CN110042658A - A kind of flame-proof antibiotic liquid and its preparation method and application - Google Patents
A kind of flame-proof antibiotic liquid and its preparation method and application Download PDFInfo
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- CN110042658A CN110042658A CN201910322809.9A CN201910322809A CN110042658A CN 110042658 A CN110042658 A CN 110042658A CN 201910322809 A CN201910322809 A CN 201910322809A CN 110042658 A CN110042658 A CN 110042658A
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- flame
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- proof antibiotic
- antibiotic liquid
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- 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
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/68—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
- D06M11/70—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
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- 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
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/68—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
- D06M11/72—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with metaphosphoric acids or their salts; with polyphosphoric acids or their salts; with perphosphoric acids or their salts
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- 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
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- 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
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
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- 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
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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- 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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- 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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/30—Flame or heat resistance, fire retardancy properties
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a kind of flame-proof antibiotic liquid, it is the aqueous solution of chitosan and inorganic phosphor-contained acid, chitosan and inorganic phosphor-contained acid are mixed to prepare, excellent in stability and has broad spectrum antibacterial performance, again because thus having flame retardant property outstanding using phosphoric acid as " acid source ", chitosan as " carbon source " and " gas source ".Simultaneously, the present invention discloses the above-mentioned preparation method with fire-retardant and antibiotic property chitosan solution, such preparation method raw material is cheap and easy to get, and without using poisonous and harmful reagents such as organic solvent and formaldehyde, preparation process is simple, mild condition, by-product is not generated, it is quick, energy saving and pollution-free, it can large-scale industrial production.It is disclosed by the invention that there is fire-retardant and antibiotic property chitosan solution to be widely used, for arranging the textiles such as cotton, terylene, polyester-cotton blend, textile can be made to have broad spectrum antibacterial and excellent flame retardant property, there is application prospect in fields such as public transport, home decoration and bio-medicals.
Description
Technical field
The invention belongs to textile fabric finishing technique fields, and in particular to a kind of flame-proof antibiotic liquid and preparation method thereof.
Background technique
Chitin (chitin) be referred to as after protein, fat, carbohydrate, vitamin, minerals " the sixth-largest life is wanted
Element " is be only second to cellulose second largest using biomass regenerated resources, extensively from crustaceans shells such as shrimp, crabs
In, in the cell wall of mollusk endoskeleton, insect wing and fungi and algae, the chitin in the crusts waste such as shrimp, crab
Content be even as high as 10%-20%.Chitosan (chitosan) is also known as chitosan, is the deacetylated production of chitin
Object (deacetylation >=55%), usually may be dissolved in dilute formic acid, acetic acid diluted and dilute hydrochloric acid, through alkylation, acylation, carboxymethyl
The different chitosan derivatives of various performances can be made in change, sulfonation, nitrification or halogenation etc..Chitosan and its derivative (such as carboxylic
Methyl chitosan, n-trimethyl chitosan chloride, Guanoctine chitosan etc.) permeability of bacterial cell membrane can be changed or in its cell interior suction
Attached flocculent cell matter, interference DNA replication dna and transcription etc., have broad spectrum antibacterial；Meanwhile chitosan and its derivative contains largely
Hydroxyl, amino groups, and when burning release ammonia etc. non-ignitable/fire retardant gas excellent at charcoal, with phosphonium flame retardant (such as poly- phosphorus
Sour ammonium, phytate etc.) Intumescent Retardant System can be constructed.The value added applications that chitosan is realized with simple technology, to can be again
Raw low value waste rationally recycles, reduces environmental pollution and improves production efficiency and is of great significance.Such as patent
A kind of flame-retardant antibacterial finishing liquid disclosed in CN201811041919X includes: organic-pillared vermiculite 5-10% (weight ratio, similarly hereinafter),
Cyclo-dextrin-modified 3- glycydoxy trialkoxy silane 1-5%, chitosan 1-5%, polybasic carboxylic acid 5-10% are secondary
Sodium phosphite 1-5%, surplus are water, can be allowed to have flame-proof antibiotic effect for padding finishing embryo cloth.But prepare such resistance
Combustion antibiotic finishing solution need to use high boiling organic solvent dimethylformamide (DMF), remove needed for DMF that energy consumption is high and not ring
It protects.
Summary of the invention
The object of the present invention is to provide a kind of flame-proof antibiotic liquid and preparation method thereof, the chitosan solution be chitosan with contain
The aqueous solution of phosphorus inorganic acid.The chitosan solution stability is strong, has broad spectrum antibacterial performance, and because using phosphoric acid as " acid
Source ", chitosan are used as " carbon source " and " gas source ", and thus have flame retardant property outstanding.
It is a further object of the present invention to provide the above-mentioned preparation methods with flame-proof antibiotic liquid, can solve existing flame-proof antibiotic
Liquid preparation process energy consumption is high and not environmentally the problem of.The raw material of the method is cheap and easy to get, only uses water as solvent, without using organic
The poisonous and harmful reagent such as solvent and formaldehyde, preparation process is simple, mild condition, does not generate by-product, quickly, energy conservation and without dirt
Dye, can large-scale industrial production.
To achieve the above objectives, it is water-soluble with inorganic phosphor-contained acid that a kind of flame-proof antibiotic liquid of the present invention is chitosan
Liquid.
A kind of preparation method of flame-proof antibiotic liquid of the present invention, specifically: under room temperature, chitosan is distributed in batches
It in water, is vigorously stirred down, the aqueous solution of inorganic phosphor-contained acid is added until reaction solution is transparent, resulting yellow solution is most
Final product.
The inorganic phosphor-contained acid is hypophosphorous acid, phosphorous acid, phosphoric acid, pyrophosphoric acid and polyphosphoric acid (wherein, hypophosphorous acid, phosphorous
Sour accounting should be twice or more of phosphoric acid, pyrophosphoric acid and polyphosphoric acid) one of or a variety of mixtures, preferably hypophosphorous acid
With the mixture of one of phosphorous acid or both.
Deacetylation >=60% of the chitosan, preferably deacetylation are >=70%, to guarantee chitosan phosphorous
Excellent dissolubility in the diluted acid of inorganic acid.
Viscosity≤1Pas of the chitosan of the chitosan, preferred viscosities 0.05-0.8Pas, to guarantee that shell is poly-
The film forming and dissolubility in an acidic solution of sugar.
PH≤6 of the flame-proof antibiotic liquid, preferably pH are 5-6, and the too low degradation rate that can make chitosan of pH is too fast, shadow
Ring the stability of such chitosan solution.
Solid content≤5wt% of the flame-proof antibiotic liquid of the flame-proof antibiotic liquid, preferably solid content are 2-3wt%, according to
The deacetylation and molecular weight of chitosan are different, to ensure that flame-proof antibiotic liquid is transparent uniform.
The present invention also provides the applications of the flame-proof antibiotic liquid, by impregnating or spraying, for arrange cotton, terylene,
The textiles such as polyester-cotton blend make textile have broad spectrum antibacterial and excellent flame retardant property.
Compared with the prior art, the invention has the following advantages:
1, flame-proof antibiotic liquid provided by the invention has fire-retardant and antibiotic property simultaneously.This chitosan acid solution stability
It is excellent, have a broad spectrum antibacterial performance, and because using inorganic phosphor-contained acid as " acid source ", chitosan as " carbon source " and " gas source ", structure
At Intumescent Retardant System, and it is allowed to have flame retardant property outstanding.
2, the preparation method of above-mentioned flame-proof antibiotic liquid provided by the invention, be chitosan is dissolved in it is inorganic phosphor-contained acid it is water-soluble
Raw materials used cheap and easy to get without adding acetic acid and hydrochloric acid etc. in liquid, preparation process is simple, mild condition, and without using organic molten
Agent etc., it is quick, energy saving and pollution-free, it is conducive to expanding production, realizes industrialization.
3, flame-proof antibiotic liquid provided by the invention is widely used, especially suitable for arranging the weaving such as cotton, terylene, polyester-cotton blend
Product can make textile have broad spectrum antibacterial and excellent flame retardant property, lead in public transport, home decoration and bio-medical etc.
Domain has broad application prospect.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph (× 100) of polyester-cotton blend embryo cloth (a) He application examples 3 (b), because of the excellent film forming of chitosan,
Uniform flame-proof antibiotic layer can be formed on textile fiber surface.
Fig. 2 is that application examples 2 is tested according to GB/T 20944.1-2007 " evaluation of anti-microbial property: agar plate diffusion method "
As a result, Escherichia coli (a) and staphylococcus aureus (b), show that it belongs to low dissolution type antibacterial agent.
Specific embodiment
Example given below is with the invention will be further described.It is necessarily pointed out that following embodiment is not
It can be interpreted as limiting the scope of the invention, if the person skilled in the art in the field is according to aforementioned present invention content to this
Some nonessential modifications and adaptations are made in invention, still fall within the scope of the present invention.
It is worth noting that, following application examples 1) limit oxygen index measures according to ASTM D 2863-00 standard,
Vertical burn test is measured according to ASTM D 6413-08 standard；2) bacteriostasis rate test is according to GB/T 20944.3-2008
Standard " antibacterial textile performance evaluation: succusion " is tested.
Embodiment 1
At normal temperatures and pressures, 2g chitosan (viscosity 0.2-0.4Pas, deacetylation 60%) is distributed in batches
In 80g water, in being vigorously stirred, 50% aqueous solution of hypophosphorous acid is added until reaction solution is transparent (pH is about 5), it is resulting light
Yellow solution is final product.
Embodiment 2
At normal temperatures and pressures, 2g chitosan (viscosity 0.05-0.8Pas, deacetylation 70%) is distributed in batches
In 100g water, in being vigorously stirred, 45% aqueous solution of phosphorous acid is added until reaction solution is transparent (pH is about 5), it is resulting
Yellow solution is final product.
Embodiment 3
At normal temperatures and pressures, 2g chitosan (viscosity 0.05-0.8Pas, deacetylation 70%) is distributed in batches
In 90g water, in being vigorously stirred, (weight ratio of hypophosphorous acid and phosphorous acid is 1:1, is implemented below for addition hypophosphorous acid and phosphorous acid
Example it is all the same) 40% aqueous solution until reaction solution is transparent (pH is about 5), resulting yellow solution is final product.
Embodiment 4
At normal temperatures and pressures, 1g chitosan (viscosity 0.05-0.8Pas, deacetylation 75%) is distributed in batches
In 100g water, in being vigorously stirred, 35% aqueous solution that hypophosphorous acid, phosphorous acid and phosphoric acid (2:2:1) is added is transparent to reaction solution
Until (pH is about 4), resulting yellow solution is final product.
Embodiment 5
At normal temperatures and pressures, 1g chitosan (viscosity 0.05-0.8Pas, deacetylation 80%) is distributed in batches
In 75g water, in being vigorously stirred, 35% aqueous solution that hypophosphorous acid, phosphorous acid and pyrophosphoric acid (3:3:1) is added is transparent to reaction solution
Until (pH is about 4), resulting yellow solution is final product.
Embodiment 6
At normal temperatures and pressures, 1g chitosan (viscosity 0.1-0.2Pas, deacetylation 95%) is distributed in batches
In 80g water, in being vigorously stirred, 35% water of hypophosphorous acid, phosphorous acid, phosphoric acid, pyrophosphoric acid and polyphosphoric acid (5:5:1:1:1) is added
Solution (pH is about 4) until reaction solution is transparent, resulting yellow solution is final product.
Application examples 1
The application example is by 3 products therefrom finishing of cotton textiles of embodiment, and preparing flame-proof antibiotic cotton fabric, (rate of body weight gain is
12.5%).Such cotton fabric is both greater than 99% to the bacteriostasis rate of staphylococcus aureus and Escherichia coli；Limit oxygen index value is
30.5%, and pass through vertical burn test.
Application examples 2
1 products therefrom of embodiment is arranged dacron by the application example, prepares flame-proof antibiotic terylene (rate of body weight gain 15%).
Such terylene is both greater than 99% to the bacteriostasis rate of staphylococcus aureus and Escherichia coli；Limit oxygen index value is 29.0%, and
Pass through vertical burn test.
Application examples 3
2 products therefrom of embodiment is arranged polyester-cotton blend (35/65) by the application example, and (rate of body weight gain is the flame-proof antibiotic polyester-cotton blend of preparation
18.5%).Such polyester-cotton blend is both greater than 99% to the bacteriostasis rate of staphylococcus aureus and Escherichia coli；Limit oxygen index value is
27.5%, and pass through vertical burn test.
Claims (10)
1. a kind of flame-proof antibiotic liquid, it is characterised in that be the aqueous solution of chitosan Yu inorganic phosphor-contained acid.
2. flame-proof antibiotic liquid according to claim 1, it is characterised in that the inorganic phosphor-contained acid is hypophosphorous acid, phosphorous
One of acid, phosphoric acid, pyrophosphoric acid and polyphosphoric acid or a variety of mixtures.
3. flame-proof antibiotic liquid according to claim 1, it is characterised in that described is deacetylation >=60% of chitosan.
4. flame-proof antibiotic liquid according to claim 1, it is characterised in that viscosity≤1Pas of the chitosan.
5. flame-proof antibiotic liquid according to claim 1-4, it is characterised in that the inorganic phosphor-contained acid is time phosphorus
The viscosity of the mixture of one of acid and phosphorous acid or both, the chitosan is 0.05-0.8Pas, and described is shell
The deacetylation of glycan is >=70%.
6. a kind of preparation method for the flame-proof antibiotic liquid that claim 5 is stated, it is characterised in that steps are as follows: under room temperature, shell being gathered
Sugar batch is distributed in water, and in being vigorously stirred, the aqueous solution of inorganic phosphor-contained acid is added until reaction solution is transparent, resulting light
Yellow solution is final product.
7. the preparation method of flame-proof antibiotic liquid according to claim 6, it is characterised in that fire-retardant anti-obtained by this method
PH≤6 of bacterium solution.
8. the preparation method of flame-proof antibiotic liquid according to claim 7, it is characterised in that fire-retardant anti-obtained by this method
Solid content≤5wt% of bacterium solution.
9. the preparation method of flame-proof antibiotic liquid according to claim 8, it is characterised in that the pH of flame-proof antibiotic liquid is 5-6,
Solid content is 2-3wt%.
10. a kind of application of flame-proof antibiotic liquid described in claim 1.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910322809.9A CN110042658B (en) | 2019-04-22 | 2019-04-22 | Flame-retardant antibacterial liquid and preparation method and application thereof |
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| CN201910322809.9A CN110042658B (en) | 2019-04-22 | 2019-04-22 | Flame-retardant antibacterial liquid and preparation method and application thereof |
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| CN110042658A true CN110042658A (en) | 2019-07-23 |
| CN110042658B CN110042658B (en) | 2021-08-31 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111962298A (en) * | 2020-09-03 | 2020-11-20 | 应急管理部四川消防研究所 | Metal ion synergistic low-concentration organic biomass durable flame-retardant after-finishing modified nylon fabric and preparation method thereof |
| CN112878050A (en) * | 2021-01-19 | 2021-06-01 | 众望布艺股份有限公司 | 3D (three-dimensional) breathable fabric and preparation method thereof |
| CN114701230A (en) * | 2022-03-25 | 2022-07-05 | 龙岩东腾再生资源科技有限公司 | Needle cotton with good flame-retardant effect and processing method thereof |
| CN115651207A (en) * | 2022-10-14 | 2023-01-31 | 江西省安安科技有限公司 | In-situ polymerization flame retardant and preparation method thereof |
| CN116285677A (en) * | 2023-03-20 | 2023-06-23 | 四川大学 | Transparent intumescent fireproof antibacterial coating and preparation method thereof |
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| WO2011008204A1 (en) * | 2009-07-15 | 2011-01-20 | Technical Textiles | Ionized performance fabric with antimicrobial/antibacterial/antifungal properties |
| CN102659959A (en) * | 2012-04-13 | 2012-09-12 | 同济大学 | Preparation method of three-in-one intumescent fire retardant |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111962298A (en) * | 2020-09-03 | 2020-11-20 | 应急管理部四川消防研究所 | Metal ion synergistic low-concentration organic biomass durable flame-retardant after-finishing modified nylon fabric and preparation method thereof |
| CN112878050A (en) * | 2021-01-19 | 2021-06-01 | 众望布艺股份有限公司 | 3D (three-dimensional) breathable fabric and preparation method thereof |
| CN114701230A (en) * | 2022-03-25 | 2022-07-05 | 龙岩东腾再生资源科技有限公司 | Needle cotton with good flame-retardant effect and processing method thereof |
| CN114701230B (en) * | 2022-03-25 | 2024-09-17 | 龙岩东腾再生资源科技有限公司 | Needle cotton with good flame retardant effect and processing method thereof |
| CN115651207A (en) * | 2022-10-14 | 2023-01-31 | 江西省安安科技有限公司 | In-situ polymerization flame retardant and preparation method thereof |
| CN116285677A (en) * | 2023-03-20 | 2023-06-23 | 四川大学 | Transparent intumescent fireproof antibacterial coating and preparation method thereof |
| CN116285677B (en) * | 2023-03-20 | 2024-03-01 | 四川大学 | Transparent intumescent fireproof antibacterial coating and preparation method thereof |
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