CN107012698A - Natural fibre products and method of modifying that a kind of utilization super critical CO 2 technology is modified - Google Patents
Natural fibre products and method of modifying that a kind of utilization super critical CO 2 technology is modified Download PDFInfo
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- CN107012698A CN107012698A CN201710213544.XA CN201710213544A CN107012698A CN 107012698 A CN107012698 A CN 107012698A CN 201710213544 A CN201710213544 A CN 201710213544A CN 107012698 A CN107012698 A CN 107012698A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/94—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using dyes dissolved in solvents which are in the supercritical state
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B9/00—Solvent-treatment of textile materials
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/34—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using natural dyestuffs
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/02—Material containing basic nitrogen
- D06P3/04—Material containing basic nitrogen containing amide groups
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/02—Material containing basic nitrogen
- D06P3/04—Material containing basic nitrogen containing amide groups
- D06P3/14—Wool
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/02—After-treatment
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Abstract
The present invention provides the natural fibre products that a kind of utilization super critical CO 2 technology is modified, and modified natural fibre products are cotton, fiber crops, silk, hair natural fiber or yarn, fabric or the ready-made clothes being made using the natural fiber.The present invention also provides a kind of method of utilization super critical CO 2 technology modified natural fibers product, and methods described includes the addition step of natural fiber and vegetable colour and natural plant extracts；Innovation is modified using super critical CO 2 technology to natural fiber, solvent is used as without water or other reagents, the generation and discharge of waste water and waste are not had, with ecological, environmental protective and the features such as fabric variety wide adaptability, belong to the function modified technique of environment-friendly type；It is splendid using natural fiber uniform color, reappearance of the super critical CO 2 technology progress of the present invention after function modified, natural fibre will not be damaged.
Description
Technical field
The present invention relates to the method for modifying of natural fiber, particularly a kind of utilization super critical CO 2 technology is modified
Natural fibre products and method of modifying.
Background technology
Natural fiber be that nature is original or plant through cultivation on, directly obtain on the animal of artificial feeding
Textile fabric, is the important materials source of textile industry.Although synthetic fibers yield is increased rapidly since 20 middle of century,
Natural fiber still accounts for 50% in textile fabric gross annual output amount.Therefore, currently, natural fiber is still that textile industry is main
Raw material.
The natural fiber that nature is present mainly has：Cotton, crudefiber crop, silk and animal wool.Wherein the molecule of cotton and crudefiber crop into
Part is mainly cellulose, and the molecular constituents of silk and hairs are mainly protein (being in the presence of polyamide macromolecular form).
The traditional dyeing of natural fiber and it is function modified be hygrometric state chemical reaction process, during which need to consume a large amount of
Water resource and chemicals, and a large amount of high concentrations, high COD coloured, odorous or even poisonous waste water are produced, to its week
Side waters and ecological environment cause serious pollution.
At present, supercritical CO 2 dyeing technology has obtained stage as a kind of new green dyeing-finishing technology and entered
Exhibition, the joint exploratory development to its process conditions, dyeing mechanism and dyeing installation is more ripe.But because dyeing needs pass through
Special dyeing installation realizes that disposable input cost is higher.In addition, because existing equipment is all single formula device,
Cause the problem of energy consumption high efficiency is low.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides the natural fiber that a kind of utilization super critical CO 2 technology is modified
Product and method of modifying, to solve technical problem：
1st, natural fiber is modified using the super critical CO 2 technology of the present invention, without water or other reagents as molten
Agent, the generation and discharge of waste water and waste are not had, belong to the function modified technique of environment-friendly type；
2nd, it is function modified to natural fiber progress using the super critical CO 2 technology of the present invention, technological process is shortened, is saved
The expense of Final finishing has been saved, cost is reduced；
3rd, function modified speed is carried out to natural fiber soon using the super critical CO 2 technology of the present invention, efficiency high；
4th, after being modified using the super critical CO 2 technology of the present invention to natural fiber, modified natural fiber color and luster
Uniformly, reappearance is splendid, and natural fibre will not have been damaged；
5th, the feed carbon dioxide and vegetable colour and natural plant extracts used in process of the present invention, after use can be complete
Complete reclaim uses, and reduces production cost, reduces pollution, with good social benefit, can largely be pushed away in textile industry
It is wide to use；
6th, the textile products such as the fabric, ready-made clothes, home textile of making are modified using the super critical CO 2 technology of the present invention not
By bleaching, the residual without other chemical reagent is safer；
8th, the modified natural fibre products of the present invention have good physical property；
9th, the modified natural fibre products of the present invention have outstanding antibacterial, bacteriostasis property.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is：
One kind utilizes super critical CO 2 technology modified natural fibers method, comprises the following steps：
1st, the addition of natural fiber and vegetable colour and natural plant extracts
Load 200-220 kilograms of natural fiber in function modified kettle, 0.5-2kg rhodizonate dyes and 1- are loaded in mixing kettle
3kg mint extracts；
Described natural fiber is cotton, fiber crops, silk or hair；
Described natural plant extracts kind is the one or more of mint extract, wormwood extract, Herba Pileae Scriptae extract；
Described vegetable colour is the one or more in rhodizonate dye, violet dyes, safflower, purple perilla dyestuff；
The rhodizonate dye, comes from the production of Henan De Yu Chemical Co., Ltd.s, color code：#E71B64；
The mint extract, is produced, moisture 2.5-3% by Shaanxi Sen Fu natural products Co., Ltd, and content of ashes is
0.3-0.5%, content of beary metal≤3ppm, mesh number is 200-240 mesh, saccharomycete and mould bacterial content ＜ 20cfu/g；
Described natural plant extracts and vegetable colour are commercially available.
2nd, prepared by supercritical carbon dioxide
Then the liquid carbon dioxide being stored in liquid carbon dioxide storage tank is injected into CO 2 high pressure pump by pipeline
In；In high-pressure pump, its temperature is heated to 90-120 DEG C and obtained by carbon dioxide pressurization to 30-32MPa, then process preheater
Supercritical carbon dioxide.
3rd, the dissolving of vegetable colour and natural plant extracts compound
Supercritical carbon dioxide fluid made from step 2 is injected into mixing kettle from preheater, pressure 30- is kept in tank
32MPa, 90-120 DEG C of temperature is fully contacted and dissolved with vegetable colour and natural plant extracts compound, disperses equal
It is even；
4th, function modified process
By function modified kettle carry out heating pressurization, standby function be modified kettle in temperature reach 90-120 DEG C, pressure reach 30MPa
When, the supercritical carbon dioxide in mixing kettle is injected into recycle stream in the function modified kettle equipped with natural fiber to be modified
It is dynamic, it is sufficiently mixed, function modified 120-180 min；
5th, last handling process
It is modified after terminating, supercritical carbon dioxide is separated through separator with vegetable colour and natural plant extracts, now,
The temperature of separator is 80-100 DEG C, pressure 2-3MPa, and gaseous carbon dioxide enters in condensation kettle, vegetable colour and natural plants
Extract is then stayed in separating still；The temperature for condensing kettle is 20-25 DEG C（Room temperature）, pressure 4-6MPa, gaseous carbon dioxide transformation
For liquid carbon dioxide, it is then refluxed for entering in liquid CO 2 storage tank, participates in modified technique next time, recycles；
Opening function is modified kettle, and the natural fibers such as modified cotton, fiber crops, silk or hair are taken out；
By adopting the above-described technical solution, the present invention reach have the technical effect that：
1st, innovation is modified using super critical CO 2 technology to natural fiber, without water or other reagents as solvent,
The generation and discharge of waste water and waste are not had, the huge cost of processing solid, liquid discarded object is saved, with ecological, environmental protective and knitting
The features such as article kind wide adaptability, belong to the function modified technique of environment-friendly type；
2nd, after carrying out function modified end to natural fiber using super critical CO 2 technology, pressure reduction, carbon dioxide
Rapid gasification, thus the natural fiber after function modified need not be dried, technological process is both shortened, save again after
The expense of arrangement；
3rd, it is fast using the super critical CO 2 technology speed function modified to natural fiber progress；
4th, natural fiber uniform color, the reappearance using super critical CO 2 technology progress after function modified are splendid, will not
Natural fibre has been damaged；
5th, carbon dioxide is nontoxic in itself, tasteless, non-ignitable, recyclable, reuses；
6th, vegetable colour or the repeatable utilization of natural plant extracts, need not add any dispersant, stabilizer and ease up when modified
The auxiliary agents such as electuary, reduce production cost, reduce pollution, many advantages, such as with energy-saving and emission-reduction, can be big in textile industry
Amount is promoted the use.
7th, the textile product such as fabric, ready-made clothes, home textile made is without bleaching, the residual without other chemical reagent, more
Safety.
8th, the modified natural fibre products of the present invention have good physical property；The wet of modified natural cotton fiber breaks
Resistance to spalling is 2.87-3.5 cN/dtex；The wet breaking strength of modified natural silk fibers is 30.2-32.2cN/dtex；Change
Property after natural wool fibre wet breaking strength be 1.91-2.61cN/dtex；
9th, the modified natural fibre products of the present invention have outstanding antibacterial, bacteriostasis property；Modified natural cotton fiber is to big
The bacteriostasis rate of enterobacteria is 93-95%；Bacteriostasis rate to staphylococcus aureus is 91-95%；To the bacteriostasis rate of Candida albicans
For 87-89%；Modified natural silk fibers are 90-98%, the bacteriostasis rate of staphylococcus aureus to the bacteriostasis rate of Escherichia coli
For 92-96%, the bacteriostasis rate to Candida albicans is 87-88%；Modified natural wool fibre is to the bacteriostasis rate of Escherichia coli
93-97%, the bacteriostasis rate to staphylococcus aureus is 93-95%, and the bacteriostasis rate to Candida albicans is 87-96%.
Brief description of the drawings
Fig. 1 is the structural representation of present system.
Embodiment
A kind of method of utilization super critical CO 2 technology modified natural fibers of embodiment 1, comprises the following steps：
1st, the addition of natural fiber and vegetable colour and natural plant extracts
Load 200 kilograms of cotton natural fiber in function modified kettle, load 2kg rhodizonate dyes in mixing kettle and 1kg peppermints carry
Take thing；
Described natural plant extracts and vegetable colour can bought on the market；
The rhodizonate dye, comes from the production of Henan De Yu Chemical Co., Ltd.s, color code：#E71B64；
The mint extract, is produced, moisture 2.5-3% by Shaanxi Sen Fu natural products Co., Ltd, and content of ashes is
0.3-0.5%, content of beary metal≤3ppm, mesh number is 200-240 mesh, saccharomycete and mould bacterial content ＜ 20cfu/g.
2nd, prepared by supercritical carbon dioxide
Then the liquid carbon dioxide being stored in liquid carbon dioxide storage tank is injected into CO 2 high pressure pump by pipeline
In；In high-pressure pump, its temperature is heated to 120 DEG C and obtains overcritical by carbon dioxide pressurization to 30MPa, then process preheater
Carbon dioxide；
3rd, the dissolving of vegetable colour and natural plant extracts compound
Supercritical carbon dioxide fluid made from step 2 is injected into mixing kettle from preheater, keeping temperature in mixing kettle
120 DEG C, pressure 30MPa, fully contact and are dissolved with vegetable colour and natural plant extracts compound, are uniformly dispersed；
4th, function modified process
Function modified kettle is subjected to heating pressurization, the temperature that standby function is modified in kettle reaches 120 DEG C, pressure is when reaching 30MPa, will
The supercritical carbon dioxide of mixing kettle is injected into the function modified kettle equipped with cotton to be modified, fiber crops, silk or hair natural fiber and followed
Circulation is moved, and is sufficiently mixed, function modified 120 min；
5th, last handling process
It is modified after terminating, supercritical carbon dioxide is separated through separator with vegetable colour and natural plant extracts, now,
The temperature of separator is 100 DEG C, pressure 2MPa, and gaseous carbon dioxide enters in condensation kettle, vegetable colour and extracted form natural plant
Thing is then stayed in separating still；The temperature for condensing kettle is 20 or so（Room temperature）, pressure 4MPa, gaseous carbon dioxide is changed into liquid two
Carbonoxide, is then refluxed for entering in liquid CO 2 storage tank, participates in modified technique next time, recycles；Opening function
Modified kettle, the natural fibers such as modified cotton, fiber crops, silk or hair are taken out；
In order to which the technique further to embodiment 1 is optimized, tests below is carried out：
Following table is that cotton natural fiber is modified using rhodizonate dye and mint extract, obtained natural fiber it is antibacterial
Rate, table 1 gives influence of the function modified time to specific antibiotic property rate：
In following examples, the natural fiber and raw material of the selected same title used, without before modified, except clearly mark differs
Outside causing, its physical index is all consistent.
Influence of the function modified time of table 1 to anti-microbial property
As can be seen from Table 1, with the extension of function modified time, it is function modified after natural fiber to Escherichia coli, golden yellow
The biocidal property of color staphylococcus and Candida albicans has strengthened, after 120 min, and its fungistatic effect increase is not obvious；
Therefore, time optimal function modified in the present invention is 120 mim；
As can be seen from the above table, cotton natural fiber is modified using rhodizonate dye and mint extract, made after 120 minutes
The cotton natural fiber obtained is 93-94% to the bacteriostasis rate of Escherichia coli；Bacteriostasis rate to staphylococcus aureus is 94-95%；It is right
The bacteriostasis rate of Candida albicans is 87-89%.
And by the use of super critical CO 2 technology without water or other reagents as solvent, waste water and waste are not had
Produce with discharging, more environmentally friendly, safer, technique is simpler.
The performance test that the mint extract of embodiment 3 and rhodizonate dye are modified to natural fiber
The physical indexs such as the unmodified preceding respective fiber number of cotton, silk, hair, fracture strength are consistent.
In following examples in addition to the species of natural fiber is different, other process conditions and embodiment 1 are all.
The performance test results after the mint extract modified natural fibers listed in table 1.
Experimental group is the functional fibre prepared using super critical CO 2 technology, and control group is to be prepared with water as solvent
Functional fibre.
The experimental group of table 2 and control group quality index
It can be seen from upper table 2 3-5 of the embodiment of the present invention be utilized respectively super critical CO 2 technology preparation contain peppermint
Extract（Content is account for fiber quality 1%）Cotton, silk, hair natural fiber and use water as solvent preparation contain peppermint
The cotton of extract, silk, hair natural fiber, under conditions of preparation technology is differed, preparation contains the natural of mint extract
It is essentially the same that the mechanical index of fiber does fracture strength, wet breaking strength, dry elongation at break etc.；To Escherichia coli, to golden yellow
Color staphylococcus, the bacteriostasis rate to Candida albicans are also more or less the same；
Meanwhile, as can be seen from Table 2, natural silk fibers are modified using rhodizonate dye and mint extract, at 120 minutes
It is 28.7cN/dtex that obtained natural silk fibers, which do fracture strength, afterwards；Wet breaking strength is 32.2 cN/dtex；Dry extension at break
Rate is 35%；Bacteriostasis rate to Escherichia coli is 98%；Bacteriostasis rate to staphylococcus aureus is 96%；To Candida albicans
Bacteriostasis rate is 97%.
Natural wool fibre is modified using rhodizonate dye and mint extract, modified natural wool fibre, does disconnected
Resistance to spalling is 2.83cN/dtex, and wet breaking strength is 2.61cN/dtex；Bacteriostasis rate to Escherichia coli is 97%；To golden yellow
Staphylococcic bacteriostasis rate is 95%；Bacteriostasis rate to Candida albicans is 96%.
In addition to above performance detection, due to also having the chemical composition of cool feeling in peppermint containing menthones, menthol etc.；
Because fiber has been made into fabric by us, and the detection of moment cool feeling, instantaneous touch cool feeling are carried out to it（Q-max）：Simulation
During human contact's fabric, the maximum of skin surface moment heat losses is also that fabric moment maximum type of thermal communication is excessive, unit with
Heat maxima every square centimeter is represented.Fabric moment cool feeling heat flow（W/cm2）≥0.140.This test sample be 20 ×
20 square centimeters（Measured area is 5 × 5 square centimeters）, must be by sample to be tested as 20 ± 2 DEG C of environment temperature, humidity 65
± 2% time placement 24 hours, can continue test.Instrument is fuel factor analyzer（KES-F7 THERMOⅡ）
Result of the test：Result of the test is the average value of 5 test datas.
Test report valid data are three after decimal point.
Its testing result is 0.390W/cm2, far above examination criteria（0.14 W/cm2）；And in overcritical titanium dioxide
The soaping fastness that the fiber of rhodizonate dye dyeing is carried out in carbon is 3 grades of the soaping fastness of 5 grades of fibers for being better than water-bath dyeing.
The embodiment shows to carry out function modified prepare containing natural to cotton, hair, silk using super critical CO 2 technology
The natural fiber of plant extracts and vegetable colour is feasible；And using super critical CO 2 technology without water or
Other reagents do not have the generation and discharge of waste water and waste as solvent, and more environmentally friendly, safer, technique is simpler.
The natural fiber containing peppermint prepared using the technology of the present invention is spinned, is made into fabric, and then makes weaving
Product；Testing result shows：When the content of mint fibers reaches 30%, and common viscose fiber content is 70%, its is corresponding
Performance indications are that can reach These parameters.
The performance test that the wormwood extract of embodiment 6 and violet dyes are modified to natural fiber
The physical index such as its respective fiber number, fracture strength is consistent before modification for cotton, fiber crops, silk, hair.
In following examples in addition to the species of natural fiber is different, other process conditions and embodiment 1 are all.
The wormwood extract listed in table 3, the violet dyes performance modified to cotton, fiber crops, silk, hair natural fiber respectively
Test result.Experimental group is that control group is as solvent with water using super critical CO 2 technology modified natural fiber
The fiber of preparation.
The experimental group of table 3 and control group quality index
It can be seen from upper table 3 7-10 of the embodiment of the present invention be utilized respectively super critical CO 2 technology preparation containing Chinese mugwort
The cotton of careless extract, silk, hair natural fiber contain peppermint with our company before by the use of water or other reagents as prepared by solvent
The cotton of extract, silk, hair natural fiber, under conditions of preparation technology is differed, preparation contains the natural of wormwood extract
It is essentially the same that the mechanical index of fiber does fracture strength, wet breaking strength, dry elongation at break etc.；
Also it is more or less the same to Escherichia coli, to staphylococcus aureus, to the bacteriostasis rate of Candida albicans；And overcritical two
The soaping fastness for entering modified fiber in carbonoxide is 5 grades, 3 grades of the soaping fastness of the fiber of water-bath dyeing.Show to face using super
Boundary's CO 2 technology carries out function modified natural fibre of the preparation containing natural plant extracts and vegetable colour to cotton, hair, silk
Dimension is feasible；And by the use of super critical CO 2 technology without water or other reagents as solvent, do not have waste water and
The generation and discharge of waste, more environmentally friendly, safer, technique are simpler.
Modified natural fiber manufactured in the present embodiment is spinned, is made into fabric, and then makes textile product, detection
As a result show：When the content of natural modified fiber manufactured in the present embodiment reaches 30%, and remaining fiber is Modal fibre,
Its corresponding performance indications is that can reach These parameters.
The performance test that the Herba Lysimachiae foenumgraeci extract of embodiment 11 and safflower are modified to natural fiber
The physical index such as its respective fiber number, fracture strength is consistent before modification for cotton, fiber crops, silk, hair.In following examples except
The species of natural fiber is different outer, and other process conditions and embodiment 1 are all.
The performance test results after the Herba Lysimachiae foenumgraeci extract listed in table 4, safflower modified natural fibers.Experimental group is
The modified function fiber prepared using super critical CO 2 technology, control group is the functional fibre prepared with water as solvent.
The experimental group of table 4 and control group quality index
It can be seen from upper table 4 12-15 of the embodiment of the present invention be utilized respectively super critical CO 2 technology preparation containing smoking
The clothing grass cotton of extract, silk, hair natural fiber and our company before use water as solvent preparation containing mint extract
Cotton, silk, hair natural fiber, under conditions of preparation technology is differed, the natural fiber containing Herba Lysimachiae foenumgraeci extract of preparation
It is essentially the same that mechanical index does fracture strength, wet breaking strength, dry elongation at break etc.；To Escherichia coli, to golden yellow grape
Coccus, the bacteriostasis rate to Candida albicans are also more or less the same；
The soaping fastness for carrying out the fiber of safflower dyeing in supercritical carbon dioxide simultaneously is better than water-bath dyeing for 5 grades
3 grades of the soaping fastness of fiber.Show that carrying out function modified preparation to cotton, hair, silk using super critical CO 2 technology contains day
The natural fiber of right plant extracts and vegetable colour is feasible；And using super critical CO 2 technology without water or
Other reagents do not have the generation and discharge of waste water and waste as solvent, and more environmentally friendly, safer, technique is simpler.
Meanwhile, from table 2-4, on the premise of every physical index is consistent before fiber treatment, wherein in table 2, peppermint
Extract and the rhodizonate dye fiber modified to natural fiber, its wet breaking strength tool improve significantly, wherein, by peppermint
Extract and the modified cotton fiber of rhodizonate dye, its wet breaking strength is up to 3.5 cN/dtex；Contaminated by mint extract and rose
The modified silk fiber of material, its wet breaking strength is 32.2 cN/dtex；By the modified hair of mint extract and rhodizonate dye
Fiber, its wet breaking strength is 2.61 cN/dtex；And it is fine by the modified cotton of mint extract and rhodizonate dye, silk, hair
Dimension, its antibiotic rate to Escherichia coli, staphylococcus aureus, Candida albicans all has lifting by a relatively large margin.
The natural fiber containing lavender prepared using the technology of the present invention is spinned, is made into fabric, and then makes spinning
Product is knitted, testing result shows：When modified natural fibers content manufactured in the present embodiment reaches 30% in yarn, its is corresponding
Performance indications be can reach it is described above.
The performance test that the wormwood extract of embodiment 16 and purple perilla dyestuff are modified to yarn
The physical index such as its respective fiber number, fracture strength is consistent before modification for cotton, fiber crops, silk, hair.
The performance test results after wormwood extract that table 5 is listed, purple perilla modification yarn.Experimental group is using implementation
Method described in example 1, only changes the modified natural fiber of the species of extract, the yarn being made of conventional method, control
Group is, using the method described in embodiment 1, only to change the species of solvent, with water as solvent modified natural fiber, using routine
The yarn that method is made.
The experimental group of table 5 and control group quality index
It can be seen from upper table 5 17-20 of the embodiment of the present invention be utilized respectively super critical CO 2 technology preparation containing Chinese mugwort
The cotton of careless extract, silk, the yarn of hair used water as with our company before solvent preparation the cotton containing mint extract,
Silk, the yarn of hair, under conditions of preparation technology is differed, the mechanical index of the yarn containing wormwood extract of preparation is dry disconnected
Resistance to spalling, wet breaking strength, dry elongation at break etc. are basically unchanged；To Escherichia coli, to staphylococcus aureus, to white thought
The bacteriostasis rate of pearl bacterium is also more or less the same；
The soaping fastness of yarn manufactured in the present embodiment is 5 grades simultaneously, 3 grades of the soaping fastness of the yarn of water-bath dyeing.Show profit
With super critical CO 2 technology to cotton, hair, silk yarn carry out it is function modified prepare contain natural plant extracts and plant
The natural fiber of dyestuff is feasible；And by the use of super critical CO 2 technology without water or other reagents as solvent,
The generation and discharge of waste water and waste are not had, and more environmentally friendly, safer, technique is simpler.
The yarn containing wormwood prepared using the technology of the present invention is made into after textile product, and testing result shows：Work as wormwood
When the content of yarn reaches 30%, its corresponding performance indications be can reach it is described above.It is fine with other of Wormwood fiber blending
Dimension can be common viscose fiber, Modal, tencel etc., and other fiber contents of both blending are 70%.
The rhodizonate dye of embodiment 21 carries out function modified with mint extract to pure-cotton fabric
1st, the addition of pure-cotton fabric and rhodizonate dye and mint extract
When carrying out function modified, 200 kilograms of pure-cotton fabric is loaded in function modified cylinder, 2kg roses dye is loaded in mixing kettle
Material and 1kg mint extracts.
2nd, supercritical carbon dioxide is obtained
Then the liquid carbon dioxide being stored in liquid carbon dioxide storage tank is injected into CO 2 high pressure pump by pipeline
In；In high-pressure pump, its temperature is heated to 100 DEG C and obtains overcritical by carbon dioxide pressurization to 30MPa, then process preheater
Carbon dioxide；
3rd, the dissolving of rhodizonate dye and mint extract compound
Supercritical carbon dioxide fluid injection prepared by step 2 is equipped with rhodizonate dye and mint extract mixing kettle, in tank
100 DEG C of keeping temperature, pressure 30MPa, fully contact and are dissolved with rhodizonate dye and mint extract compound, disperse equal
It is even；
4th, function modified process
First by function modified kettle carry out heating pressurization, standby function be modified kettle in temperature reach 100 DEG C, pressure reach 30MPa
When, the supercritical carbon dioxide containing rhodizonate dye and mint extract after dissolving is injected into equipped with pure cotton face to be modified
Circulated in the function modified kettle of material, function modified 30min, 60min, 90min, 120 min, 150min are carried out respectively.
5th, last handling process
It is modified after terminating, supercritical carbon dioxide is separated through separator with vegetable colour and natural plant extracts, now,
The temperature of separator is 90 DEG C, pressure 2MPa, and gaseous carbon dioxide enters in condensation kettle, vegetable colour and natural plant extracts
Then stay in separating still；The temperature for condensing kettle is 20 DEG C or so（Room temperature）, pressure 4MPa, gaseous carbon dioxide is changed into liquid two
Carbonoxide is entered in liquid CO 2 storage tank, participates in modified technique next time, is recycled；Opening function is modified kettle, will
Modified pure-cotton fabric takes out；
Following table gives influence of the function modified time to fabric anti-microbial property：
Influence of the function modified time of table 6 to anti-microbial property
With the extension of function modified time it can be seen from upper table 6, function modified rear pure-cotton fabric is to Escherichia coli, golden yellow
The biocidal property of color staphylococcus and Candida albicans has strengthened, after 90 min, and its fungistatic effect increase is not obvious；Cause
This, the function modified time is 90 mim in the present invention.
Its soaping fastness is tested to the pure-cotton fabric after above-mentioned carry out plant dyeing by GB/T3921.3-1997 standards, surveyed
Test result shows：The soaping fastness that the fabric of rhodizonate dye dyeing is carried out in supercritical carbon dioxide is better than water-bath dye for 5 grades
3 grades of the soaping fastness of the fabric of color.And to pure-cotton fabric in supercritical carbon dioxide and progress rhodizonate dye dyeing in a water bath
With it is function modified when mechanical property be tested, test result surface：Rhodizonate dye is dyed in supercritical carbon dioxide
When, the strength of fabric drops to 10%, far smaller than fabric when water-bath rhodizonate dye is dyed 40% strength loss.
In addition to having carried out anti-microbial property detection to the pure-cotton fabric and ready-made clothes after function modified, due in mint extract
Also there is the chemical composition of cool feeling containing menthones, menthol etc., therefore, our inspections that also it has carried out moment cool feeling to fabric
Survey, its testing result is in 0.320W/cm2Left and right is higher than examination criteria（0.14 W/cm2）；Show to utilize supercritical carbon dioxide skill
It is feasible that art, which carries out function modified pure-cotton fabric of the preparation containing natural plant extracts to pure-cotton fabric,；
And by the use of super critical CO 2 technology without water or other reagents as solvent, the generation of waste water and waste is not had
With discharge, more environmentally friendly, safer, technique is simpler.
The safflower of embodiment 22 carries out function modified with wormwood extract to pure cotton ready-made clothes
1st, the addition of pure cotton ready-made clothes and safflower and wormwood extract
When carrying out function modified, in function modified cylinder load 200 kilograms of pure-cotton fabric, in mixing kettle load safflower and
Wormwood extract 2kg safflowers and 1kg wormwood extracts；
2nd, supercritical carbon dioxide is obtained
Then the liquid carbon dioxide being stored in liquid carbon dioxide storage tank is injected into CO 2 high pressure pump by pipeline
In；
In high-pressure pump, its temperature is heated to 90 DEG C and obtains overcritical by carbon dioxide pressurization to 30MPa, then process preheater
Carbon dioxide；
3rd, the dissolving of safflower and wormwood extract compound
Supercritical carbon dioxide fluid enters in the mixing kettle equipped with safflower and wormwood extract, keeping temperature 90 in tank
DEG C, pressure 30MPa, fully contact and dissolved with safflower and wormwood extract compound, be uniformly dispersed；
4th, function modified process
Function modified kettle is subjected to heating pressurization, the temperature that standby function is modified in kettle reaches 90 DEG C, pressure is when reaching 30MPa, will
The supercritical carbon dioxide containing safflower and wormwood extract after dissolving is injected into equipped with pure cotton ready-made clothes to be modified
Circulated in function modified kettle, respectively function modified 30min, 60min, 90min, 120 min, 150min, 180min,
210min；
5th, last handling process
It is modified after terminating, overcritical titanium dioxide is separated through separator with vegetable colour and natural plant extracts, now, point
Temperature from device is 80 DEG C, and pressure 2MPa, gaseous carbon dioxide enters in condensation kettle, and vegetable colour and natural plant extracts are then
Stay in separating still；The temperature for condensing kettle is 20 DEG C or so（Room temperature）, pressure 4MPa, gaseous carbon dioxide is changed into liquid dioxy
Change carbon to enter in liquid CO 2 storage tank, participate in modified technique next time, recycle；Opening function is modified kettle, will change
Property after pure cotton ready-made clothes take out；
Following table gives influence of the function modified time to pure cotton ready-made clothes anti-microbial property：
Influence of the function modified time of table 7 to anti-microbial property
With the extension of function modified time it can be seen from upper table 7, function modified rear pure cotton ready-made clothes is to Escherichia coli, golden yellow
The biocidal property of color staphylococcus and Candida albicans has strengthened, after 150 min, and its fungistatic effect increase is not obvious；
Therefore, the time function modified in the present invention is 150 mim.
Its soaping fastness is tested to the pure-cotton fabric after above-mentioned carry out plant dyeing by GB/T3921.3-1997 standards, surveyed
Test result shows：The soaping fastness that the ready-made clothes of safflower dyeing is carried out in supercritical carbon dioxide is better than water-bath dye for 5 grades
3 grades of the soaping fastness of the ready-made clothes of color.And to pure cotton ready-made clothes in supercritical carbon dioxide and progress safflower dyeing in a water bath
With it is function modified when mechanical property be tested, test result surface：Safflower is dyed in supercritical carbon dioxide
When, the strength of ready-made clothes drops to 10%, far smaller than ready-made clothes when water-bath safflower is dyed 40% strength loss.
Using super critical CO 2 technology pure cotton ready-made clothes is carried out it is function modified prepare containing natural plant extracts and
The pure cotton ready-made clothes of vegetable colour is feasible；And by the use of super critical CO 2 technology without water or other reagents as molten
Agent, the generation and discharge of waste water and waste are not had, and more environmentally friendly, safer, technique is simpler.
Natural fiber after being retrofited using super critical CO 2 technology can produce non-woven fabric；, can after spinning
To make all kinds of textile products such as underwear, T-shirt, towel, bed necessaries.
As can be seen here, the present invention is in function modified technical process is carried out to cotton, fiber crops, silk, hair and its fabric ready-made clothes
The waste water containing other chemical reagent and other discarded objects are produced, green, ecology, environmental protection, clean manufacturing, recyclable profit can be achieved
With, with cost is low, economic benefit, obvious environment benefit the characteristics of.
Finally it should be noted that：The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention,
Although the present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art, it still may be used
To be modified to the technical scheme described in foregoing embodiments, or equivalent substitution is carried out to which part technical characteristic.
Within the spirit and principles of the invention, any modification, equivalent substitution and improvements made etc., should be included in the present invention's
Within protection domain.
Claims (10)
1. the natural fibre products that a kind of utilization super critical CO 2 technology is modified, it is characterised in that：The modification it is natural
Fibre is cotton, fiber crops, silk, hair natural fiber or yarn, fabric or the ready-made clothes being made using the natural fiber.
2. the natural fibre products that a kind of utilization super critical CO 2 technology according to claim 1 is modified, its feature
It is：The wet breaking strength of the modified natural cotton fiber is 2.87-3.50 cN/dtex；The modified natural silk
The wet breaking strength of fiber is 30.2-32.2cN/dtex；The wet breaking strength of the modified natural wool fibre is 1.91-
2.61cN/dtex。
3. the natural fibre products that a kind of utilization super critical CO 2 technology according to claim 1 is modified, its feature
It is：The modified natural cotton fiber is 93-95% to the bacteriostasis rate of Escherichia coli；To the antibacterial of staphylococcus aureus
Rate is 91-95%；Bacteriostasis rate to Candida albicans is 87-89%；Suppression of the modified natural silk fibers to Escherichia coli
Bacterium rate is 90-98%, and the bacteriostasis rate to staphylococcus aureus is 92-96%, and the bacteriostasis rate to Candida albicans is 87-88%；Institute
It is 93-97% to the bacteriostasis rate of Escherichia coli to state modified natural wool fibre, and the bacteriostasis rate to staphylococcus aureus is 93-
95%, the bacteriostasis rate to Candida albicans is 87-96%.
4. a kind of method of utilization super critical CO 2 technology modified natural fibers product, it is characterised in that：Methods described bag
Include the addition step of natural fiber and vegetable colour and natural plant extracts；The natural fiber and vegetable colour and natural plant
The addition step of thing extract includes：Load natural fiber in function modified kettle；Load dyestuff and natural plant in mixing kettle
Thing extract；The amount for loading natural fiber is 200-220kg kilograms；The amount for loading dyestuff and natural plant extracts
Respectively 0.5-2kg and 1-3kg；Described natural fiber is cotton, fiber crops, silk or hair.
5. a kind of method of utilization super critical CO 2 technology modified natural fibers product according to claim 4, its
It is characterised by：Described natural plant extracts kind is mint extract, wormwood extract, one kind of Herba Pileae Scriptae extract or several
Kind.
6. a kind of method of utilization super critical CO 2 technology modified natural fibers product according to claim 4, its
It is characterised by：Described vegetable colour is the one or more in rhodizonate dye, violet dyes, safflower, purple perilla dyestuff.
7. a kind of method of utilization super critical CO 2 technology modified natural fibers product according to claim 4, its
It is characterised by：Described natural plant extracts kind is mint extract；Described vegetable colour is rhodizonate dye.
8. a kind of method of utilization super critical CO 2 technology modified natural fibers product according to claim 4, its
It is characterised by：Methods described also includes function modified process；The function modified process includes：Function modified kettle is heated up
Pressurization, the temperature that standby function is modified in kettle reaches 90-120 DEG C, pressure is when reaching 30MPa, by the overcritical dioxy in mixing kettle
Change carbon and be injected into mixing in the function modified kettle equipped with natural fiber to be modified；The incorporation time is 120-180min.
9. a kind of method of utilization super critical CO 2 technology modified natural fibers product according to claim 4, its
It is characterised by：Methods described also includes last handling process；The last handling process includes：By supercritical carbon dioxide through separator
Separated with vegetable colour and natural plant extracts；The temperature of the separator is 80-100 DEG C；The pressure of the separator
Power is 2-3Mpa.
10. a kind of method of utilization super critical CO 2 technology modified natural fibers product according to claim 9, its
It is characterised by：The last handling process also includes being condensed the gaseous carbon dioxide injection condensation kettle after separation；It is described cold
The temperature of solidifying kettle is 20-25 DEG C, pressure 4-6Mpa.
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| CN201710213544.XA CN107012698A (en) | 2017-04-01 | 2017-04-01 | Natural fibre products and method of modifying that a kind of utilization super critical CO 2 technology is modified |
| US15/870,927 US10947667B2 (en) | 2017-04-01 | 2018-01-13 | Methods and apparatuses for processing textile fibers, kettle automatic operation devices, and textile fiber products |
| PCT/CN2018/073622 WO2018177000A1 (en) | 2017-04-01 | 2018-01-22 | Methods and apparatuses for processing textile fibers, kettle automatic operation devices, and textile fiber products |
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| CN107904986A (en) * | 2017-12-26 | 2018-04-13 | 中原工学院 | Supercritical CO2Fluid natural textile dye composite and coloring system and method |
| CN107974844A (en) * | 2017-11-14 | 2018-05-01 | 江苏新瑞贝科技股份有限公司 | A kind of colouring method of natural fiber |
| CN108691201A (en) * | 2018-06-08 | 2018-10-23 | 滨州亚光家纺有限公司 | One kind being based on supercritical CO2Fluid technique makes processing method of the cellulose fibre with function for expelling pests |
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| CN108914599A (en) * | 2018-06-08 | 2018-11-30 | 滨州亚光家纺有限公司 | One kind being based on supercritical CO2Fluid technique makes processing method of the cellulose fibre with moisture-keeping functions |
| CN109023960A (en) * | 2018-06-08 | 2018-12-18 | 滨州亚光家纺有限公司 | One kind being based on supercritical CO2Fluid technique makes processing method of the cellulose fibre with crease-resistant function |
| CN108716110B (en) * | 2018-06-08 | 2021-04-20 | 苏州大学 | Based on supercritical CO2Processing method for making cellulose fibre possess antibacterial function by fluid technology |
| CN109056342B (en) * | 2018-06-08 | 2021-04-23 | 苏州大学 | Based on supercritical CO2Processing method for making cellulose fibre possess anti-inflammatory function by fluid technology |
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