CN105926077A - Cellulosic fiber with antibacterial anti-mold anti-mite functions and preparation method of cellulosic fiber - Google Patents

Cellulosic fiber with antibacterial anti-mold anti-mite functions and preparation method of cellulosic fiber Download PDF

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Publication number
CN105926077A
CN105926077A CN201610494383.1A CN201610494383A CN105926077A CN 105926077 A CN105926077 A CN 105926077A CN 201610494383 A CN201610494383 A CN 201610494383A CN 105926077 A CN105926077 A CN 105926077A
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China
Prior art keywords
semen cassiae
preparation
herba houttuyniae
cellulosic fiber
ramulus
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CN201610494383.1A
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Inventor
吴娇
万兴云
田平
胡流云
张晨
于湖生
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Infinitus China Co Ltd
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Infinitus China Co Ltd
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Priority to CN201610494383.1A priority Critical patent/CN105926077A/en
Publication of CN105926077A publication Critical patent/CN105926077A/en
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/02Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D1/00Treatment of filament-forming or like material
    • D01D1/06Feeding liquid to the spinning head
    • D01D1/065Addition and mixing of substances to the spinning solution or to the melt; Homogenising
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D10/00Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/06Wet spinning methods
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • D01F1/103Agents inhibiting growth of microorganisms

Abstract

The invention belongs to the technical field of functional cellulosic fiber, and in particular relates to a cellulosic fiber with antibacterial anti-mold anti-mite functions and a preparation method of the cellulosic fiber. The cellulosic fiber comprises cassia seeds, houttuynia cordata, picrasma quassioides and a cellulosic fiber body. The invention further provides the preparation method of the cellulosic fiber. The invention further provides application of the cellulosic fiber or a product prepared by using the preparation method in fields of miteprevention, mold prevention and bacterium prevention. Experimental tests show that the inhibition rate of the cellulosic fiber provided by the invention for mites can be greater than or equal to 80% when compared with that of conventional adhesive fiber, the anti-mold grade of the cellulosic fiber can be greater than the level 2 provided by the GB/T 24346-2009 Textiles Evaluation On Anti-Mold Activity, the inhibition rate of the cellulosic fiber for staphylococcus aureus is greater than or equal to 90.2%, the inhibition rate of the cellulosic fiber for escherichia coli is greater than or equal to 91.8%, and the inhibition rate of the cellulosic fiber for candida albicans is greater than or equal to 89.6%. By adopting the cellulosic fiber, the technical defects that in the prior art cellulosic fiber is single in function and poor in anti-mite or anti-mold effect are solved.

Description

A kind of cellulose fibre with antibacterial and mouldproof anti-bacteria and mite-proof functional and preparation method thereof
Technical field
The invention belongs to functional cellulose fibre technology field, particularly relate to one and there is the anti-demodicid mite of antibacterial and mouldproof Cellulose fibre of function and preparation method thereof.
Background technology
Viscose rayon goods have moisture absorption, good permeability, feature comfortable and easy to wear, it is thus achieved that widely should With.But China's viscose rayon majority is common variety, along with raising and healthy, the ring of living standards of the people Protecting the continuous enhancing of consciousness, common variety does not the most adapt to the demand of market and enterprise development, carries forward vigorously The functional fiber of exploitation health, environment-friendly products and green has become as trend of the times.
Acarid belongs to the animal that a class build of Arthropoda Arachnoidea wide abdomen subclass is small, body size General the most all in 0.5 millimeter, the harm of human body is mainly reflected in parasitism, sting thorn, poison is stung, suck blood, Anaphylactic disease, the aspect such as spread disease, and healthy to the mankind causes serious harm.Mycete is silk Being commonly called as of shape fungus, implies that " mouldy fungus ", and the existence of mycete can produce a lot of unfavorable shadows to textile Ring, as fiber is degraded, produces ugly color and luster, given off an unpleasant smell.People contacts mouldy Textile after, the textile with mycete can invade blood by the pore of human skin and draw Sending out disease, cardinal symptom has allergy, cough, headache etc..
Semen Cassiae is leguminous herbaceous plant's Semen Cassiae or the mature seed of little Semen Cassiae, and bitter in the mouth, sweet and property are shied, tool There are the functions such as clearing away liver-fire, wind-damp dispelling, tonifying kidney and improving eyesight.Modern pharmacological research confirms, having contained by Semen Cassiae Effect composition has the regulation effect such as immune, antibacterial, anticancer, blood pressure lowering, regulation blood fat and eyesight-improving bowels-relaxing, Acarid, staphylococcus aureus, escherichia coli, streptococcus pneumoniae etc. all there is inhibitory action in various degree. In addition to medicinal ingredient, Semen Cassiae is possibly together with multivitamin and abundant aminoacid, fat, carbon hydrate Things etc., its health care is increasingly subject to the attention of people in recent years.Herba Houttuyniae is a kind of natural antibiotic. Modern pharmacology test shows, Herba Houttuyniae has the effects such as antibacterial, antiviral, raising immunity of organisms, right Various microorganisms (especially yeast and mycete) all have inhibitory action, streptococcus, the gold to hemolytic Staphylococcus aureus, hemophilus influenza, micrococcus catarrhalis, streptococcus pneumoniae have obvious inhibitory action, have simultaneously There are radiation resistance and the effect of enhancing human body immunity function.Ramulus Et Folium Picrasmae is quassia, and China mainly divides Cloth is each provinces and regions on the south the Yellow River, have the effect of heat-clearing and toxic substances removing, removing dampness and killing parasites.
From above-mentioned background content it can be seen that prior art, cellulose fibre is primarily present function list One, anti-demodicid mite or the technological deficiency of anti-mold effect difference.
Therefore, develop a kind of cellulose fibre, be used for solving in prior art, cellulose fibre function Demodicid mite single, anti-or the technological deficiency of anti-mold effect difference, become urgently to be resolved hurrily the asking of those skilled in the art Topic.
Summary of the invention
In view of this, the invention provides a kind of cellulose fibre with antibacterial and mouldproof anti-bacteria and mite-proof functional and Preparation method, is used for solving in prior art, and cellulose fibre function singleness, anti-demodicid mite or anti-mold effect are poor Technological deficiency.
The invention provides a kind of cellulose fibre, described cellulose fibre includes: Semen Cassiae, Herba Houttuyniae, Ramulus Et Folium Picrasmae and cellulose fibre matrix.
Present invention also offers a kind of preparation method including above-mentioned cellulose fibre, described preparation method is: Step one, prepare Semen Cassiae-Herba Houttuyniae microcapsule;Step 2, prepare viscose spinning solution: Ramulus Et Folium Picrasmae pulp Glue after mixing with other pulp, obtains viscose spinning solution, and other pulp described is selected from: wood pulps, cotton One or more in pulp and bamboo pulp;Step 3, prepare co-blended spinning stock solution;Described Semen Cassiae-fish Raw meat grass microcapsule and the mixing of described viscose spinning solution, described Semen Cassiae-Herba Houttuyniae microcapsule and described viscose The mass ratio of spinning solution is (5~16): 100, prepares co-blended spinning stock solution;Step 4, spinning and after Process: described co-blended spinning stock solution spinning bunchy after coagulating bath, post-treated product.
Preferably, the preparation method of Semen Cassiae-Herba Houttuyniae microcapsule is: Semen Cassiae and Herba Houttuyniae are mixed after pulverizing Closing, sieve to obtain Semen Cassiae-Heartleaf Houttuynia Herb;Described Semen Cassiae-Heartleaf Houttuynia Herb is dissolved in ethanol solution, For the first time after agitation grinding, filter, collect filtrate, described filtrate is concentrated to give Semen Cassiae-Herba Houttuyniae clear paste; After being mixed with emulsifying agent, initiator and water by described Semen Cassiae-Herba Houttuyniae clear paste, stir to obtain emulsion, to Dripping methyl methacrylate in described emulsion, stand sucking filtration after reaction, sucking filtration thing is after washing with alcohol It is dried, obtains Semen Cassiae-Herba Houttuyniae microcapsule.
Preferably, the particle diameter of described Semen Cassiae-Heartleaf Houttuynia Herb is 20~100 mesh, described Semen Cassiae-fish raw meat The quality at grass meal end is (10~30) with the volume ratio of described ethanol solution: 1, the volume of described ethanol solution Concentration is 60%~95%, and the pressure of described first time agitation grinding is 0.4~0.8Mpa, and described first time stirs The temperature mixing grinding is 10~20 DEG C, and the time of described first time agitation grinding is 30~120min, described breast Agent is selected from: Tween-80, dodecylbenzene sodium sulfonate, Span-80 and OP-10 one or more, Described initiator is benzoyl peroxide or azodiisobutyronitrile, described Semen Cassiae-Herba Houttuyniae clear paste and emulsifying The mass ratio of agent, initiator and water is 100:(1.0~5.0): (0.5~2.5): (200~700), described Diameter D≤1.2 μm of Semen Cassiae-Herba Houttuyniae microcapsule.
Preferably, the mass ratio of described Ramulus Et Folium Picrasmae pulp and other pulp described is (1~10): 100;Described hardship The preparation method of wood pulps is: Ramulus Et Folium Picrasmae presoaks to obtain preimpregnation product in sodium sulfite solution, and described preimpregnation is produced Thing carries out steam explosion and processes to obtain steam explosion product, after being immersed in NMMO process after the washing of described steam explosion product, Washing, filter and dry after, obtain Ramulus Et Folium Picrasmae pulp.
Preferably, described sodium sulfite solution for 5.0%~20%, Ramulus Et Folium Picrasmae and described sodium sulfite solution Mass ratio be 1:(10~30), the temperature of described preimpregnation is 50~90 DEG C, the time of described preimpregnation be 12~ 36h, the temperature of described immersion is 80~120 DEG C, and the time of described immersion is 1.0~3.0h.
Preferably, described coagulating bath need to add sulphuric acid 85~120g/L, aluminum sulfate 5.0~10.0g/L, sulphuric acid Zinc 0~5.0g/L and sodium sulfate 280~320g/L.
Preferably, described post processing includes: desulfurization, oil bath, washes and dries.
Preferably, described desulfurization need to add Na2SO35.0~8.0g/L material to be desulfurization, and described oil bath need to add Enter 4.0~6.0g/L and treat oil bath material.
Present invention also offers a kind of product including that above-mentioned cellulose fibre or above-mentioned preparation method obtain to exist Anti-demodicid mite, mildew-resistant and the application in antibacterial field.
In sum, the invention provides a kind of cellulose fibre, including: Semen Cassiae, Herba Houttuyniae, hardship Wood and cellulose fibre matrix.Present invention also offers the preparation method of a kind of above-mentioned cellulose fibre, this The product that invention additionally provides a kind of above-mentioned cellulose fibre or above-mentioned preparation method obtains is in anti-demodicid mite, mildew-resistant Application with antibacterial field.Can obtain through measuring, compared with conventional viscose rayon, the present invention provides Cellulose fibre suppression ratio >=80% to acarid, has stronger anti-demodicid mite effect, and mildew-resistant grade can reach 2 grades and level above in GB/T 24346-2009 " evaluation of textile fungicidal properties ", to golden yellow Staphylococcic suppression ratio >=90.2%, to colibacillary suppression ratio >=91.8%, to Candida albicans Suppression ratio >=89.6%.Illustrate the cellulose fibre that the present invention provides, take into account simultaneously good anti-demodicid mite, Mildew-resistant and anti-microbial property, solve in prior art, cellulose fibre function singleness, anti-demodicid mite or mildew-resistant effect The poorest technological deficiency.
Detailed description of the invention
The invention provides a kind of cellulose fibre with antibacterial and mouldproof anti-bacteria and mite-proof functional and preparation method thereof, For solving in prior art, cellulose fibre function singleness, anti-demodicid mite or the technological deficiency of anti-mold effect difference.
Technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that institute The embodiment described is only a part of embodiment of the present invention rather than whole embodiments.Based on this Embodiment in bright, those of ordinary skill in the art are obtained under not making creative work premise Every other embodiment, broadly falls into the scope of protection of the invention.
In order to the present invention is described in more detail, below in conjunction with embodiment, the one that the present invention provides is had antibacterial Cellulose fibre of mildew-resistant anti-bacteria and mite-proof functional and preparation method thereof, is specifically described.
Embodiment 1
Present embodiments provide prepare a kind of specification be 1.11dtex*32mm there is anti-demodicid mite, mildew-resistant and anti- The cellulose fibre of bacterium function.
Step one, prepare Semen Cassiae-Herba Houttuyniae alcohol extraction thing microcapsule
Semen Cassiae and Herba Houttuyniae are pulverized, obtains Semen Cassiae and Herba Houttuyniae mixed powder, mixed powder Particle diameter be 120 mesh, standby.Semen Cassiae and the Herba Houttuyniae powder body of above-mentioned pulverizing are placed in pressure pan, Being that 30:1 adds in the ethanol solution that concentration is 60% by bath raio, holding temperature stabilization is at 10 DEG C, at 0.4MPa Pressure effect under be stirred grinding after 120min, the feed liquid of process is filtered, obtained respectively Filtrate and material slag, material slag is given up, and then filtrate carries out heating and concentrates, remove unnecessary moisture and second Alcohol, obtains mainly containing the clear pasty masses of Semen Cassiae and Herba Houttuyniae extract.Clear paste by above-mentioned preparation Shape material, emulsifying agent Tween-80, initiator benzoyl peroxide and distilled water are put into heating, are stirred Mixing in the equipment of device, pasty masses, emulsifying agent, initiator and distilled water used is 100:1.0:0.5:200 (calculating in mass ratio), makes the clear pasty masses containing Semen Cassiae and Herba Houttuyniae extract form stable breast Change liquid;Then methyl methacrylate is slowly dropped in above-mentioned emulsion, carries out prepolymerization reaction and gather Close reaction.After reaction terminates, gained reactant liquor is stood, sucking filtration, and take out filtered material by washing with alcohol And be dried, i.e. can get Semen Cassiae-Herba Houttuyniae extract microcapsule, prepared Semen Cassiae-Herba Houttuyniae The Particle size requirements of extract microcapsules be D97 be 1.198 μm.
Step 2, prepare viscose spinning solution
By Ramulus Et Folium Picrasmae impurity removing, dedusting, being cut into applicable size, screening is with standby.By above-mentioned Ramulus Et Folium Picrasmae raw material Being immersed in mass fraction is to carry out pre-preg in 5.0% sodium sulfite, and dipping bath is than for 1:30, pre-stain temperature Degree is 50 DEG C, and the time is 36h;The Ramulus Et Folium Picrasmae raw material obtained after above-mentioned process is put into Steam explosion treatment set Steam explosion process is carried out in Bei.By the Ramulus Et Folium Picrasmae raw material after Steam explosion treatment obtained above wash after It is immersed in NMMO process 3.0h under the conditions of 80 DEG C, then washes, filter, dry prepared Ramulus Et Folium Picrasmae pulp. Being raw material by Ramulus Et Folium Picrasmae pulp and wood pulps, wherein Ramulus Et Folium Picrasmae pulp is 1:100 with the mass ratio of wood pulps, passes through Conventional viscose preparation technology prepares viscose spinning solution.
Step 3, prepare co-blended spinning stock solution
Front injection device is spun in utilization, and effective ingredient calculates and adds content of alphacellulose 5.0% in viscose spinning The Semen Cassiae-Herba Houttuyniae extract microcapsule of above-mentioned preparation, through follow-up known viscose glue preparation section, system Standby co-blended spinning stock solution.
Step 4, spinning and post processing
By above-mentioned prepared co-blended spinning stock solution by the coagulating bath adjusted, coagulation bath composition is sulphuric acid 85g/L, aluminum sulfate 5.0g/L, zinc sulfate 5.0g/L, sodium sulfate 280g/L carry out spinning, nascent tow warp Molding tow is obtained after crossing drawing-off.Gained tow is through cutting off, relaxing sulfur removal technology, finish application bath, washing Etc. concise bath, wherein desulfurization bath: Na2SO35.0g/L, oil bath: 4.0g/L, after not bleaching and drying, Obtain the cellulose fibre with anti-demodicid mite antimildew and antibacterial function.
Containing Semen Cassiae, Herba Houttuyniae in the fiber that specification is 1.11dtex*32mm of the present embodiment 1 preparation And the functional component such as Ramulus Et Folium Picrasmae, compared with conventional viscose rayon, the fiber the prepared suppression to acarid Rate 83%, mildew-resistant grade can reach 2 in GB/T 24346-2009 " evaluation of textile fungicidal properties " Level level.Suppression ratio 90.2% to staphylococcus aureus, to colibacillary suppression ratio 91.8%, right The suppression ratio 89.2% of Candida albicans, the antibacterial experiment in the present embodiment, with reference to GB/T20944.3-2008 " the evaluation third portion of antibacterial textile performance: concussion method " is carried out.
Embodiment 2
Present embodiments provide prepare a kind of specification be 1.56dtex*38mm there is anti-demodicid mite, mildew-resistant and anti- The cellulose fibre of bacterium function.
Step one, prepare Semen Cassiae-Herba Houttuyniae alcohol extraction thing microcapsule
Semen Cassiae and Herba Houttuyniae are pulverized, obtains Semen Cassiae and Herba Houttuyniae mixed powder, mixed powder Particle diameter be 98 mesh, standby.Semen Cassiae and the Herba Houttuyniae powder body of above-mentioned pulverizing are placed in pressure pan, press Bath raio is that 25:1 adds in the ethanol solution that concentration is 69%, and holding temperature stabilization is at 12 DEG C, at 0.5MPa Pressure effect under be stirred grinding after 107min, the feed liquid of process is filtered, obtained respectively Filtrate and material slag, material slag is given up, and then filtrate carries out heating and concentrates, remove unnecessary moisture and second Alcohol, obtains mainly containing the clear pasty masses of Semen Cassiae and Herba Houttuyniae extract.Clear paste by above-mentioned preparation Shape material, emulsifying agent dodecylbenzene sodium sulfonate, initiator azodiisobutyronitrile and distilled water put into Heating, agitating device equipment in, pasty masses, emulsifying agent, initiator and distilled water used are (100:1.6:0.9:289 calculating in mass ratio), make the clear pasty masses containing Semen Cassiae and Herba Houttuyniae extract Form stable emulsion;Then methyl methacrylate is slowly dropped in above-mentioned emulsion, carries out Prepolymerization reaction and polyreaction.After reaction terminates, gained reactant liquor is stood, sucking filtration, and wash with ethanol Wash and take out filtered material and be dried, i.e. can get Semen Cassiae-Herba Houttuyniae extract microcapsule, prepared The Particle size requirements of Semen Cassiae-Herba Houttuyniae extract microcapsule be D97 be 1.156 μm.
Step 2, prepare viscose spinning solution
By Ramulus Et Folium Picrasmae impurity removing, dedusting, being cut into applicable size, screening is with standby.By above-mentioned Ramulus Et Folium Picrasmae raw material Being immersed in mass fraction is to carry out pre-preg in 8.6% sodium sulfite, and dipping bath is than for 1:25, pre-stain temperature Degree is 62 DEG C, and the time is 31h;The Ramulus Et Folium Picrasmae raw material obtained after above-mentioned process is put into Steam explosion treatment set Steam explosion process is carried out in Bei.By the Ramulus Et Folium Picrasmae raw material after Steam explosion treatment obtained above wash after It is immersed in NMMO process 2.5h under the conditions of 86 DEG C, then washes, filter, dry prepared Ramulus Et Folium Picrasmae pulp. Being raw material by Ramulus Et Folium Picrasmae pulp and Cotton Pulp, wherein Ramulus Et Folium Picrasmae pulp is 1:85 with the mass ratio of Cotton Pulp, passes through Conventional viscose preparation technology prepares viscose spinning solution.
Step 3, prepare co-blended spinning stock solution
Front injection device is spun in utilization, and effective ingredient calculates and adds content of alphacellulose 7.6% in viscose spinning The Semen Cassiae-Herba Houttuyniae extract microcapsule of above-mentioned preparation, through follow-up known viscose glue preparation section, system Standby co-blended spinning stock solution.
Step 4, spinning and post processing
By above-mentioned prepared co-blended spinning stock solution by the coagulating bath adjusted, coagulation bath composition is sulphuric acid 85g/L, aluminum sulfate 6.2g/L, zinc sulfate 4.6g/L, sodium sulfate 292g/L carry out spinning, nascent tow warp Molding tow is obtained after crossing drawing-off.Gained tow is through cutting off, relaxing sulfur removal technology, finish application bath, washing Etc. concise bath, wherein desulfurization bath: Na2SO35.6g/L, oil bath: 4.3g/L, after not bleaching and drying, Obtain the cellulose fibre with anti-demodicid mite antimildew and antibacterial function.
Containing Semen Cassiae, Herba Houttuyniae in the fiber that specification is 1.33dtex*38mm of the present embodiment 2 preparation And the functional component such as Ramulus Et Folium Picrasmae, compared with conventional viscose rayon, the fiber the prepared suppression to acarid Rate 85%, mildew-resistant grade can reach 1 in GB/T 24346-2009 " evaluation of textile fungicidal properties " Level level.Suppression ratio 92.5% to staphylococcus aureus, to colibacillary suppression ratio 93.9%, right The suppression ratio 91.2% of Candida albicans, the antibacterial experiment in the present embodiment, with reference to GB/T20944.3-2008 " the evaluation third portion of antibacterial textile performance: concussion method " is carried out.
Embodiment 3
Present embodiments provide prepare a kind of specification be 1.56dtex*38mm there is anti-demodicid mite, mildew-resistant and anti- The cellulose fibre of bacterium function.
Step one, prepare Semen Cassiae-Herba Houttuyniae alcohol extraction thing microcapsule
Semen Cassiae and Herba Houttuyniae are pulverized, obtains Semen Cassiae and Herba Houttuyniae mixed powder, mixed powder Particle diameter be 75 mesh, standby.Semen Cassiae and the Herba Houttuyniae powder body of above-mentioned pulverizing are placed in pressure pan, press Bath raio is that 20:1 adds in the ethanol solution that concentration is 76%, and holding temperature stabilization is at 15 DEG C, at 0.6MPa Pressure effect under be stirred grinding after 88min, the feed liquid of process is filtered, obtained respectively Filtrate and material slag, material slag is given up, and then filtrate carries out heating and concentrates, remove unnecessary moisture and second Alcohol, obtains mainly containing the clear pasty masses of Semen Cassiae and Herba Houttuyniae extract.Clear paste by above-mentioned preparation Shape material, emulsifying agent Span-80, initiator azodiisobutyronitrile and distilled water are put into heating, stirring In the equipment of device, pasty masses, emulsifying agent, initiator and distilled water used is 100:2.5:1.5:400 (calculating in mass ratio), makes the clear pasty masses containing Semen Cassiae and Herba Houttuyniae extract form stable breast Change liquid;Then methyl methacrylate is slowly dropped in above-mentioned emulsion, carries out prepolymerization reaction and gather Close reaction.After reaction terminates, gained reactant liquor is stood, sucking filtration, and take out filtered material by washing with alcohol And be dried, i.e. can get Semen Cassiae-Herba Houttuyniae extract microcapsule, prepared Semen Cassiae-Herba Houttuyniae The Particle size requirements of extract microcapsules be D97 be 1.185 μm.
Step 2, prepare viscose spinning solution
By Ramulus Et Folium Picrasmae impurity removing, dedusting, being cut into applicable size, screening is with standby.By above-mentioned Ramulus Et Folium Picrasmae raw material Being immersed in mass fraction is to carry out pre-preg in 12.5% sodium sulfite, and dipping bath is than for 1:20, pre-stain temperature Degree is 75 DEG C, and the time is 25h;The Ramulus Et Folium Picrasmae raw material obtained after above-mentioned process is put into Steam explosion treatment set Steam explosion process is carried out in Bei.By the Ramulus Et Folium Picrasmae raw material after Steam explosion treatment obtained above wash after It is immersed in NMMO process 2.0h under the conditions of 105 DEG C, then washes, filter, dry prepared Ramulus Et Folium Picrasmae slurry The dregs of rice.Being raw material by Ramulus Et Folium Picrasmae pulp and Cotton Pulp, wherein Ramulus Et Folium Picrasmae pulp is 1:50 with the mass ratio of bamboo pulp, Viscose spinning solution is prepared through conventional viscose preparation technology.
Step 3, prepare co-blended spinning stock solution
Front injection device is spun in utilization, and effective ingredient calculates and adds content of alphacellulose 11.5% in viscose spinning The Semen Cassiae-Herba Houttuyniae extract microcapsule of above-mentioned preparation, through follow-up known viscose glue preparation section, system Standby co-blended spinning stock solution.
Step 4, spinning and post processing
By above-mentioned prepared co-blended spinning stock solution by the coagulating bath adjusted, coagulation bath composition is sulphuric acid 105g/L, aluminum sulfate 8.3g/L, zinc sulfate 3.5g/L, sodium sulfate 300g/L carry out spinning, nascent tow Molding tow is obtained after drawing-off.Gained tow is through cutting off, relaxing sulfur removal technology, finish application bath, water Concise bath, wherein desulfurization bath: the Na such as wash2SO36.8g/L, oil bath: 4.8g/L, after not bleaching and drying, Obtain the cellulose fibre with anti-demodicid mite antimildew and antibacterial function.
Containing Semen Cassiae, Herba Houttuyniae in the fiber that specification is 1.56dtex*38mm of the present embodiment 3 preparation And the functional component such as Ramulus Et Folium Picrasmae, compared with conventional viscose rayon, the fiber the prepared suppression to acarid Rate 89%, mildew-resistant grade can reach 1 in GB/T 24346-2009 " evaluation of textile fungicidal properties " Level level.Suppression ratio 95.6% to staphylococcus aureus, to colibacillary suppression ratio 94.8%, right The suppression ratio 93.4% of Candida albicans, the antibacterial experiment in the present embodiment, with reference to GB/T20944.3-2008 " the evaluation third portion of antibacterial textile performance: concussion method " is carried out.
Embodiment 4
Present embodiments provide prepare a kind of specification be 1.67dtex*38mm there is anti-demodicid mite, mildew-resistant and anti- The cellulose fibre of bacterium function.
Step one, prepare Semen Cassiae-Herba Houttuyniae alcohol extraction thing microcapsule
Semen Cassiae and Herba Houttuyniae are pulverized, obtains Semen Cassiae and Herba Houttuyniae mixed powder, mixed powder Particle diameter be 50 mesh, standby.Semen Cassiae and the Herba Houttuyniae powder body of above-mentioned pulverizing are placed in pressure pan, press Bath raio is that 15:1 adds in the ethanol solution that concentration is 88%, and holding temperature stabilization is at 18 DEG C, at 0.7MPa Pressure effect under be stirred grinding after 55min, the feed liquid of process is filtered, obtained respectively Filtrate and material slag, material slag is given up, and then filtrate carries out heating and concentrates, remove unnecessary moisture and second Alcohol, obtains mainly containing the clear pasty masses of Semen Cassiae and Herba Houttuyniae extract.Clear paste by above-mentioned preparation Shape material, emulsifier op-10, initiator benzoyl peroxide and distilled water are put into heating, stirring dress In the equipment put, pasty masses, emulsifying agent, initiator and distilled water used is that 100:3.6:2.0:550 (presses Mass ratio calculates), make the clear pasty masses containing Semen Cassiae and Herba Houttuyniae extract form stable emulsion; Then methyl methacrylate is slowly dropped in above-mentioned emulsion, carries out prepolymerization reaction and polyreaction. After reaction terminates, gained reactant liquor is stood, sucking filtration, and take out filtered material by washing with alcohol and do Dry, i.e. can get Semen Cassiae-Herba Houttuyniae extract microcapsule, prepared Semen Cassiae-Herba Houttuyniae extract is micro- The Particle size requirements of capsule be D97 be 1.177 μm.
Step 2, prepare viscose spinning solution
By Ramulus Et Folium Picrasmae impurity removing, dedusting, being cut into applicable size, screening is with standby.By above-mentioned Ramulus Et Folium Picrasmae raw material Being immersed in mass fraction is to carry out pre-preg in 16.8% sodium sulfite, dipping bath ratio for 1:15, preimpregnation temperature Degree is 86 DEG C, and the time is 19h;The Ramulus Et Folium Picrasmae raw material obtained after above-mentioned process is put into Steam explosion treatment set Steam explosion process is carried out in Bei.By the Ramulus Et Folium Picrasmae raw material after Steam explosion treatment obtained above wash after It is immersed in NMMO process 1.5h under the conditions of 114 DEG C, then washes, filter, dry prepared Ramulus Et Folium Picrasmae slurry The dregs of rice.It is raw material by Ramulus Et Folium Picrasmae pulp, bamboo pulp and Cotton Pulp, wherein Ramulus Et Folium Picrasmae pulp and the mass ratio of Cotton Pulp For 1:20, prepare viscose spinning solution through conventional viscose preparation technology.
Step 3, prepare co-blended spinning stock solution
Front injection device is spun in utilization, and effective ingredient calculates and adds content of alphacellulose 14.0% in viscose spinning The Semen Cassiae-Herba Houttuyniae extract microcapsule of above-mentioned preparation, through follow-up known viscose glue preparation section, system Standby co-blended spinning stock solution.
Step 4, spinning and post processing
By above-mentioned prepared co-blended spinning stock solution by the coagulating bath adjusted, coagulation bath composition is sulphuric acid 112g/L, aluminum sulfate 9.0g/L, zinc sulfate 2.7g/L, sodium sulfate 312g/L carry out spinning, nascent tow Molding tow is obtained after drawing-off.Gained tow is through cutting off, relaxing sulfur removal technology, finish application bath, water Concise bath, wherein desulfurization bath: the Na such as wash2SO37.2g/L, oil bath: 5.1g/L, after not bleaching and drying, Obtain the cellulose fibre with anti-demodicid mite antimildew and antibacterial function.
Containing Semen Cassiae, Herba Houttuyniae in the fiber that specification is 1.67dtex*38mm of the present embodiment 4 preparation And the functional component such as Ramulus Et Folium Picrasmae, compared with conventional viscose rayon, the fiber the prepared suppression to acarid Rate 92%, mildew-resistant grade can reach in GB/T 24346-2009 " evaluation of textile fungicidal properties " 0 grade of level.Suppression ratio 96.8% to staphylococcus aureus, to colibacillary suppression ratio 95.9%, Suppression ratio 94.6% to Candida albicans, the antibacterial experiment in the present embodiment, reference GB/T20944.3-2008 " the evaluation third portion of antibacterial textile performance: concussion method " is carried out.
Embodiment 5
Present embodiments provide prepare a kind of specification be 2.22dtex*38mm there is anti-demodicid mite, mildew-resistant and anti- The cellulose fibre of bacterium function.
Step one, prepare Semen Cassiae-Herba Houttuyniae alcohol extraction thing microcapsule
Semen Cassiae and Herba Houttuyniae are pulverized, obtains Semen Cassiae and Herba Houttuyniae mixed powder, mixed powder Particle diameter be 20 mesh, standby.Semen Cassiae and the Herba Houttuyniae powder body of above-mentioned pulverizing are placed in pressure pan, press Bath raio is that 10:1 adds in the ethanol solution that concentration is 95%, and holding temperature stabilization is at 20 DEG C, at 0.4MPa Pressure effect under be stirred grinding after 30min, the feed liquid of process is filtered, obtained respectively Filtrate and material slag, material slag is given up, and then filtrate carries out heating and concentrates, remove unnecessary moisture and second Alcohol, obtains mainly containing the clear pasty masses of Semen Cassiae and Herba Houttuyniae extract.Clear paste by above-mentioned preparation Shape material, emulsifying agent dodecylbenzene sodium sulfonate, initiator dodecylbenzene sodium sulfonate and distilled water are put into With heating, agitating device equipment in, pasty masses, emulsifying agent, initiator and distilled water used For 100:5.0:2.5:700 (calculating in mass ratio), make the clear paste shape containing Semen Cassiae and Herba Houttuyniae extract Material forms stable emulsion;Then methyl methacrylate is slowly dropped in above-mentioned emulsion, Carry out prepolymerization reaction and polyreaction.After reaction terminates, gained reactant liquor is stood, sucking filtration, and use second Alcohol washing is taken out filtered material and is dried, and i.e. can get Semen Cassiae-Herba Houttuyniae extract microcapsule, made The Particle size requirements of standby Semen Cassiae-Herba Houttuyniae extract microcapsule be D97 be 1.187 μm.
Step 2, prepare viscose spinning solution
By Ramulus Et Folium Picrasmae impurity removing, dedusting, being cut into applicable size, screening is with standby.By above-mentioned Ramulus Et Folium Picrasmae raw material Being immersed in mass fraction is to carry out pre-preg in 20% sodium sulfite, and dipping bath is than for 1:10, pre-stain temperature Degree is 90 DEG C, and the time is 12h;The Ramulus Et Folium Picrasmae raw material obtained after above-mentioned process is put into Steam explosion treatment set Steam explosion process is carried out in Bei.By the Ramulus Et Folium Picrasmae raw material after Steam explosion treatment obtained above wash after It is immersed in NMMO process 1.0h under the conditions of 120 DEG C, then washes, filter, dry prepared Ramulus Et Folium Picrasmae slurry The dregs of rice.Being raw material by Ramulus Et Folium Picrasmae pulp, bamboo pulp and Cotton Pulp, wherein Ramulus Et Folium Picrasmae pulp mixes with bamboo pulp-Cotton Pulp The mass ratio of compound is 1:85, prepares viscose spinning solution through conventional viscose preparation technology.
Step 3, prepare co-blended spinning stock solution
Front injection device is spun in utilization, and effective ingredient calculates and adds content of alphacellulose 16.0% in viscose spinning The Semen Cassiae-Herba Houttuyniae extract microcapsule of above-mentioned preparation, through follow-up known viscose glue preparation section, system Standby co-blended spinning stock solution.
Step 4, spinning and post processing
By above-mentioned prepared co-blended spinning stock solution by the coagulating bath adjusted, coagulation bath composition is sulphuric acid 120g/L, aluminum sulfate 10.0g/L, sodium sulfate 320g/L carry out spinning, and nascent tow obtains after drawing-off Molding tow.Gained tow passes through cut-out, relaxes the concise baths such as sulfur removal technology, finish application bath, washing, its Middle desulfurization is bathed: Na2SO38.0g/L, oil bath: 6.0g/L, after not bleaching and drying, obtain having anti-demodicid mite The cellulose fibre of antimildew and antibacterial function.
Containing Semen Cassiae, Herba Houttuyniae in the fiber that specification is 2.22dtex*56mm of the present embodiment 5 preparation And the functional component such as Ramulus Et Folium Picrasmae, compared with conventional viscose rayon, the fiber the prepared suppression to acarid Rate 96%, mildew-resistant grade can reach 0 in GB/T 24346-2009 " evaluation of textile fungicidal properties " Level level.Suppression ratio 98.1% to staphylococcus aureus, to colibacillary suppression ratio 97.0%, right The suppression ratio 96.2% of Candida albicans, the antibacterial experiment in the present embodiment, with reference to GB/T20944.3-2008 " the evaluation third portion of antibacterial textile performance: concussion method " is carried out.
In sum, the invention provides a kind of cellulose fibre, including: Semen Cassiae, Herba Houttuyniae, hardship Wood and cellulose fibre matrix.Present invention also offers the preparation method of a kind of above-mentioned cellulose fibre, this The product that invention additionally provides a kind of above-mentioned cellulose fibre or above-mentioned preparation method obtains is in anti-demodicid mite, mildew-resistant Application with antibacterial field.Can obtain through measuring, compared with conventional viscose rayon, the present invention provides Cellulose fibre suppression ratio >=80% to acarid, has stronger anti-demodicid mite effect, and mildew-resistant grade can reach 2 grades and level above in GB/T 24346-2009 " evaluation of textile fungicidal properties ", to golden yellow Staphylococcic suppression ratio >=90.2%, to colibacillary suppression ratio >=91.8%, to Candida albicans Suppression ratio >=89.6%.Illustrate the cellulose fibre that the present invention provides, take into account simultaneously good anti-demodicid mite, Mildew-resistant and anti-microbial property, solve in prior art, cellulose fibre function singleness, anti-demodicid mite or mildew-resistant effect The poorest technological deficiency.
The above is only the preferred embodiment of the present invention, it is noted that general for the art For logical technical staff, under the premise without departing from the principles of the invention, it is also possible to make some improvement and profit Decorations, these improvements and modifications also should be regarded as protection scope of the present invention.

Claims (10)

1. a cellulose fibre, it is characterised in that described cellulose fibre includes: Semen Cassiae, fish raw meat Grass, Ramulus Et Folium Picrasmae and cellulose fibre matrix.
2. the preparation method of the cellulose fibre included described in claim 1, it is characterised in that institute Stating preparation method is:
Step one, prepare Semen Cassiae-Herba Houttuyniae microcapsule;
Step 2, prepare viscose spinning solution: Ramulus Et Folium Picrasmae pulp and other pulp mix after glue, obtain viscose Spinning solution, other pulp described is selected from: one or more in wood pulps, Cotton Pulp and bamboo pulp;
Step 3, prepare co-blended spinning stock solution;Described Semen Cassiae-Herba Houttuyniae microcapsule and described viscose spinning Stock solution mixes, and the mass ratio of described Semen Cassiae-Herba Houttuyniae microcapsule and described viscose spinning solution is (5~16): 100, prepare co-blended spinning stock solution;
Step 4, spinning and post processing: described co-blended spinning stock solution spinning bunchy after coagulating bath, through after Process to obtain product.
Preparation method the most according to claim 2, it is characterised in that Semen Cassiae-Herba Houttuyniae microcapsule Preparation method be: Semen Cassiae and Herba Houttuyniae mix after pulverizing, and sieve to obtain Semen Cassiae-Heartleaf Houttuynia Herb;Will Described Semen Cassiae-Heartleaf Houttuynia Herb is dissolved in ethanol solution, for the first time after agitation grinding, filters, collects filter Liquid, is concentrated to give Semen Cassiae-Herba Houttuyniae clear paste by described filtrate;By described Semen Cassiae-Herba Houttuyniae clear paste and emulsifying After agent, initiator and water mixing, stir to obtain emulsion, in described emulsion, drip methyl methacrylate Ester, stands sucking filtration after reaction, sucking filtration thing is dried after washing with alcohol, obtains Semen Cassiae-Herba Houttuyniae microcapsule.
Preparation method the most according to claim 3, it is characterised in that described Semen Cassiae-Herba Houttuyniae powder The particle diameter at end is 20~100 mesh, the quality of described Semen Cassiae-Heartleaf Houttuynia Herb and the volume of described ethanol solution Than being (10~30): 1, the volumetric concentration of described ethanol solution is 60%~95%, and described first time stirs The pressure ground is 0.4~0.8Mpa, and the temperature of described first time agitation grinding is 10~20 DEG C, described the The time of agitation grinding is 30~120min, and described emulsifying agent is selected from: Tween-80, detergent alkylate Sodium sulfonate, Span-80 and OP-10 one or more, described initiator is benzoyl peroxide or azo Bis-isobutyronitrile, described Semen Cassiae-Herba Houttuyniae clear paste is 100 with the mass ratio of emulsifying agent, initiator and water: (1.0~5.0): (0.5~2.5): (200~700), the diameter of described Semen Cassiae-Herba Houttuyniae microcapsule D≤1.2μm。
Preparation method the most according to claim 2, it is characterised in that described Ramulus Et Folium Picrasmae pulp and described The mass ratio of other pulp is (1~10): 100;
The preparation method of described Ramulus Et Folium Picrasmae pulp is: Ramulus Et Folium Picrasmae presoaks to obtain preimpregnation product in sodium sulfite solution, Described preimpregnation product carries out steam explosion and processes to obtain steam explosion product, is immersed in NMMO after the washing of described steam explosion product After middle process, after washing, filter and drying, obtain Ramulus Et Folium Picrasmae pulp.
Preparation method the most according to claim 5, it is characterised in that described sodium sulfite solution Being 5.0%~20%, Ramulus Et Folium Picrasmae is 1:(10~30 with the mass ratio of described sodium sulfite solution), described preimpregnation Temperature be 50~90 DEG C, the time of described preimpregnation is 12~36h, the temperature of described immersion be 80~ 120 DEG C, the time of described immersion is 1.0~3.0h.
Preparation method the most according to claim 2, it is characterised in that described coagulating bath need to add sulfur Acid 85~120g/L, aluminum sulfate 5.0~10.0g/L, zinc sulfate 0~5.0g/L and sodium sulfate 280~320g/L.
Preparation method the most according to claim 2, it is characterised in that described post processing includes: de- Sulfur, oil bath, wash and dry.
Preparation method the most according to claim 8, it is characterised in that described desulfurization needs to add Na2SO35.0~8.0g/L materials to be desulfurization, described oil bath need to add 4.0~6.0g/L and treat oil bath material.
10. the cellulose fibre included described in claim 1 or claim 2 to 9 any one The product that described preparation method obtains is in anti-demodicid mite, mildew-resistant and the application in antibacterial field.
CN201610494383.1A 2016-06-27 2016-06-27 Cellulosic fiber with antibacterial anti-mold anti-mite functions and preparation method of cellulosic fiber Pending CN105926077A (en)

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CN114059234A (en) * 2021-11-26 2022-02-18 成都大学 Fruit and vegetable preservative film and preparation method and application thereof
CN114059234B (en) * 2021-11-26 2023-05-26 成都大学 Fruit and vegetable preservative film and preparation method and application thereof

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Application publication date: 20160907