The flaxen fiber and preparation method thereof of the modified preparation of one Plant Extracts
Technical field
The invention belongs to fibre modification fields, are related to flaxen fiber and its preparation side of the modified preparation of a Plant Extracts
Method.
Background technique
It is wet fast that flaxen fiber has many advantages, such as that strength height, moisture absorption dissipate, but the cellulose macromolecule degree of orientation and crystallinity are higher, table
No curling that face is straight causes big fiber rigidity, small, the obvolvent performance of elasticity and spinning property poor.
For the wearability and dyeability for improving its spinning property fabric, the general method for using chemical modification.Mainly
There are alkaline process, sulfonation method, urea method, cationization method etc..
Application No. is CN201711077894.4, it discloses a kind of preparation methods for being modified enhanced flaxen fiber, comprising:
It prepares working solution: using water as base fluid, using JFC bleeding agent as additive, being configured to bleeding agent working solution and keep the temperature dipping;Using this
The bond strength of modified enhanced flaxen fiber made from method, flaxen fiber and macromolecule PP fiber is high, low close so as to realize
Linen fiber composite plates under the conditions of degree still maintain higher intensity, and then realize the lightweight of linen fiber composite plates.
Application number: CN200710191881.X discloses a kind of fibrilia modified method, is related to a kind of fibrilia grafting amine
Change modified technique, the oxidizing agent solutions selective oxidations such as flaxen fiber sodium metaperiodate are first obtained into oxidation flaxen fiber, are then utilized
Oxidation flaxen fiber surface aldehydes and amine-terminated hyperbranced compound and its amino on quaternary ammonium salt surface react and with covalently bonded
It closes and grafting amination flaxen fiber is made, reaction speed is fast, and grafting efficiency is high, fastness is good, simple and easy to do.Obtained fiber surface introduces
Amino, imido grpup and quaternary ammonium salt branch abundant, are remarkably improved the dyeability of flaxen fiber, meanwhile, numb fibre also can be improved
Flexibility, hygroscopicity and the anti-microbial property of dimension.
Shaoxing University application No. is the patents of CN201610059805.2 to provide a kind of poly- cream of modified flaxen fiber
The preparation method of sour composite material, the modified flaxen fiber polylactic acid of fiber pretreatment → alkali process → waterproofing agent treatment → preparation are compound
Material → molding, in which: fiber pretreatment, which is taken, separates the root, middle part and taper of flaxen fiber, then by each position point
It is not cut off, shredding, mixing, then carries out subsequent alkali process, water-proofing treatment, alkali process can remove non-cellulose object with effect
Matter, while improving the intensity and toughness of fiber;Waterproofing agent treatment can improve the boundary of fiber and polylactic acid by hydrophobic surface
Face compatibility and adhesion strength, and fibrous mechanical property is influenced smaller.
In conclusion domestic at present less to the research of flaxen fiber, plant study on the modification and application to flaxen fiber are still located
In primary research and development and market exploration stage.
Summary of the invention
The present invention in order to solve the above technical problems, in view of the deficiencies of the prior art, provides one kind, is issued with realizing
Improving eyesight:
(1) flaxen fiber of the modified preparation of plant extracts of the present invention, breaking strength is high, content of formaldehyde 0, and elastic recovery rate is high,
It is low to dye fleck rate;
(2) flaxen fiber of the modified preparation of plant extracts of the present invention, to staphylococcus aureus, Candida albicans, Escherichia coli
Bacteriostasis rate it is low;Washing 50 times after, to staphylococcus aureus, Candida albicans, Escherichia coli bacteriostasis rate almost without reduction;
(3) flaxen fiber of the modified preparation of plant extracts of the present invention, chlorine-resistant float the oxygen that color fastness reduced rate is low, after chlorine rinsing 50 times
Index is high;
(4) flaxen fiber of the modified preparation of plant extracts of the present invention, flame retardant property is good, the oxygen index (OI) drop after washing 50 times, 100 times
It is low small.
In order to solve the above technical problems, the technical solution adopted by the present invention is as follows:
The flaxen fiber of the modified preparation of the plant extracts, breaking strength 8.8-9.4cN/dtex, content of formaldehyde 0mg/kg, elasticity
Response rate 62.4-66.9%, dyeing fleck rate are 0.00-0.005%.
It is further improvement to above-mentioned technical proposal below:
The flaxen fiber of the modified preparation of the plant extracts, it is 0.02-0.04% that chlorine-resistant, which floats color fastness reduced rate, and chlorine rinses 50 times
Oxygen index (OI) 28.0-28.2% afterwards.
The flaxen fiber of the modified preparation of the plant extracts, oxygen index (OI) 28.0-28.2%, the oxygen index (OI) after washing 50 times
28.0%, the oxygen index (OI) 27.7-27.9% after washing 100 times.
The present invention also provides the preparation method of the flaxen fiber of the modified preparation of a Plant Extracts, a kind of plant is mentioned
Take the flaxen fiber and preparation method thereof of the modified preparation of object, comprising the following steps: pretreatment, the preparation of A treatment fluid.
The pretreatment, including degumming, wash that material, high-temperature steam be stifling and drying;
The degumming: after ramie fiber crops former stem soak at room temperature 10-30 minutes, temperature is controlled between 25-50 DEG C, adds 2-5%'s
Composite bacteria agent stirs evenly, and is left to ferment 20-100h, is completed using fermentation to the destruction of pectin, lignin in fiber etc.
Degumming.
The composite bacteria agent, including Rhodopseudomonas palustris, trichoderma viride, bacillus subtilis, bite pectin Flavobacterium
With black green trichoderma, mass ratio 3:2:15:2:1.
The bacteria containing amount of the Rhodopseudomonas palustris is 10g/L, and trichoderma viride bacteria containing amount is 0.8g/L, bacillus subtilis
The bacteria containing amount of bacterium is 10g/L, and the bacteria containing amount for biting pectin Flavobacterium is 2.5g/L, and black green trichoderma bacteria containing amount is 0.4g/L.
The high-temperature steam is stifling: 112-130 DEG C of high-temperature steam fumigation temperature, high-temperature steam fumigation time 10-15min,
The moisture equilibration time 1-2 hours, second of high-temperature steam suffocating treatment 15-25min, the temperature of second of high-temperature steam was
110-125℃。
The preparation of the A treatment fluid, A inorganic agent include the raw material of following parts by weight:
10-20 parts of sulfamate-phenol-formaldehyde condensate, 10-15 parts of polysaccharide, 8-15 parts of polyoxyethylene tallow amine, dimethyl methyl
1-4 parts of amide, 2-5 parts of the talcum powder of 2000 mesh, 0.8-2 part of trichloroacetic acid, 6-10 parts of hydrogenated castor oil polyoxyethylene ether is steamed
60-100 parts of distilled water.
The polysaccharide is the mixture of galactomannans, β-Isosorbide-5-Nitrae-poly- D- Glucosamine and astragalus polyose, described
The mass ratio of the poly- D- Glucosamine of galactomannans, β -1,4- and astragalus polyose is 10:1:2;
The galactomannans, purity 98%, the protein of 0.5-1%, the fiber of 0.2-0.3%, 0.1% ash content;
The astragalus polyose, density 1.439g/cm3, 154.5 DEG C of fusing point, 406.3 DEG C of 760 mmHg of at of boiling point, flash-point 199.5
DEG C, refractive index 1.638.
The dimethylformamide, No. CAS be 68-12-2, No. EINECS be 200-679-5, -61 DEG C of fusing point, boiling point
153 DEG C, 20 DEG C, 136 °F of flash-point of 0.948 g/mL at of density.
The trichloroacetic acid, 56.0-58.0 DEG C of crystalline temperature, chloride (Cl)≤0.005%, sulfate (SO4)≤0.01%,
Nitrate (NO3)≤0.001%, phosphate (PO4)≤0.001%, ignition residue (in terms of sulfate)≤0.03%, heavy metal (with
Pb meter)≤0.0005%, iron (Fe)≤0.0005%.
The hydrogenated castor oil polyoxyethylene ether, appearance are pale yellow transparent grease (25 DEG C), saponification number 90-100 mg
KOH/g, cloud point (1% aqueous solution)≤30, moisture≤1.00%, pH value (1% aqueous solution) 5.0-7.0, HLB value 9-10.
The A inorganic agent the preparation method comprises the following steps:
By the parts by weight by sulfamate-phenol-formaldehyde condensate, polysaccharide, polyoxyethylene tallow amine, dimethylformamide,
The talcum powder of hydrogenated castor oil polyoxyethylene ether and 2000 mesh is mixed, and is stirred with the speed of 950rad/min, temperature 130
DEG C, the formic acid, trichloroacetic acid and distilled water of the parts by weight is added, stirs, time 9-14min, it is cooling, it crushes, be sieved
To A inorganic agent.
The preparation A treatment fluid, the A treatment fluid the preparation method comprises the following steps:
By the A inorganic agent of 2Kg step (1), according to 1:20 bath raio, the glacial acetic acid tune of 0.3-1.1% is added in 80-90 DEG C of temperature dissolution
Section pH value, adition process are stirred continuously, and filtering uses and (all dissolves the state that is translucent) after heat preservation 2 hours.
It further include flaxen fiber single treatment
Pretreated flaxen fiber is put into A treatment fluid, is mixed, is first warming up to 25 DEG C, keeps the temperature 20 minutes;
Then 95 DEG C are warming up to, heating rate is 3-5 DEG C/min, after 15min is placed in heat preservation,
The impulse electric field for using frequency to be 1.5kV/cm for 15Hz, electric field strength handles 13-20s, obtains electric field single treatment object.
Then object processed material of electric field is placed in sealed storage tank, is 1.25 × 10 in intensity under stream of nitrogen gas- 2w/in2Ultraviolet light and 1.75 × 108The gamma-rays of rads irradiates 5-10min, and the flow of nitrogen stream is 25-35ml/min, obtains purple
- γ processed material outside.
The carbonic acid sodium powder of 1.0-2.0gD90≤0.75um is added into ultraviolet-γ processed material, mixes, under magnetic stirring apparatus
7-17min is stirred, the impulse electric field for then using frequency to be 5.0kV/cm for 18Hz, electric field strength handles 25-35 s, obtains electric field
Secondary treatment object.
Continue after keeping placing 3-4min at 95 DEG C of temperature, removes sodium carbonate, take out washing, dry to moisture content < 5%.
Further include flaxen fiber secondary treatment:
A. plant dyeing agent solution is prepared, it is molten that the vegetable dyeing agent that concentration is 1-5% is made in vegetable dyeing agent addition deionized water
Liquid;
The vegetable dyeing agent, the Herba Menthae powder and Chloranthus glaber powder of the quality such as selection, the Herba Menthae powder, 99.5% crosses 500 mesh
Sieve, appearance: shallow green powder, it is loose, without agglomeration, it is visible by naked eyes impurity, color uniformity;Smell is uniform;Effective component
Content >=98.5%, moisture≤3%, total plate count < 99cfu/g, salmonella and Escherichia coli must not detect, and the shelf-life is
12 months;Effective component: menthol, menthones, menthyl acetate, limonene, isomenthone, peppermint esters, rheum emodin, big
Yellow phenol, robinin etc..
The Chloranthus glaber powder, 99.8% crosses 500 meshes, and appearance: brown ceramic powder, loose no agglomeration are visible by naked eyes miscellaneous
Matter, color uniformity;Smell is uniform;Active constituent content >=98.5%, moisture≤3%, total plate count < 99cfu/g, sramana
Salmonella and Escherichia coli must not detect, and the shelf-life is 12 months, and effective component is isofraxidin, left-handed class myrrh element first, prolongs
Fumarate, succinic acid, glycosides displayed, wherein Determination of isofraxidin 3.5-8.0%;
B. it is 2.0-20%, bath raio 1:10 that vegetable dyeing agent, which accounts for the percent mass ratio of flaxen fiber,;
C. flaxen fiber above-mentioned steps obtained is placed in vegetable dyeing agent solution bath (addition glacial acetic acid 1.2g/L, additive amount
Depending on water in dye vat), 2-5 DEG C of heating rate/min is warming up to 90 DEG C, handles time 15-35 minutes.
Using above-mentioned technology, the invention has the benefit that
(1) flaxen fiber of the modified preparation of plant extracts of the present invention, breaking strength 8.8-9.4cN/dtex, content of formaldehyde 0mg/
Kg, elastic recovery rate 62.4-66.9%, dyeing fleck rate are 0.00-0.005%;
(2) flaxen fiber of the modified preparation of plant extracts of the present invention, to staphylococcus aureus, Candida albicans, Escherichia coli
Bacteriostasis rate be respectively 91.5-92.6%, 96.3-96.4%, 97.7-99.0%;After washing 50 times, to staphylococcus aureus, white
Color candida albicans, Escherichia coli bacteriostasis rate be respectively 88.5-89.0%, 90.5-91.1%, 88.8-88.9%;
(3) flaxen fiber of the modified preparation of plant extracts of the present invention, it is 0.02-0.04%, chlorine rinsing that chlorine-resistant, which floats color fastness reduced rate,
Oxygen index (OI) (effective chlorine density 1.2g/l) 28.0-28.2% after 50 times;
(4) flaxen fiber of the modified preparation of plant extracts of the present invention, oxygen index (OI) 28.0-28.2%, the oxygen index (OI) after washing 50 times
28.0%, the oxygen index (OI) 27.7-27.9% after washing 100 times.
Specific embodiment
Hereinafter, preferred embodiments of the present invention will be described, it should be understood that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
The flaxen fiber and preparation method thereof of the modified preparation of 1 one Plant Extracts of embodiment
The flaxen fiber and preparation method thereof of the modified preparation of a Plant Extracts of the invention, comprising the following steps:
Step 1, pretreatment
1) degumming: after ten minutes by the former stem soak at room temperature of ramie fiber crops, controlling temperature between 25 DEG C, add 2% composite bacteria agent,
It stirs evenly, is left to ferment 20h, degumming is completed to the destruction of pectin, lignin in fiber etc. using fermentation.
The composite bacteria agent, including Rhodopseudomonas palustris, trichoderma viride, bacillus subtilis, bite pectin Flavobacterium
With black green trichoderma, mass ratio 3:2:15:2:1.
The bacteria containing amount of the Rhodopseudomonas palustris (deposit number CICC 23812) is 10g/L, trichoderma viride (deposit number
CGMCC 3.2942) bacteria containing amount is 0.8g/L, the bacteria containing amount of bacillus subtilis (deposit number ATCC 6633) is 10g/L, bites fruit
The bacteria containing amount of glue Flavobacterium (deposit number CGMCC 1.12362) is 2.5g/L, and black green trichoderma (deposit number BNCC172476) contains bacterium
Amount is 0.4g/L, and the above strain has the synergistic effect of height, forms the stable ecosystem self, can be in non-sterilized day
It quickly bred in right raw material, colonize and occupy advantage, the above strain is all from commercially available.
2) it washes material: above-mentioned degumming flaxen fiber being cleaned and impregnated using washing immersion liquid, cleaning temperature is 66-70 DEG C,
Obtain flaxen fiber;
The washing immersion liquid, is made of following component by weight: 8 parts of anhydrous sodium sulphate, 8 parts of sodium chloride, 2 parts of saleratus power, lemon
5 parts of lemon acid sodium, 0.1 part of bismuth oxide powder, 0.5 part of sodium dithionite, 2.0 parts of heptose sodium sugar, 100 parts of deionized water.
3) high-temperature steam is stifling: carrying out the steaming of first time high temperature to the flaxen fiber that above-mentioned steps obtain using 112 DEG C of high temperature
Vapour suffocating treatment 10min is then placed in water balance room and carries out moisture equilibration 1 hour, then carries out second of high temperature steaming
Vapour suffocating treatment 15min, the temperature of second of high-temperature steam are 110 DEG C, then cooled to room temperature again;
4) dry: above-mentioned flaxen fiber is placed in 40 DEG C of clear water and impregnates 20min, take out, 110 DEG C at a temperature of control water so that
Water content is 5%, obtains flaxen fiber.
Through intermediate sample detection, obtained flaxen fiber, content of lignin is lower than 3.2%, and pectin content is lower than 0.15%.
The preparation of step 2, A treatment fluid
(1) preparation of raw material
The A inorganic agent includes the raw material of following parts by weight:
10 parts of sulfamate-phenol-formaldehyde condensate, 15 parts of polysaccharide, 8 parts of polyoxyethylene tallow amine, 4 parts of dimethylformamide,
2 parts of the talcum powder of 2000 mesh, 2 parts of trichloroacetic acid, 6 parts of hydrogenated castor oil polyoxyethylene ether, 100 parts of distilled water.
The polysaccharide is the mixture of galactomannans, β-Isosorbide-5-Nitrae-poly- D- Glucosamine and astragalus polyose, described
The mass ratio of the poly- D- Glucosamine of galactomannans, β -1,4- and astragalus polyose is 10:1:2;
The galactomannans, purity 98%, 0.5% protein, 0.3% fiber, 0.1% ash content.
The astragalus polyose, density 1.439g/cm3, 154.5 DEG C of fusing point, 406.3 DEG C of 760 mmHg of at of boiling point, flash-point
199.5 DEG C, refractive index 1.638;
The dimethylformamide, No. CAS be 68-12-2, No. EINECS be 200-679-5, -61 DEG C of fusing point, boiling point 153
DEG C, 20 DEG C, 136 °F of flash-point of 0.948 g/mL at of density;
The trichloroacetic acid, 56.0-58.0 DEG C of crystalline temperature, chloride (Cl)≤0.005%, sulfate (SO4)≤0.01%, nitric acid
Salt (NO3)≤0.001%, phosphate (PO4)≤0.001%, ignition residue (in terms of sulfate)≤0.03%, heavy metal (in terms of Pb)
≤ 0.0005%, iron (Fe)≤0.0005%;
The hydrogenated castor oil polyoxyethylene ether, appearance are pale yellow transparent grease (25 DEG C), saponification number 90-100 mg
KOH/g, cloud point (1% aqueous solution)≤30, moisture≤1.00%, pH value (1% aqueous solution) 5.0-7.0, HLB value 9-10.
The A inorganic agent the preparation method comprises the following steps:
By the parts by weight by sulfamate-phenol-formaldehyde condensate, polysaccharide, polyoxyethylene tallow amine, dimethylformamide,
The talcum powder of hydrogenated castor oil polyoxyethylene ether and 2000 mesh is mixed, and is stirred with the speed of 950rad/min, temperature 130
DEG C, the formic acid, trichloroacetic acid and distilled water of the parts by weight is added, stirs, time 9-14min, it is cooling, it crushes, be sieved
To A inorganic agent.
(2) A treatment fluid is prepared
The A treatment fluid the preparation method comprises the following steps:
By the A inorganic agent of 2Kg step (1), according to 1:20 bath raio, 80 DEG C of temperature dissolutions, the glacial acetic acid for being added 0.3% adjusts pH
It is worth, adition process is stirred continuously, and filtering uses and (all dissolves the state that is translucent) after heat preservation 2 hours.
Step 3, flaxen fiber single treatment
Pretreated flaxen fiber is put into A treatment fluid, is mixed, is first warming up to 25 DEG C, keeps the temperature 20 minutes;
Then 95 DEG C are warming up to, heating rate is 3 DEG C/min, after 15min is placed in heat preservation,
The impulse electric field for using frequency to be 1.5kV/cm for 15Hz, electric field strength handles 13s, obtains electric field single treatment object;
Then object processed material of electric field is placed in sealed storage tank, is 1.25 × 10 in intensity under stream of nitrogen gas-2w/
in2Ultraviolet light and 1.75 × 108The gamma-rays of rads irradiates 5.2min, and the flow of nitrogen stream is 25-35ml/min, obtains ultraviolet-γ
Processed material;
The carbonic acid sodium powder of 1.0gD90≤0.75um is added into ultraviolet-γ processed material, mixes, stirs 7min under magnetic stirring apparatus,
Then the impulse electric field for using frequency to be 5.0kV/cm for 18Hz, electric field strength handles 25 s, obtains electric field secondary treatment object;
Continue after keeping placing 3-4min at 95 DEG C of temperature, removes sodium carbonate, take out washing, dry to moisture content < 5%.
Step 4, flaxen fiber secondary treatment
A. plant dyeing agent solution is prepared, it is molten that the vegetable dyeing agent that concentration is 1.2% is made in vegetable dyeing agent addition deionized water
Liquid;
The vegetable dyeing agent, the Herba Menthae powder and Chloranthus glaber powder of the quality such as selection, the Herba Menthae powder, 99.5% crosses 500 mesh
Sieve, appearance: shallow green powder, it is loose, without agglomeration, it is visible by naked eyes impurity, color uniformity;Smell is uniform;Effective component
Content >=98.5%, moisture≤3%, total plate count < 99cfu/g, salmonella and Escherichia coli must not detect, and the shelf-life is
12 months;Effective component: menthol, menthones, menthyl acetate, limonene, isomenthone, peppermint esters, rheum emodin, big
Yellow phenol, robinin etc..
The Chloranthus glaber powder, 99.8% crosses 500 meshes, and appearance: brown ceramic powder, loose no agglomeration are visible by naked eyes miscellaneous
Matter, color uniformity;Smell is uniform;Active constituent content >=98.5%, moisture≤3%, total plate count < 99cfu/g, sramana
Salmonella and Escherichia coli must not detect, and the shelf-life is 12 months, and effective component is isofraxidin, left-handed class myrrh element first, prolongs
Fumarate, succinic acid, glycosides displayed, wherein Determination of isofraxidin 3.5%;
B. it is 2.0% that vegetable dyeing agent, which accounts for the percent mass ratio of flaxen fiber, bath raio 1:10;
C. flaxen fiber above-mentioned steps obtained is placed in vegetable dyeing agent solution bath (addition glacial acetic acid 1.2g/L, additive amount
Depending on water in dye vat), 2 DEG C/min of heating rate is warming up to 90 DEG C, handles time 15-35 minutes;
D. soap: will in treated flaxen fiber is placed in 5g/L soaps liquid, 60 DEG C or so 10 minutes, take out, washing, it is dry
To the flaxen fiber of the modified preparation of plant extracts of the present invention.
The flaxen fiber of the modified preparation of plant extracts of the present invention, meets GB18401-2010 National Textile basic security skill
Art specification can reduce the loss to flaxen fiber strength, and the strength loss of fiber is few after dyeing, color fastness to water, perspiration resistance color jail
Spend (color fastness to water change colour grade be 4-5 grade, staining grade is 4-5 grade, colour fastness to perspiration change colour grade for 4-5 grades, be stained with
Colour gradation is 4-5 grades), colour fastness to rubbing is good (dry friction grade is 4-5 grades), and good hand touch is formaldehydeless, free from extraneous odour, can not divide
Solve the detection of carcinogenic aromatic amine dyestuff, improve the quality of flaxen fiber after dyeing, even dyeing effect is outstanding, level dyeing rate up to 90% or more,
Simple process.
The flaxen fiber and preparation method thereof of the modified preparation of 2 one Plant Extracts of embodiment
The flaxen fiber and preparation method thereof of the modified preparation of a Plant Extracts of the invention, comprising the following steps:
Step 1, pretreatment
1) degumming: after ramie fiber crops former stem soak at room temperature 26 minutes, temperature is controlled between 33 DEG C, adds 3.5% compound bacteria
Agent stirs evenly, and is left to ferment 50h, completes degumming to the destruction of pectin, lignin in fiber etc. using fermentation.
The composite bacteria agent, including Rhodopseudomonas palustris, trichoderma viride, bacillus subtilis, bite pectin Flavobacterium
With black green trichoderma, mass ratio 3:2:15:2:1.
The bacteria containing amount of the Rhodopseudomonas palustris (deposit number CICC 23812) is 10g/L, trichoderma viride (deposit number
CGMCC 3.2942) bacteria containing amount is 0.8g/L, the bacteria containing amount of bacillus subtilis (deposit number ATCC 6633) is 10g/L, bites fruit
The bacteria containing amount of glue Flavobacterium (deposit number CGMCC 1.12362) is 2.5g/L, and black green trichoderma (deposit number BNCC172476) contains bacterium
Amount is 0.4g/L, and the above strain has the synergistic effect of height, forms the stable ecosystem self, can be in non-sterilized day
It quickly bred in right raw material, colonize and occupy advantage, the above strain is all from commercially available.
2) it washes material: above-mentioned degumming flaxen fiber being cleaned and impregnated using washing immersion liquid, cleaning temperature is 66-70 DEG C,
Obtain flaxen fiber;
The washing immersion liquid, is made of following component by weight: 10 parts of anhydrous sodium sulphate, 6 parts of sodium chloride, 2.5 parts of saleratus power,
3.5 parts of sodium citrate, 0.14 part of bismuth oxide powder, 0.42 part of sodium dithionite, 3.6 parts of heptose sodium sugar, deionized water 100
Part.
3) high-temperature steam is stifling: carrying out the steaming of first time high temperature to the flaxen fiber that above-mentioned steps obtain using 124 DEG C of high temperature
Vapour suffocating treatment 10-15min is then placed in water balance room and carries out moisture equilibration 1.3 hours, then carries out second high
Warm steam suffocating treatment 21.5min, the temperature of second of high-temperature steam are 124.5 DEG C, then cooled to room temperature again;
4) dry: above-mentioned flaxen fiber is placed in 40 DEG C of clear water and impregnates 20min, take out, 117 DEG C at a temperature of control water so that
Water content is 6.2%, obtains flaxen fiber.
Through intermediate sample detection, obtained flaxen fiber, content of lignin is lower than 3.2%, and pectin content is lower than 0.15%.
The preparation of step 2, A treatment fluid
(1) preparation of raw material
The A inorganic agent includes the raw material of following parts by weight:
16 parts of sulfamate-phenol-formaldehyde condensate, 14.5 parts of polysaccharide, 11.2 parts of polyoxyethylene tallow amine, dimethylformamide
3.2 parts, 3.5 parts of the talcum powder of 2000 mesh, 1.6 parts of trichloroacetic acid, 7 parts of hydrogenated castor oil polyoxyethylene ether, 95 parts of distilled water.
The polysaccharide is the mixture of galactomannans, β-Isosorbide-5-Nitrae-poly- D- Glucosamine and astragalus polyose, described
The mass ratio of the poly- D- Glucosamine of galactomannans, β -1,4- and astragalus polyose is 10:1:2;
The galactomannans, purity 98%, 0.8% protein, 0.28% fiber, 0.1% ash content.
The astragalus polyose, density 1.439g/cm3, 154.5 DEG C of fusing point, 406.3 DEG C of 760 mmHg of at of boiling point, flash-point
199.5 DEG C, refractive index 1.638;
The dimethylformamide, No. CAS be 68-12-2, No. EINECS be 200-679-5, -61 DEG C of fusing point, boiling point 153
DEG C, 20 DEG C, 136 °F of flash-point of 0.948 g/mL at of density;
The trichloroacetic acid, 56.0-58.0 DEG C of crystalline temperature, chloride (Cl)≤0.005%, sulfate (SO4)≤0.01%, nitric acid
Salt (NO3)≤0.001%, phosphate (PO4)≤0.001%, ignition residue (in terms of sulfate)≤0.03%, heavy metal (in terms of Pb)
≤ 0.0005%, iron (Fe)≤0.0005%;
The hydrogenated castor oil polyoxyethylene ether, appearance are pale yellow transparent grease (25 DEG C), saponification number 90-100 mg
KOH/g, cloud point (1% aqueous solution)≤30, moisture≤1.00%, pH value (1% aqueous solution) 5.0-7.0, HLB value 9-10.
The A inorganic agent the preparation method comprises the following steps:
By the parts by weight by sulfamate-phenol-formaldehyde condensate, polysaccharide, polyoxyethylene tallow amine, dimethylformamide,
The talcum powder of hydrogenated castor oil polyoxyethylene ether and 2000 mesh is mixed, and is stirred with the speed of 950rad/min, temperature 130
DEG C, the formic acid, trichloroacetic acid and distilled water of the parts by weight is added, stirs, time 9-14min, it is cooling, it crushes, be sieved
To A inorganic agent.
(2) A treatment fluid is prepared
The A treatment fluid the preparation method comprises the following steps:
By the A inorganic agent of 2Kg step (1), according to 1:20 bath raio, 0.85% glacial acetic acid adjusting is added in 83.5 DEG C of temperature dissolutions
PH value, adition process are stirred continuously, and filtering uses and (all dissolves the state that is translucent) after heat preservation 2 hours.
Step 3, flaxen fiber single treatment
Pretreated flaxen fiber is put into A treatment fluid, is mixed, is first warming up to 25 DEG C, keeps the temperature 20 minutes;
Then 95 DEG C are warming up to, heating rate is 4 DEG C/min, after 15min is placed in heat preservation,
The impulse electric field for using frequency to be 1.5kV/cm for 15Hz, electric field strength handles 17s, obtains electric field single treatment object;
Then object processed material of electric field is placed in sealed storage tank, is 1.25 × 10 in intensity under stream of nitrogen gas-2w/
in2Ultraviolet light and 1.75 × 108The gamma-rays of rads irradiates 7.5min, and the flow of nitrogen stream is 31ml/min, obtains the ultraviolet place-γ
Manage object;
The carbonic acid sodium powder of 1.6gD90≤0.75um is added into ultraviolet-γ processed material, mixes, is stirred under magnetic stirring apparatus
11min, the impulse electric field for then using frequency to be 5.0kV/cm for 18Hz, electric field strength handle 31s, obtain electric field secondary treatment
Object;
Continue after keeping placing 3-4min at 95 DEG C of temperature, removes sodium carbonate, take out washing, dry to moisture content < 5%.
Step 4, flaxen fiber secondary treatment
A. plant dyeing agent solution is prepared, it is molten that the vegetable dyeing agent that concentration is 4.5% is made in vegetable dyeing agent addition deionized water
Liquid;
The vegetable dyeing agent, the Herba Menthae powder and Chloranthus glaber powder of the quality such as selection, the Herba Menthae powder, 99.5% crosses 500 mesh
Sieve, appearance: shallow green powder, it is loose, without agglomeration, it is visible by naked eyes impurity, color uniformity;Smell is uniform;Effective component
Content >=98.5%, moisture≤3%, total plate count < 99cfu/g, salmonella and Escherichia coli must not detect, and the shelf-life is
12 months;Effective component: menthol, menthones, menthyl acetate, limonene, isomenthone, peppermint esters, rheum emodin, big
Yellow phenol, robinin etc..
The Chloranthus glaber powder, 99.8% crosses 500 meshes, and appearance: brown ceramic powder, loose no agglomeration are visible by naked eyes miscellaneous
Matter, color uniformity;Smell is uniform;Active constituent content >=98.5%, moisture≤3%, total plate count < 99cfu/g, sramana
Salmonella and Escherichia coli must not detect, and the shelf-life is 12 months, and effective component is isofraxidin, left-handed class myrrh element first, prolongs
Fumarate, succinic acid, glycosides displayed, wherein Determination of isofraxidin 5.0%;
B. it is 4.25% that vegetable dyeing agent, which accounts for the percent mass ratio of flaxen fiber, bath raio 1:10;
C. flaxen fiber above-mentioned steps obtained is placed in vegetable dyeing agent solution bath (addition glacial acetic acid 1.2g/L, additive amount
Depending on water in dye vat), 3.3 DEG C/min of heating rate is warming up to 90 DEG C, handles time 15-35 minutes;
D. soap: will in treated flaxen fiber is placed in 5g/L soaps liquid, 60 DEG C or so 10-15 minute, take out, washing is dry
Obtain the flaxen fiber of the modified preparation of plant extracts of the present invention.
The flaxen fiber of the modified preparation of plant extracts of the present invention, meets GB18401-2010 National Textile basic security skill
Art specification can reduce the loss to flaxen fiber strength, and the strength loss of fiber is few after dyeing, color fastness to water, perspiration resistance color jail
Spend (color fastness to water change colour grade be 4-5 grade, staining grade is 4-5 grade, colour fastness to perspiration change colour grade for 4-5 grades, be stained with
Colour gradation is 4-5 grades), colour fastness to rubbing is good (dry friction grade is 4-5 grades), and good hand touch is formaldehydeless, free from extraneous odour, can not divide
Solve the detection of carcinogenic aromatic amine dyestuff, improve the quality of flaxen fiber after dyeing, even dyeing effect is outstanding, level dyeing rate up to 90% or more,
Simple process.
The flaxen fiber and preparation method thereof of the modified preparation of 3 one Plant Extracts of embodiment
The flaxen fiber and preparation method thereof of the modified preparation of a Plant Extracts of the invention, comprising the following steps:
Step 1, pretreatment
1) degumming: after ramie fiber crops former stem soak at room temperature 30 minutes, controlling temperature between 50 DEG C, add 5% composite bacteria agent,
It stirs evenly, is left to ferment 100h, degumming is completed to the destruction of pectin, lignin in fiber etc. using fermentation.
The composite bacteria agent, including Rhodopseudomonas palustris, trichoderma viride, bacillus subtilis, bite pectin Flavobacterium
With black green trichoderma, mass ratio 3:2:15:2:1.
The bacteria containing amount of the Rhodopseudomonas palustris (deposit number CICC 23812) is 10g/L, trichoderma viride (deposit number
CGMCC 3.2942) bacteria containing amount is 0.8g/L, the bacteria containing amount of bacillus subtilis (deposit number ATCC 6633) is 10g/L, bites fruit
The bacteria containing amount of glue Flavobacterium (deposit number CGMCC 1.12362) is 2.5g/L, and black green trichoderma (deposit number BNCC172476) contains bacterium
Amount is 0.4g/L, and the above strain has the synergistic effect of height, forms the stable ecosystem self, can be in non-sterilized day
It quickly bred in right raw material, colonize and occupy advantage, the above strain is all from commercially available.
2) it washes material: above-mentioned degumming flaxen fiber being cleaned and impregnated using washing immersion liquid, cleaning temperature is 66-70 DEG C,
Obtain flaxen fiber;
The washing immersion liquid, is made of following component by weight: 12 parts of anhydrous sodium sulphate, 8 parts of sodium chloride, 5 parts of saleratus power, lemon
5 parts of lemon acid sodium, 0.2 part of bismuth oxide powder, 0.5 part of sodium dithionite, 5.5 parts of heptose sodium sugar, 100 parts of deionized water.
3) high-temperature steam is stifling: carrying out the steaming of first time high temperature to the flaxen fiber that above-mentioned steps obtain using 130 DEG C of high temperature
Vapour suffocating treatment 15min is then placed in water balance room and carries out moisture equilibration 2 hours, then carries out second of high temperature steaming
Vapour suffocating treatment 25min, the temperature of second of high-temperature steam are 125 DEG C, then cooled to room temperature again;
4) dry: above-mentioned flaxen fiber is placed in 40 DEG C of clear water and impregnates 20min, take out, 118 DEG C at a temperature of control water so that
Water content is 8%, obtains flaxen fiber.
Through intermediate sample detection, obtained flaxen fiber, content of lignin is lower than 3.2%, and pectin content is lower than 0.15%.
The preparation of step 2, A treatment fluid
(1) preparation of raw material
The A inorganic agent includes the raw material of following parts by weight:
20 parts of sulfamate-phenol-formaldehyde condensate, 10 parts of polysaccharide, 15 parts of polyoxyethylene tallow amine, 1 part of dimethylformamide,
5 parts of the talcum powder of 2000 mesh, 0.8 part of trichloroacetic acid, 10 parts of hydrogenated castor oil polyoxyethylene ether, 65 parts of distilled water.
The polysaccharide is the mixture of galactomannans, β-Isosorbide-5-Nitrae-poly- D- Glucosamine and astragalus polyose, described
The mass ratio of the poly- D- Glucosamine of galactomannans, β -1,4- and astragalus polyose is 10:1:2;
The galactomannans, purity 98%, 1% protein, 0.3% fiber, 0.1% ash content.
The astragalus polyose, density 1.439g/cm3, 154.5 DEG C of fusing point, 406.3 DEG C of 760 mmHg of at of boiling point, flash-point
199.5 DEG C, refractive index 1.638;
The dimethylformamide, No. CAS be 68-12-2, No. EINECS be 200-679-5, -61 DEG C of fusing point, boiling point 153
DEG C, 20 DEG C, 136 °F of flash-point of 0.948 g/mL at of density;
The trichloroacetic acid, 56.0-58.0 DEG C of crystalline temperature, chloride (Cl)≤0.005%, sulfate (SO4)≤0.01%, nitric acid
Salt (NO3)≤0.001%, phosphate (PO4)≤0.001%, ignition residue (in terms of sulfate)≤0.03%, heavy metal (in terms of Pb)
≤ 0.0005%, iron (Fe)≤0.0005%;
The hydrogenated castor oil polyoxyethylene ether, appearance are pale yellow transparent grease (25 DEG C), saponification number 90-100 mg
KOH/g, cloud point (1% aqueous solution)≤30, moisture≤1.00%, pH value (1% aqueous solution) 5.0-7.0, HLB value 9-10.
The A inorganic agent the preparation method comprises the following steps:
By the parts by weight by sulfamate-phenol-formaldehyde condensate, polysaccharide, polyoxyethylene tallow amine, dimethylformamide,
The talcum powder of hydrogenated castor oil polyoxyethylene ether and 2000 mesh is mixed, and is stirred with the speed of 950rad/min, temperature 130
DEG C, the formic acid, trichloroacetic acid and distilled water of the parts by weight is added, stirs, time 9-14min, it is cooling, it crushes, be sieved
To A inorganic agent.
(2) A treatment fluid is prepared
The A treatment fluid the preparation method comprises the following steps:
By the A inorganic agent of 2Kg step (1), according to 1:20 bath raio, 90 DEG C of temperature dissolutions, the glacial acetic acid for being added 1.1% adjusts pH
It is worth, adition process is stirred continuously, and filtering uses and (all dissolves the state that is translucent) after heat preservation 2 hours.
Step 3, flaxen fiber single treatment
Pretreated flaxen fiber is put into A treatment fluid, is mixed, is first warming up to 25 DEG C, keeps the temperature 20 minutes;
Then 95 DEG C are warming up to, heating rate is 5 DEG C/min, after 15min is placed in heat preservation,
The impulse electric field for using frequency to be 1.5kV/cm for 15Hz, electric field strength handles 13-20s, obtains electric field single treatment object;
Then object processed material of electric field is placed in sealed storage tank, is 1.25 × 10 in intensity under stream of nitrogen gas-2w/
in2Ultraviolet light and 1.75 × 108The gamma-rays of rads irradiates 10min, and the flow of nitrogen stream is 35ml/min, obtains ultraviolet-γ processing
Object;
The carbonic acid sodium powder of 2.0gD90≤0.75um is added into ultraviolet-γ processed material, mixes, is stirred under magnetic stirring apparatus
17min, the impulse electric field for then using frequency to be 5.0kV/cm for 18Hz, electric field strength handle 35 s, obtain electric field secondary treatment
Object;
Continue after keeping placing 3-4min at 95 DEG C of temperature, removes sodium carbonate, take out washing, dry to moisture content < 5%.
Step 4, flaxen fiber secondary treatment
A. plant dyeing agent solution is prepared, it is molten that the vegetable dyeing agent that concentration is 5% is made in vegetable dyeing agent addition deionized water
Liquid;
The vegetable dyeing agent, the Herba Menthae powder and Chloranthus glaber powder of the quality such as selection, the Herba Menthae powder, 99.5% crosses 500 mesh
Sieve, appearance: shallow green powder, it is loose, without agglomeration, it is visible by naked eyes impurity, color uniformity;Smell is uniform;Effective component
Content >=98.5%, moisture≤3%, total plate count < 99cfu/g, salmonella and Escherichia coli must not detect, and the shelf-life is
12 months;Effective component: menthol, menthones, menthyl acetate, limonene, isomenthone, peppermint esters, rheum emodin, big
Yellow phenol, robinin etc..
The Chloranthus glaber powder, 99.8% crosses 500 meshes, and appearance: brown ceramic powder, loose no agglomeration are visible by naked eyes miscellaneous
Matter, color uniformity;Smell is uniform;Active constituent content >=98.5%, moisture≤3%, total plate count < 99cfu/g, sramana
Salmonella and Escherichia coli must not detect, and the shelf-life is 12 months, and effective component is isofraxidin, left-handed class myrrh element first, prolongs
Fumarate, succinic acid, glycosides displayed, wherein Determination of isofraxidin 8.0%;
B. it is 20% that vegetable dyeing agent, which accounts for the percent mass ratio of flaxen fiber, bath raio 1:10;
C. flaxen fiber above-mentioned steps obtained is placed in vegetable dyeing agent solution bath (addition glacial acetic acid 1.2g/L, additive amount
Depending on water in dye vat), 5 DEG C/min of heating rate is warming up to 90 DEG C, handles time 15-35 minutes;
D. soap: will in treated flaxen fiber is placed in 5g/L soaps liquid, 60 DEG C or so 15 minutes, take out, washing, it is dry
To the flaxen fiber of the modified preparation of plant extracts of the present invention.
The flaxen fiber of the modified preparation of plant extracts of the present invention, meets GB18401-2010 National Textile basic security skill
Art specification can reduce the loss to flaxen fiber strength, and the strength loss of fiber is few after dyeing, color fastness to water, perspiration resistance color jail
Spend (color fastness to water change colour grade be 4-5 grade, staining grade is 4-5 grade, colour fastness to perspiration change colour grade for 4-5 grades, be stained with
Colour gradation is 4-5 grades), colour fastness to rubbing is good (dry friction grade is 4-5 grades), and good hand touch is formaldehydeless, free from extraneous odour, can not divide
Solve the detection of carcinogenic aromatic amine dyestuff, improve the quality of flaxen fiber after dyeing, even dyeing effect is outstanding, level dyeing rate up to 90% or more,
Simple process.
1, it is detected by the flaxen fiber that the preparation method described in embodiment 1-3 obtains, wherein the inspection of main indicator
Survey the results are shown in Table 1:
Table 1:
2, antibiotic property test has also been carried out to the flaxen fiber of 1-3 of embodiment of the present invention preparation, test method uses GBT20944.3-
2008 antibacterial textile performance evaluation third portions: succusion to staphylococcus aureus, to Candida albicans and Escherichia coli
Fungistatic effect test, the results are shown in Table 2;
Table 2
Remarks: chlorine-resistant floats the measurement of color fastness using the method in standard GBT-7069-1997.
3, anti-flammability test has also been carried out to the flaxen fiber of 1-3 of embodiment of the present invention preparation, flame retardant effect is as shown in the table.
From above table:
(1) flaxen fiber of the modified preparation of plant extracts of the present invention, breaking strength 8.8-9.4cN/dtex, content of formaldehyde 0mg/
Kg, elastic recovery rate 62.4-66.9%, dyeing fleck rate are 0-0.005%;
(2) flaxen fiber of the modified preparation of plant extracts of the present invention, to staphylococcus aureus, Candida albicans, Escherichia coli
Bacteriostasis rate be respectively 91.5-92.6%, 96.3-96.4%, 97.7-99.0%;After washing 50 times, to staphylococcus aureus, white
Color candida albicans, Escherichia coli bacteriostasis rate be respectively 88.5-89.0%, 90.5-91.1%, 88.8-88.9%;
(3) flaxen fiber of the modified preparation of plant extracts of the present invention, it is 0.02-0.04%, chlorine rinsing that chlorine-resistant, which floats color fastness reduced rate,
Oxygen index (OI) (effective chlorine density 1.2g/l) 28.0-28.2% after 50 times;
(4) flaxen fiber of the modified preparation of plant extracts of the present invention, oxygen index (OI) 28.0-28.2%, the oxygen index (OI) after washing 50 times
28.0%, the oxygen index (OI) 27.7-27.9% after washing 100 times.
Unless otherwise indicated, percentage employed in the present invention is mass percent, and the ratio is quality
Ratio.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.