only kept the good characteristic of pupa toranomer-protein silk, the function that also has resisting gram-positive bacteria, and can reduce the characteristics such as dissolution rate of silkworm separated protein in the pupa toranomer-protein silk.
The object of the present invention is achieved like this: a kind of crosslinked pupa chitosan viscose antibacterial azelon preparation method, with silkworm chitosan and silkworm chrysalis toranomer-protein silk is raw material, elder generation decolours to silkworm chitosan after the processing, be dissolved in the acid medium, again with the silkworm chitosan solution and the blend of silkworm chrysalis toranomer-protein silk of decolouring, pass through vacuum filtration, the silkworm chitosan infiltration is adsorbed on the silkworm chrysalis toranomer-protein silk, then with crosslinking agent under vacuum condition, consolidate-liquid is crosslinked with fixing silkworm chitosan and stablize the protein of silkworm chrysalis toranomer-protein silk, makes pupa chitosan viscose antibacterial azelon.
The manufacture method step of crosslinked pupa chitosan viscose antibacterial azelon is as follows:
1. to the silkworm chitosan processing of decolouring
In the silkworm chitosan raw material, adding soft water and concentration is the peracetic acid soln of 3%-5%, and stir, under 65-75 ℃ of temperature, decolour and handled 30-40 minute, the pH value of using NaOH (NaOH) solution to regulate the decolouring treatment fluid then is 7.0-7.5, again through centrifugation and post precipitation, and the collecting precipitation thing, with soft water to the sediment cyclic washing collected till the free from extraneous odour, last under 80 ℃ of-90 ℃ of temperature the oven dry back obtain the decolouring silkworm chitosan of white, free from extraneous odour;
2. dissolve the decolouring silkworm chitosan
It is that 2%-5%, pH value are in the acid solution (as acetate, hydrochloric acid, sulfuric acid etc.) of 2.0-4.0 that the decolouring silkworm chitosan is positioned over concentration, and obtaining concentration after the stirring and dissolving is the silkworm chitosan solution of 0.5%-2.0%;
3. the silkworm chrysalis toranomer-protein silk is carried out vacuum infiltration absorption silkworm chitosan
Silkworm chrysalis toranomer-protein silk raw material is placed vacuumfilter, add decolouring silkworm chitosan solution, make its submergence silkworm chrysalis toranomer-protein silk, it is-0.05～0.08MPa that the unlatching vacuumfilter carries out suction filtration to vacuum, and kept vacuum 15～30 minutes, make the silkworm chrysalis toranomer-protein silk fully permeate the adsorption bleaching silkworm chitosan, bleed off silkworm chitosan solution then, use the vavuum pump suction filtration again, remove excess liquid, reclaim bleeding off, can reuse behind the supplementary decoloration silkworm chitosan, to make full use of the silkworm chitosan raw material with the silkworm chitosan solution of suction filtration;
With crosslinking agent under vacuum condition, consolidate-liquid is crosslinked
Unnecessary liquid will be removed, infiltration is adsorbed with the silkworm chrysalis toranomer-protein silk of decolouring silkworm chitosan, be positioned in the vacuumfilter, adding temperature is 30 ℃-40 ℃, the pH value is 5.0-5.5, concentration is that the crosslinking agent of 10%-20% is (as glyoxal, malonaldehyde, glutaraldehyde etc.) after the submergence, the unlatching vacuumfilter carries out suction filtration to vacuum, and keep temperature and vacuum 30-50 minute, the silkworm separated protein of decolouring silkworm chitosan and silkworm chrysalis toranomer-protein silk is consolidated with crosslinking agent respectively-the liquid cross-linking reaction, fixing silkworm chitosan, and the silkworm separated protein of stable silkworm chrysalis toranomer-protein silk, obtain white crosslinked pupa chitosan viscose antibacterial azelon;
Suction filtration, the washing crosslinked silkworm chitosan viscose glue albumen anti-bacterial fibre
Carry out suction filtration with finishing silkworm chitosan viscose glue albumen anti-bacterial fibre crosslinked, white with vavuum pump, after removing excess liquid, use the soft water filtering and washing again, remove its free crosslinking agent, then the crosslinked silkworm chitosan viscose glue albumen anti-bacterial fibre of the white after the filtering and washing is dried under 60 ℃ of-65 ℃ of temperature, become white crosslinked silkworm chitosan viscose glue albumen anti-bacterial fibre finished product; To remove and filtering and washing after cross-linking agent solution reclaim and adjust concentration and pH value after, can reuse, to make full use of crosslinking agent;
After the present invention adopts technique scheme, the crosslinked silkworm chitosan viscose glue albumen anti-bacterial fibre that produces has not only kept the silkworm chrysalis toranomer-protein silk to have good characteristics such as good flexibility, hygroscopicity, drapability, wrinkle resistance, dyeability, but also has the function of resisting gram-positive bacteria because of infiltration absorption, crosslinked decolouring silkworm chitosan, become white anti-bacterial fibre, enlarged range of application; Again because of consolidate with crosslinking agent-liquid is crosslinked, not only infiltration absorption silkworm chitosan becomes anti-bacterial fibre on the silkworm chrysalis toranomer-protein silk, but also stablized silkworm separated protein in the silkworm chrysalis toranomer-protein silk, thereby the dissolution rate that has reduced silkworm separated protein in the silkworm chrysalis toranomer-protein silk surpasses 93%.Therefore, finished product of the present invention can be widely used as the base material of antibiotic fabric, is the good method of making white anti-bacterial fibre.
Four. description of drawings
Fig. 1 is a process chart of the present invention.
Five. the specific embodiment
Below in conjunction with the specific embodiment, further specify the present invention.
A kind of manufacture method step of pupa chitosan viscose antibacterial azelon is as follows:
1. to the silkworm chitosan processing of decolouring
In 100g silkworm chitosan raw material, 10% peracetic acid soln that adds 10 times of weight, stir, processing decolouring under 65 ℃ of temperature after 30 minutes, the pH value that NaOH with 10% (NaOH) solution is regulated treatment fluid is 7.0, through centrifugation precipitation, collecting precipitation, and with soft water to the precipitation cyclic washing collected till the free from extraneous odour, last under 80 ℃ of temperature the oven dry back obtain the silkworm chitosan 85g of white, free from extraneous odour;
2. dissolve the decolouring silkworm chitosan
Take by weighing decolouring silkworm chitosan 50g, adding the pH value is 2% acetic acid solution of 4.0,10 times of weight, and under agitation dissolving back acquisition concentration is 1% decolouring silkworm chitosan solution;
3. the silkworm chrysalis toranomer-protein silk is carried out vacuum infiltration absorption silkworm chitosan
Get 500g silkworm chrysalis toranomer-protein silk raw material, place vacuumfilter, adding concentration is 1% decolouring silkworm chitosan solution, make the silkworm chrysalis toranomer-protein silk of its submergence 500g, the unlatching vacuumfilter carries out suction filtration to vacuum, and kept vacuum 15 minutes, make the silkworm chrysalis toranomer-protein silk fully permeate the adsorption bleaching silkworm chitosan, bleeding off silkworm chitosan solution then goes out and uses the vavuum pump suction filtration, remove excess liquid, to reusing behind the silkworm chitosan solution recovery supplementary decoloration silkworm chitosan that bleeds off;
With crosslinking agent under vacuum condition, consolidate-liquid is crosslinked
Unnecessary liquid will be removed, the silkworm chrysalis toranomer-protein silk that infiltration is adsorbed with the decolouring silkworm chitosan places vacuumfilter, adding temperature is 30 ℃, the pH value is 5.0, concentration is 10% glyoxal crosslinking agent submergence, the unlatching vacuumfilter carries out suction filtration to vacuum, and kept temperature and vacuum 30 minutes, make silkworm separated protein in decolouring silkworm chitosan and the silkworm chrysalis toranomer-protein silk consolidate with the glyoxal crosslinking agent respectively-liquid is crosslinked, fixing silkworm chitosan, and the silkworm chrysalis protein of stable silkworm chrysalis toranomer-protein silk, obtain white crosslinked silkworm chitosan viscose glue albumen anti-bacterial fibre;
Suction filtration, the washing crosslinked silkworm chitosan viscose glue albumen anti-bacterial fibre
Bleed off unnecessary, concentration and be 10% glyoxal crosslinking agent, the silkworm chitosan viscose glue albumen anti-bacterial fibre of finishing crosslinked white is carried out suction filtration with vavuum pump, after removing excess liquid, use the soft water filtering and washing of 5000ml again, remove its free glyoxal crosslinking agent, then the crosslinked silkworm chitosan viscose glue albumen anti-bacterial fibre of the white after the filtering and washing is dried under 60 ℃ of temperature, become white crosslinked silkworm chitosan viscose glue albumen anti-bacterial fibre finished product, the glyoxal cross-linking agent solution that bleeds off is reclaimed and adjust reuse once more after concentration and the pH value.
Claims (3)
1. crosslinked pupa chitosan viscose antibacterial azelon preparation method is characterized in that the method step of making is as follows:
(1) to the silkworm chitosan processing of decolouring
In the silkworm chitosan raw material, adding soft water and concentration is the peracetic acid soln of 3%-5%, and stir, under 65-75 ℃ of temperature, decolour and handled 30-40 minute, pH value with sodium hydroxide solution adjusting decolouring treatment fluid is 7.0-7.5 then, again through centrifugation and post precipitation, and the collecting precipitation thing, with soft water to the sediment cyclic washing collected till the free from extraneous odour, under 80 ℃ of-90 ℃ of temperature, dry at last;
(2) dissolving decolouring silkworm chitosan
It is that 2%-5%, pH value are in the acid solution of 2.0-4.0 that the decolouring silkworm chitosan is positioned over concentration, and obtaining concentration after the stirring and dissolving is the silkworm chitosan solution of 0.5%-2.0%;
(3) the silkworm chrysalis toranomer-protein silk is carried out vacuum infiltration absorption silkworm chitosan
Silkworm chrysalis toranomer-protein silk raw material is placed vacuumfilter, add decolouring silkworm chitosan solution, make its submergence silkworm chrysalis toranomer-protein silk, the unlatching vacuumfilter carries out suction filtration to vacuum, and keeps vacuum 15-30 minute, bleeds off silkworm chitosan solution then, use the vavuum pump suction filtration again, remove excess liquid, reclaim, can reuse behind the supplementary decoloration silkworm chitosan bleeding off with the silkworm chitosan solution of suction filtration;
(4) with crosslinking agent under vacuum condition, consolidate-liquid is crosslinked
With remove unnecessary liquid, the infiltration be adsorbed with the decolouring silkworm chitosan the silkworm chrysalis toranomer-protein silk, be positioned in the vacuumfilter, adding temperature and be 30 ℃-40 ℃, pH value is after 5.0-5.5, concentration are the crosslinking agent submergence of 10%-20%, open vacuumfilter and carry out suction filtration to vacuum and be-0.05--0.08MPa, and keep temperature and vacuum 30-50 minute;
(5) suction filtration, the crosslinked silkworm chitosan viscose glue albumen anti-bacterial fibre of washing
Carry out suction filtration with finishing silkworm chitosan viscose glue albumen anti-bacterial fibre crosslinked, white with vavuum pump, after removing excess liquid, use the soft water filtering and washing again, then the crosslinked silkworm chitosan viscose glue albumen anti-bacterial fibre of the white after the filtering and washing is dried under 60 ℃ of-65 ℃ of temperature, to remove and filtering and washing after described cross-linking agent solution reclaim and adjust concentration and pH value after, can reuse.
2. according to the described crosslinked pupa chitosan viscose antibacterial azelon preparation method of claim 1, it is characterized in that the acid solution described in (2) step is acetic acid solution or hydrochloric acid solution or sulfuric acid solution; At the crosslinking agent described in (4) step is glyoxal or malonaldehyde or glutaraldehyde.
3. crosslinked pupa chitosan viscose antibacterial azelon preparation method is characterized in that its method step is as follows:
(1) to the silkworm chitosan processing of decolouring
In 100g silkworm chitosan raw material, 10% peracetic acid soln that adds 10 times of weight, stir, processing decolouring under 65 ℃ of temperature after 30 minutes, the pH value that sodium hydroxide solution with 10% is regulated treatment fluid is 7.0, through centrifugation precipitation, collecting precipitation, and with soft water to the precipitation cyclic washing collected till the free from extraneous odour, last under 80 ℃ of temperature the oven dry back obtain the silkworm chitosan 85g of white, free from extraneous odour;
(2) dissolving decolouring silkworm chitosan
Take by weighing decolouring silkworm chitosan 50g, adding the pH value is 2% acetic acid solution of 4.0,10 times of weight, and under agitation dissolving back acquisition concentration is 1% decolouring silkworm chitosan solution;
(3) the silkworm chrysalis toranomer-protein silk is carried out vacuum infiltration absorption silkworm chitosan
Get 500g silkworm chrysalis toranomer-protein silk raw material, place vacuumfilter, adding concentration is 1% decolouring silkworm chitosan solution, make the silkworm chrysalis toranomer-protein silk of its submergence 500g, open vacuumfilter and carry out suction filtration to vacuum and be-0.05MPa, and kept vacuum 15 minutes, bleed off silkworm chitosan solution then and go out and use the vavuum pump suction filtration, remove excess liquid, to reusing behind the silkworm chitosan solution recovery supplementary decoloration silkworm chitosan that bleeds off;
(4) with crosslinking agent under vacuum condition, consolidate-liquid is crosslinked
With remove unnecessary liquid, the infiltration be adsorbed with the decolouring silkworm chitosan the silkworm chrysalis toranomer-protein silk place vacuumfilter, add temperature and be 30 ℃, pH value and be 5.0, concentration is 10% glyoxal crosslinking agent submergence, open vacuumfilter and carry out suction filtration to vacuum and be-0.05MPa, and kept temperature and vacuum 30 minutes;
(5) suction filtration, the crosslinked silkworm chitosan viscose glue albumen anti-bacterial fibre of washing
Bleed off unnecessary, concentration and be 10% glyoxal crosslinking agent, the silkworm chitosan viscose glue albumen anti-bacterial fibre of finishing crosslinked white is carried out suction filtration with vavuum pump, after removing excess liquid, use the soft water filtering and washing of 5000ml again, remove its free glyoxal crosslinking agent, then the crosslinked silkworm chitosan viscose glue albumen anti-bacterial fibre of the white after the filtering and washing is dried under 60 ℃ of temperature, the glyoxal cross-linking agent solution that bleeds off is reclaimed and adjust reuse once more after concentration and the pH value.
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| CN106638028B (en) * | 2016-11-28 | 2018-11-27 | 苏州大学 | A kind of raising viscose glue and the active method of chitin blending fiber biological |
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