CN110106704A - A kind of preparation method of the chitosan crosslinked polyester fiber of mono carboxylic - Google Patents
A kind of preparation method of the chitosan crosslinked polyester fiber of mono carboxylic Download PDFInfo
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- CN110106704A CN110106704A CN201910283137.5A CN201910283137A CN110106704A CN 110106704 A CN110106704 A CN 110106704A CN 201910283137 A CN201910283137 A CN 201910283137A CN 110106704 A CN110106704 A CN 110106704A
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- mono carboxylic
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/06—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyolefin as constituent
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/18—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/20—Polyalkenes, polymers or copolymers of compounds with alkenyl groups bonded to aromatic groups
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Artificial Filaments (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The present invention relates to a kind of preparation methods of the chitosan crosslinked polyester fiber of mono carboxylic, it uses ad hoc approach to prepare mono carboxylic Chitosan powder, it is low in cost, pollution-free, preparation condition is mild, easy to operate, reaction process is easily controllable, obtained mono carboxylic Chitosan powder with supplementary materials such as polyester materials again after reacting, the manufactured chitosan crosslinked polyester fiber of mono carboxylic has stronger fibre strength, the technical indicators such as its elongation at break, breaking strength, creasy recovery angle are preferable, suitable for textile further genralrlization use.
Description
Technical field
The present invention relates to new textile material technical fields, more particularly to a kind of chitosan crosslinked polyester fiber of mono carboxylic
Preparation method.
Background technique
The raw material sources of chitosan are in largely discarded shrimp shell, and the oxidation chitosan aqueous solution after reacting is through at dry
Reason, and oxidation chitosan can be re-dissolved to preparation reaction solution and be used for graft modification, recovery utilization rate is high, and at low cost, workshop is set
Standby and energy demand is few.Common chitosan graft textile fabric need to be dissolved in the acid solution containing chemical cross-linking agent, be polluted
Environment has a negative impact to textile good characteristic and human health.
It is soluble easily in water to aoxidize chitosan, chemical graft can occur with fiber under the conditions of no chemical cross-linking agent, it is lasting to obtain
Efficient antibacterial functions, and chitosan aqueous solution is aoxidized after moisture removal is removed in drying, and can be recycled again.Water soluble oxidized
Amino in chitosan molecule can have positive charge (- NH3+) by carboxylic protons, have efficient durable, reproducible antibacterial
Activity.Aoxidize and contain carboxyl and amino in chitosan molecule chain simultaneously, be a kind of amphoteric polysaccharide, macromolecular structure and property with
Protein is similar, has excellent biocompatibility, degradability, can be used as green crosslinking agent, antibacterial agent, accelerant in textile
Functional treatment in use safely.If but oxidation chitosan uses conventional chitosan used in the process of being grafted textile fabric
Supplementary material and preparation method, obtained fibrous material often have the shortcomings that fibre strength deficiency, limit to a certain extent
Application of the oxidation chitosan in textile material.
Summary of the invention
Based on this, it is necessary to insufficient for oxidation chitosan is currently prepared fibre strength present in forming material
Problem provides a kind of preparation method of chitosan crosslinked polyester fiber of mono carboxylic.
A kind of preparation method of the chitosan crosslinked polyester fiber of mono carboxylic, comprising the following steps:
(1) 20 g chitosans are dissolved in the acetum that concentration is 3.5% according to mass ratio 1:30, then instill 800 ul
Concentrated nitric acid and 1500 ul concentrated phosphoric acids are added -3 methylimidazole acetate of 3.5 g 1- butyl and 1.8 g isopropanols, stir and evenly mix
Tinfoil closed container is used afterwards, is placed in progress ultrasonic reaction in ultrasonic vibration instrument and is obtained reaction solution, wherein ultrasonic power is 250 KW,
Ultrasonic time is 20 minutes;
(2) reaction solution that step (1) obtains is stood 16-20 hours in Cool Room 4 DEG C;
(3) by step (2) through the solution filtration washing after stand at low temperature, obtained solid is deposited at 42-45 DEG C and dries, then
Ground crushing obtains mono carboxylic Chitosan powder;
(4) by 350 g polyester materials, -3 methyl imidazolium tetrafluoroborate of 6.3 g 1- butyl, 4.5 g sodium nitrites, 4.2 g
Benzaldehyde,2-hydroxy, 2.8 g stearic amides and 3.5 g crosslinking agents are added in reacting furnace jointly, are risen to in-furnace temperature
It 90-95 DEG C, is persistently stirred according to 300-500 revs/min of stirring rate, until mixture is at thick;
(5) the mono carboxylic Chitosan powder that step (3) obtains is taken out into half and is added to the viscous mixture that step (4) obtains
In, it keeps reaction temperature at 90-95 DEG C, persistently stirs 30 minutes, obtained most according to 1000-1200 revs/min of stirring rate
Whole mixture;
(6) final mixture obtained step (5) injects double screw extruder, sets extruder temperature as 220-260 DEG C, screw rod
Revolving speed is 1000 revs/min, and it is crude to obtain fiber then according to 2-5m/ minutes spinning speed melt spinnings for extruding pelletization
Product;
(7) fiber preform in step (6) is placed in nitrogen atmosphere, remaining mono carboxylic shell is sprayed on fiber preform
Glycan powder, while reaction temperature is improved to 105 DEG C, 3-5 minutes are kept the temperature, is cooled to room temperature after taking-up poly- to get mono carboxylic shell
Sugared cross-linked polyester fiber.
The preparation method of the above-mentioned chitosan crosslinked polyester fiber of mono carboxylic, prepares mono carboxylic chitosan powder using ad hoc approach
End, low in cost, pollution-free, preparation condition is mild, easy to operate, reaction process is easily controllable, and obtained mono carboxylic shell is poly-
Again after reacting with supplementary materials such as polyester materials, the manufactured chitosan crosslinked polyester fiber of mono carboxylic has stronger fibre at Icing Sugar end
Intensity is tieed up, the technical indicators such as elongation at break, breaking strength, creasy recovery angle are preferable, suitable for further textile
It promotes the use of.
It is preferable to use dehydrated alcohols to be filtered washing in the step (3) in one of the embodiments,.
The polyester material in the step (4) is selected from polyester piece, polypropylene foil, polyamide in one of the embodiments,
Piece, polycaprolactone, polypropylene, any one in polyethylene terephthalate.
The crosslinking agent in the step (4) is preferably dibutyl phthalate in one of the embodiments,.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph for the chitosan crosslinked polyester fiber of mono carboxylic that the embodiment of the present invention 2 obtains.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, with reference to the accompanying drawing to the present invention
Specific embodiment be described in detail.Many details are explained in the following description in order to fully understand this hair
It is bright.But the invention can be embodied in many other ways as described herein, those skilled in the art can be not
Similar improvement is done in the case where violating intension of the present invention, therefore the present invention is not limited by the specific embodiments disclosed below.
Embodiment 1
(1) 20 g chitosans are dissolved in the acetum that concentration is 3.5% according to mass ratio 1:30, then instill 800 ul
Concentrated nitric acid and 1500 ul concentrated phosphoric acids are added -3 methylimidazole acetate of 3.5 g 1- butyl and 1.8 g isopropanols, stir and evenly mix
Tinfoil closed container is used afterwards, is placed in progress ultrasonic reaction in ultrasonic vibration instrument and is obtained reaction solution, wherein ultrasonic power is 250 KW,
Ultrasonic time is 20 minutes;
(2) reaction solution that step (1) obtains is stood 16 hours in Cool Room 4 DEG C;
(3) by step (2) through the solution filtration washing after stand at low temperature, obtained solid is deposited at 42 DEG C and dries, then passes through
It grinds to obtain mono carboxylic Chitosan powder;
(4) by 350 g polypropylene foils, -3 methyl imidazolium tetrafluoroborate of 6.3 g 1- butyl, 4.5 g sodium nitrites, 4.2 g
Benzaldehyde,2-hydroxy, 2.8 g stearic amides and 3.5 g dibutyl phthalates are added in reacting furnace jointly, in furnace
Temperature rises to 90 DEG C, persistently stirs according to 300 revs/min of stirring rates, until mixture is at thick;
(5) the mono carboxylic Chitosan powder that step (3) obtains is taken out into half and is added to the viscous mixture that step (4) obtains
In, it keeps reaction temperature at 90 DEG C, is persistently stirred 30 minutes according to 1000 revs/min of stirring rates, obtain final mixture;
(6) final mixture obtained step (5) injects double screw extruder, sets extruder temperature as 220 DEG C, screw speed
It is 1000 revs/min, extruding pelletization obtains fiber preform then according to 2m/ minutes spinning speed melt spinnings;
(7) fiber preform in step (6) is placed in nitrogen atmosphere, remaining mono carboxylic shell is sprayed on fiber preform
Glycan powder, while reaction temperature is improved to 105 DEG C, 3 minutes are kept the temperature, is cooled to room temperature after taking-up to get mono carboxylic chitosan
Cross-linked polyester fiber.
Embodiment 2
(1) 20 g chitosans are dissolved in the acetum that concentration is 3.5% according to mass ratio 1:30, then instill 800 ul
Concentrated nitric acid and 1500 ul concentrated phosphoric acids are added -3 methylimidazole acetate of 3.5 g 1- butyl and 1.8 g isopropanols, stir and evenly mix
Tinfoil closed container is used afterwards, is placed in progress ultrasonic reaction in ultrasonic vibration instrument and is obtained reaction solution, wherein ultrasonic power is 250 KW,
Ultrasonic time is 20 minutes;
(2) reaction solution that step (1) obtains is stood 18 hours in Cool Room 4 DEG C;
(3) by step (2) through the solution filtration washing after stand at low temperature, obtained solid is deposited at 45 DEG C and dries, then passes through
It grinds to obtain mono carboxylic Chitosan powder;
(4) by 350 g polyester pieces, -3 methyl imidazolium tetrafluoroborate of 6.3 g 1- butyl, 4.5 g sodium nitrites, 4.2 g 2-
Hydroxy benzaldehyde, 2.8 g stearic amides and 3.5 g dibutyl phthalates are added in reacting furnace jointly, to warm in furnace
Degree rises to 92 DEG C, persistently stirs according to 400 revs/min of stirring rates, until mixture is at thick;
(5) the mono carboxylic Chitosan powder that step (3) obtains is taken out into half and is added to the viscous mixture that step (4) obtains
In, it keeps reaction temperature at 92 DEG C, is persistently stirred 30 minutes according to 1100 revs/min of stirring rates, obtain final mixture;
(6) final mixture obtained step (5) injects double screw extruder, sets extruder temperature as 240 DEG C, screw speed
It is 1000 revs/min, extruding pelletization obtains fiber preform then according to 3.5 m/ minutes spinning speed melt spinning;
(7) fiber preform in step (6) is placed in nitrogen atmosphere, remaining mono carboxylic shell is sprayed on fiber preform
Glycan powder, while reaction temperature is improved to 105 DEG C, 4 minutes are kept the temperature, is cooled to room temperature after taking-up to get mono carboxylic chitosan
Cross-linked polyester fiber.
Embodiment 3
(1) 20 g chitosans are dissolved in the acetum that concentration is 3.5% according to mass ratio 1:30, then instill 800 ul
Concentrated nitric acid and 1500 ul concentrated phosphoric acids are added -3 methylimidazole acetate of 3.5 g 1- butyl and 1.8 g isopropanols, stir and evenly mix
Tinfoil closed container is used afterwards, is placed in progress ultrasonic reaction in ultrasonic vibration instrument and is obtained reaction solution, wherein ultrasonic power is 250 KW,
Ultrasonic time is 20 minutes;
(2) reaction solution that step (1) obtains is stood 20 hours in Cool Room 4 DEG C;
(3) by step (2) through the solution filtration washing after stand at low temperature, obtained solid is deposited at 45 DEG C and dries, then passes through
It grinds to obtain mono carboxylic Chitosan powder;
(4) by 350 g polyethylene terephthalates, -3 methyl imidazolium tetrafluoroborate of 6.3 g 1- butyl, 4.5 g nitrous
Sour sodium, 4.2 g Benzaldehyde,2-hydroxies, 2.8 g stearic amides and 3.5 g dibutyl phthalates are added to reaction jointly
In furnace, 95 DEG C are risen to in-furnace temperature, is persistently stirred according to 500 revs/min of stirring rates, until mixture is at sticky
Shape;
(5) the mono carboxylic Chitosan powder that step (3) obtains is taken out into half and is added to the viscous mixture that step (4) obtains
In, it keeps reaction temperature at 95 DEG C, is persistently stirred 30 minutes according to 1200 revs/min of stirring rates, obtain final mixture;
(6) final mixture obtained step (5) injects double screw extruder, sets extruder temperature as 260 DEG C, screw speed
It is 1000 revs/min, extruding pelletization obtains fiber preform then according to 5 m/ minutes spinning speed melt spinning;
(7) fiber preform in step (6) is placed in nitrogen atmosphere, remaining mono carboxylic shell is sprayed on fiber preform
Glycan powder, while reaction temperature is improved to 105 DEG C, 5 minutes are kept the temperature, is cooled to room temperature after taking-up to get mono carboxylic chitosan
Cross-linked polyester fiber.
Elongation at break, fracture are strong after measured for the chitosan crosslinked polyester fiber of mono carboxylic that 1-3 of the embodiment of the present invention is obtained
The technical indicators such as degree, creasy recovery angle, elongation at break is up to 30-35%, breaking strength up to 130-138N, crease recovery
Angle is greater than 200 °, is superior to similar product.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (4)
1. a kind of preparation method of the chitosan crosslinked polyester fiber of mono carboxylic, which comprises the following steps:
(1) 20 g chitosans are dissolved in the acetum that concentration is 3.5% according to mass ratio 1:30, then instill 800 ul
Concentrated nitric acid and 1500 ul concentrated phosphoric acids are added -3 methylimidazole acetate of 3.5 g 1- butyl and 1.8 g isopropanols, stir and evenly mix
Tinfoil closed container is used afterwards, is placed in progress ultrasonic reaction in ultrasonic vibration instrument and is obtained reaction solution, wherein ultrasonic power is 250 KW,
Ultrasonic time is 20 minutes;
(2) reaction solution that step (1) obtains is stood 16-20 hours in Cool Room 4 DEG C;
(3) by step (2) through the solution filtration washing after stand at low temperature, obtained solid is deposited at 42-45 DEG C and dries, then
Ground crushing obtains mono carboxylic Chitosan powder;
(4) by 350 g polyester materials, -3 methyl imidazolium tetrafluoroborate of 6.3 g 1- butyl, 4.5 g sodium nitrites, 4.2 g
Benzaldehyde,2-hydroxy, 2.8 g stearic amides and 3.5 g crosslinking agents are added in reacting furnace jointly, are risen to in-furnace temperature
It 90-95 DEG C, is persistently stirred according to 300-500 revs/min of stirring rate, until mixture is at thick;
(5) the mono carboxylic Chitosan powder that step (3) obtains is taken out into half and is added to the viscous mixture that step (4) obtains
In, it keeps reaction temperature at 90-95 DEG C, persistently stirs 30 minutes, obtained most according to 1000-1200 revs/min of stirring rate
Whole mixture;
(6) final mixture obtained step (5) injects double screw extruder, sets extruder temperature as 220-260 DEG C, screw rod
Revolving speed is 1000 revs/min, and it is crude to obtain fiber then according to 2-5m/ minutes spinning speed melt spinnings for extruding pelletization
Product;
(7) fiber preform in step (6) is placed in nitrogen atmosphere, remaining mono carboxylic shell is sprayed on fiber preform
Glycan powder, while reaction temperature is improved to 105 DEG C, 3-5 minutes are kept the temperature, is cooled to room temperature after taking-up poly- to get mono carboxylic shell
Sugared cross-linked polyester fiber.
2. the preparation method of the chitosan crosslinked polyester fiber of mono carboxylic according to claim 1, which is characterized in that the step
Suddenly it is preferable to use dehydrated alcohols to be filtered washing in (3).
3. the preparation method of the chitosan crosslinked polyester fiber of mono carboxylic according to claim 1, which is characterized in that the step
Suddenly the polyester material in (4) is selected from polyester piece, polypropylene foil, polyamide slices, polycaprolactone, polypropylene, poly terephthalic acid second
Any one in diol ester.
4. the preparation method of the chitosan crosslinked polyester fiber of mono carboxylic according to claim 1, which is characterized in that the step
Suddenly the crosslinking agent in (4) is preferably dibutyl phthalate.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113116007A (en) * | 2021-02-04 | 2021-07-16 | 雅蒂诗(广州)时装有限公司 | Double-sided wind coat and processing technology thereof |
Citations (4)
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CN1425695A (en) * | 2003-01-20 | 2003-06-25 | 河北职业技术师范学院 | Amphoteric chitosan and its preparing method |
CN105061637A (en) * | 2015-09-07 | 2015-11-18 | 安徽农业大学 | Water-soluble antibacterial monocarboxylic chitosan as well as preparation method and application thereof |
CN105803576A (en) * | 2016-03-10 | 2016-07-27 | 安徽翰联纺织有限公司 | Process method for producing antibacterial and deodorant polyester fibers by adopting monocarboxy-chitosan |
CN107474161A (en) * | 2017-10-19 | 2017-12-15 | 安徽农业大学 | A kind of selective oxidation chitosan and its heterogeneous preparation method |
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2019
- 2019-04-10 CN CN201910283137.5A patent/CN110106704A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1425695A (en) * | 2003-01-20 | 2003-06-25 | 河北职业技术师范学院 | Amphoteric chitosan and its preparing method |
CN105061637A (en) * | 2015-09-07 | 2015-11-18 | 安徽农业大学 | Water-soluble antibacterial monocarboxylic chitosan as well as preparation method and application thereof |
CN105803576A (en) * | 2016-03-10 | 2016-07-27 | 安徽翰联纺织有限公司 | Process method for producing antibacterial and deodorant polyester fibers by adopting monocarboxy-chitosan |
CN107474161A (en) * | 2017-10-19 | 2017-12-15 | 安徽农业大学 | A kind of selective oxidation chitosan and its heterogeneous preparation method |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113116007A (en) * | 2021-02-04 | 2021-07-16 | 雅蒂诗(广州)时装有限公司 | Double-sided wind coat and processing technology thereof |
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