CN107557904A - Antimicrobial fabric and its production method with nano silver particles - Google Patents
Antimicrobial fabric and its production method with nano silver particles Download PDFInfo
- Publication number
- CN107557904A CN107557904A CN201710957218.XA CN201710957218A CN107557904A CN 107557904 A CN107557904 A CN 107557904A CN 201710957218 A CN201710957218 A CN 201710957218A CN 107557904 A CN107557904 A CN 107557904A
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- CN
- China
- Prior art keywords
- functional poly
- nano silver
- purchased
- poly carbamate
- carbamate fibre
- Prior art date
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 130
- 239000004744 fabric Substances 0.000 title claims abstract description 56
- 230000000845 anti-microbial effect Effects 0.000 title claims abstract description 53
- 239000002245 particle Substances 0.000 title claims abstract description 50
- 238000004519 manufacturing process Methods 0.000 title abstract description 5
- 239000000835 fiber Substances 0.000 claims abstract description 145
- 229920002635 polyurethane Polymers 0.000 claims abstract description 141
- 239000002904 solvent Substances 0.000 claims abstract description 69
- 150000005846 sugar alcohols Polymers 0.000 claims abstract description 69
- 239000000654 additive Substances 0.000 claims abstract description 66
- 230000000996 additive effect Effects 0.000 claims abstract description 66
- 239000012948 isocyanate Substances 0.000 claims abstract description 65
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 61
- 239000004970 Chain extender Substances 0.000 claims abstract description 60
- 239000003054 catalyst Substances 0.000 claims abstract description 60
- 239000002994 raw material Substances 0.000 claims abstract description 38
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 90
- -1 silver ions Chemical class 0.000 claims description 77
- 238000002360 preparation method Methods 0.000 claims description 70
- 239000000178 monomer Substances 0.000 claims description 63
- 229920000642 polymer Polymers 0.000 claims description 52
- 238000006243 chemical reaction Methods 0.000 claims description 48
- 238000009987 spinning Methods 0.000 claims description 27
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 23
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 20
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
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- 238000000034 method Methods 0.000 claims description 16
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- 239000000543 intermediate Substances 0.000 claims description 13
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- 238000001704 evaporation Methods 0.000 claims description 12
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- 239000000047 product Substances 0.000 claims description 11
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- 150000002148 esters Chemical class 0.000 claims description 10
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 10
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 9
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 9
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- 239000000843 powder Substances 0.000 claims description 9
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- HXMVNCMPQGPRLN-UHFFFAOYSA-N 2-hydroxyputrescine Chemical compound NCCC(O)CN HXMVNCMPQGPRLN-UHFFFAOYSA-N 0.000 claims description 8
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- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 8
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- 239000005457 ice water Substances 0.000 claims description 6
- UUIQMZJEGPQKFD-UHFFFAOYSA-N n-butyric acid methyl ester Natural products CCCC(=O)OC UUIQMZJEGPQKFD-UHFFFAOYSA-N 0.000 claims description 6
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- YKNYRRVISWJDSR-UHFFFAOYSA-N methyl oxirane-2-carboxylate Chemical class COC(=O)C1CO1 YKNYRRVISWJDSR-UHFFFAOYSA-N 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
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- 229940126680 traditional chinese medicines Drugs 0.000 description 91
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- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 26
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- 238000005516 engineering process Methods 0.000 description 23
- 150000003077 polyols Chemical class 0.000 description 20
- WBRYLZHYOFBTPD-PEPZGXQESA-N (nz)-n-[(4z)-4-hydroxyiminopentan-2-ylidene]hydroxylamine Chemical compound O/N=C(/C)C\C(C)=N/O WBRYLZHYOFBTPD-PEPZGXQESA-N 0.000 description 19
- 239000004814 polyurethane Substances 0.000 description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 13
- 230000000844 anti-bacterial effect Effects 0.000 description 13
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 12
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- GTACSIONMHMRPD-UHFFFAOYSA-N 2-[4-[2-(benzenesulfonamido)ethylsulfanyl]-2,6-difluorophenoxy]acetamide Chemical compound C1=C(F)C(OCC(=O)N)=C(F)C=C1SCCNS(=O)(=O)C1=CC=CC=C1 GTACSIONMHMRPD-UHFFFAOYSA-N 0.000 description 4
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- 150000001412 amines Chemical class 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- XLJMAIOERFSOGZ-UHFFFAOYSA-N anhydrous cyanic acid Natural products OC#N XLJMAIOERFSOGZ-UHFFFAOYSA-N 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
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- 239000012752 auxiliary agent Substances 0.000 description 1
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- 230000009286 beneficial effect Effects 0.000 description 1
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- 229940106691 bisphenol a Drugs 0.000 description 1
- OHJMTUPIZMNBFR-UHFFFAOYSA-N biuret Chemical class NC(=O)NC(N)=O OHJMTUPIZMNBFR-UHFFFAOYSA-N 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000009954 braiding Methods 0.000 description 1
- BMRWNKZVCUKKSR-UHFFFAOYSA-N butane-1,2-diol Chemical class CCC(O)CO BMRWNKZVCUKKSR-UHFFFAOYSA-N 0.000 description 1
- IAQRGUVFOMOMEM-UHFFFAOYSA-N butene Natural products CC=CC IAQRGUVFOMOMEM-UHFFFAOYSA-N 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 150000004657 carbamic acid derivatives Chemical class 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000002512 chemotherapy Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
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- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 235000019864 coconut oil Nutrition 0.000 description 1
- 239000003240 coconut oil Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- XLJMAIOERFSOGZ-UHFFFAOYSA-M cyanate Chemical compound [O-]C#N XLJMAIOERFSOGZ-UHFFFAOYSA-M 0.000 description 1
- KQWGXHWJMSMDJJ-UHFFFAOYSA-N cyclohexyl isocyanate Chemical compound O=C=NC1CCCCC1 KQWGXHWJMSMDJJ-UHFFFAOYSA-N 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 208000025729 dengue disease Diseases 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- JXCHMDATRWUOAP-UHFFFAOYSA-N diisocyanatomethylbenzene Chemical compound O=C=NC(N=C=O)C1=CC=CC=C1 JXCHMDATRWUOAP-UHFFFAOYSA-N 0.000 description 1
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 229940031098 ethanolamine Drugs 0.000 description 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
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- 150000003944 halohydrins Chemical class 0.000 description 1
- 208000006454 hepatitis Diseases 0.000 description 1
- 231100000283 hepatitis Toxicity 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 208000013403 hyperactivity Diseases 0.000 description 1
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- 239000012535 impurity Substances 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
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- 125000001261 isocyanato group Chemical group *N=C=O 0.000 description 1
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical group OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 description 1
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 description 1
- 238000009940 knitting Methods 0.000 description 1
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- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000001717 pathogenic effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
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- 229920001223 polyethylene glycol Polymers 0.000 description 1
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- 239000000344 soap Substances 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
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- 239000003381 stabilizer Substances 0.000 description 1
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- PXQLVRUNWNTZOS-UHFFFAOYSA-N sulfanyl Chemical class [SH] PXQLVRUNWNTZOS-UHFFFAOYSA-N 0.000 description 1
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- KJAMZCVTJDTESW-UHFFFAOYSA-N tiracizine Chemical compound C1CC2=CC=CC=C2N(C(=O)CN(C)C)C2=CC(NC(=O)OCC)=CC=C21 KJAMZCVTJDTESW-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The present invention relates to field of functional materials, and in particular to antimicrobial fabric and its production method with nano silver particles.A kind of functional poly carbamate fibre, the preparing raw material of the functional poly carbamate fibre, in parts by weight, is comprised at least：Polyalcohol 30~55, isocyanates 8~25, chain extender 1~4, nano silver additive 0.1~1.5, catalyst 0.1~0.8, solvent 70~110.
Description
Technical field
The present invention relates to field of functional materials, and in particular to the antimicrobial fabric with nano silver particles and its life
Production method.
Background technology
Nature material circulate growth and decline during, the presence of microorganism is extremely wide, have in these microorganisms bacterium,
Virus, fungi and algae etc..Because textile is an important medium for transmission germ, so people in daily life can not
Touch various microorganisms with can avoiding.Generally, the harm of our imperceptible pathogenic bacteria, but work as condition
When suitable, pathogenic bacteria on human body skin will amount reproduction, and by skin, respiratory tract, alimentary canal and blood to human body
One of the main reason for health causes greatly to endanger, and this is pathogenic.Especially bacterium, substantial amounts, serious threat the mankind
Health.Worldwide including cholera, pneumonia, malaria, tuberculosis and hepatitis etc. because of caused by bacterial infection causes the mankind
Dead event occurs again and again, allows people to talk bacterium discoloration.The coli-infection event of Japanese large area outburst from 1996, so far
Allow the epidemic diseases such as the terrified dengue fever of people, Hemorrhagic fever, to SARS, invariably to we demonstrate that：Good habits and customs, ring
The living environment of health care health and strong fitness, it is only and resists harmful microorganism infringement most efficient method.Bacterium is nowhere
Do not exist, even the clothes of wash clean, after putting on several hours, bacterium every square centimeter can reach more than one hundred million.The whole world it is annual because
Bacterium infection causes the number of death to account for more than the 30% of dead sum close to 20,000,000；The intersection infection of each hospital
Then more than 10%, therefore antibacterial is the vital task that people ensure health all the time." antibacterial " definition of broad sense is very extensive, including
Sterilization, antibacterial, sterilization and fungi-proofing a variety of implications, the antibacterial in textile generally refer to antibacterial or sterilization.
With the progress of society and developing rapidly for economy, people start to pursue the life in comfortable living space and health
Mode, higher quality requirement is proposed to environment and health；Simultaneously as excessive exploitation of the mankind to environment, causes ring
The destruction and pollution in border, various bacteriums and new virus, which are propagated, wreaks havoc so that all kinds of antiseptics and anti-biotic material medicine equipment,
The application in the fields such as household supplies, household electrical appliance, packaging for foodstuff receives more and more extensive concern.Antibacterial fiber product and people
The life of class is closely bound up, and no matter in clothes or medical field, requirement of the people to fibre has been not only endurable resistance to
With, it is also desirable to there can be some specific functions (such as antibiotic property) to adapt to the requirement of social development.This gives antibacterial fiber product
Development provide power and wide space.
Silver just has antibacterial characteristics since ancient times, and Nano Silver is even more that anti-microbial property is improved into several times.Arranged through Nano Silver
Fibrous material be generally configured with excellent anti-microbial property, can be widely applied to health care, health care underwear, house ornamentation building, environment
The fields such as protection.Such as the CLEANCOOL products of emerging promise production, Argent grain has been adsorbed in its fiber, applied to underwear and gym suit
In, possess permanent antibiotic property；Such as the Foss fiber that Foss is produced, silver-containing inorganic Wessalith CS gION is embedded in polyester bicomponent
Fiber, applied to antibiotic cleaning cloth, it can be cleaned multiple times, bleach；Such as the Nai Er Nano silver solutions that Nai Er is produced, netted cotton is arrived in arrangement
On gauze, applied to medical antibacterial dressing, there is excellent efficient antibiotic property and promote wound healing.
Actually rare on carrying the research report of silver fiber at present, it is common that research object also typically concentrates on cotton, viscose glue etc.
General fibre.However, with the continuous improvement that people are required quality of the life, the application of various different performance fibrous materials
It is more and more common.Nano Silver open soon Expand Thinking, should be applied to multiple fiber material by researcher, realized and carried silver fibre
The variation of dimension.
The content of the invention
In order to solve the above-mentioned technical problem, it is fine to provide a kind of functional poly carbamate for the first aspect of the invention
Dimension, the preparing raw material of the functional poly carbamate fibre, in parts by weight, is comprised at least：Polyalcohol 30~55, isocyanide
Acid esters 8~25, chain extender 1~4, nano silver additive 0.1~1.5, catalyst 0.1~0.8, solvent 70~110.
As a kind of preferable technical scheme of the present invention, the preparing raw material of the functional poly carbamate fibre is also wrapped
Include binary oxime；The binary oxime is binary ketoxime；The binary ketoxime is selected from：2,4- pentanes dione dioxime, 1,2- cyclohexanediones
Dioxime, 5,5- dimethyl -1,3- cyclohexanedione dioximes, 1,4- benzoquinones dioxime, 4- methyl isophthalic acids, in 2- cyclohexanedione dioximes
It is one or more.
As a kind of preferable technical scheme of the present invention, the binary ketoxime is 2,4- pentane dione dioximes.
As a kind of preferable technical scheme of the present invention, the nano silver additive includes protective agent and nano silver particles；
The protective agent is dissaving polymer；The end group of the dissaving polymer is at least one of hydroxyl, sulfydryl, amino.
As a kind of preferable technical scheme of the present invention, the preparing raw material of the dissaving polymer comprises at least the first work(
Can monomer, the second function monomer, catalyst, solvent.
As a kind of preferable technical scheme of the present invention, first function monomer is selected from 3,4- epoxies methyl butyrate, third
Olefin(e) acid -2,3- polyglycidyls, oxirane -2- carboxylate methyl esters, 4- (2- Oxiranylmethoxies) butyl propyleneglycol acid esters, 4-
(2- Oxyranyles)-methyl phenylpropionate, methyl acrylate, one kind in 4,5- epoxy -2- glycidyl methyl valerates or
It is a variety of.
As a kind of preferable technical scheme of the present invention, second function monomer is selected from diethanol amine, ethoxy second two
One or more in amine, diethylenetriamine, 3- amino-N- (2- mercaptoethyls) propionamide.
As a kind of preferable technical scheme of the present invention, the preparation method of the nano silver additive comprises at least following step
Suddenly：
(1) the second function monomer is added in container in the case where being passed through nitrogen, and is stirred under ice-water bath
(2) methanol solution with the first function monomer of the second function monomer equimolar amounts is added dropwise, and system is moved on into room
Stirred under warm environment 2~6 hours, be then concentrated by evaporation and obtain intermediate；
(3) system is warming up to 100~150 DEG C, adds p-methyl benzenesulfonic acid, stirred lower reaction 2~6 hours, be concentrated by evaporation
Obtain the dissaving polymer；
(4) silver nitrate powder is dissolved in DMSO under normal temperature, and adds the dissaving polymer that the 3rd step obtains, control
The amount of silver nitrate powder and dissaving polymer, the concentration for making dissaving polymer are 0.1g/mL, concentration of silver ions 0.01g/
ML, 30~60min is stirred, and 0.1~0.5ml reducing agents are added dropwise again, 30~120min of reaction can obtain the Nano Silver and add
Add agent.
The second aspect of the invention provides the preparation method of functional poly carbamate fibre, including at least as follows
Step：
(1) preparing raw material of functional poly carbamate fibre is weighed by defined parts by weight, and is being passed through nitrogen
In the case of polyalcohol, isocyanates, catalyst are added in reactor, controlling reaction temperature at 70~80 DEG C, reaction 2~4
Hour, polyurethane prepolymer；
(2) in a solvent, chain extender is then added dropwise in the prepolymer dissolving obtained the first step, and stirring reaction 10~
30min, controlling the dosage of solvent makes the concentration of the reaction product in system be 30~35wt%；
(3) nano silver additive is added dropwise in the system obtained toward second step, 30~45min of stirring reaction, obtains functionalization
Polyurethanes spinning solution；
(4) the functional poly carbamate spinning solution for obtaining the 3rd step filters deaeration, using dry spinning method, system
It is standby to obtain functional poly carbamate fibre.
The third aspect of the invention provides a kind of antimicrobial fabric with nano silver particles, described antimicrobial
Fabric is formed by functional poly carbamate fibre and chitin fiber mixed weaving.
As a kind of preferable technical scheme of the present invention, the functional poly carbamate fibre and chitin fiber
Mixed weaving mode is, using functional poly carbamate fibre as warp, is woven by parallel of chitin fiber；The warp
Tension force ratio with parallel is 5：1.
The fourth aspect of the invention provides the application of the antimicrobial fabric with nano silver particles, can be applied to cure
With uniform, underwear for men and women, feminine hygiene products field.
The above-mentioned of the application and other features, aspect and advantage is more readily understood with reference to described further below.
Beneficial effect：The unexpected discovery of the present inventor, it is provided by the invention antimicrobial with nano silver particles
Fabric has good fungistatic effect compared with existing fabric, while also has good ultimate strength, elongation at break, can
Meet the application in medical garments, underwear for men and women, feminine hygiene products field；In addition should anti-micro- life with nano silver particles
Thing fabric has certain degradability, it is possible to reduce waste pollution environment.Moreover, not image surface coating or electrosilvering
Silver is lost in clothes after the washing, the antimicrobial fabric provided by the invention with nano silver particles, can keep antibacterial for a long time
Effect.
Embodiment
Participate in the election of the detailed description of the invention below for being preferable to carry out method and including embodiment this hair can be more easily understood
Bright content.Unless otherwise defined, all technologies used herein and scientific terminology have common with art of the present invention
The identical implication that technical staff is generally understood that.When contradiction be present, the definition in this specification is defined.
As used herein term " by ... prepare " it is synonymous with "comprising".Term "comprising" used herein, " comprising ",
" having ", " containing " or its any other deformation, it is intended that cover including for non-exclusionism.For example, the combination comprising listed elements
Thing, step, method, product or device are not necessarily limited to those key elements, but can include not expressly listed other key elements or
Such a composition, step, method, product or the intrinsic key element of device.
Conjunction " Consists of " excludes any key element do not pointed out, step or component.If be used in claim, this
Phrase will make claim be closed, it is not included the material in addition to the material of those descriptions, but relative normal
Except rule impurity.When being rather than immediately following in the clause that phrase " Consists of " appears in claim main body after theme,
It is only limited to the key element described in the clause；Other key elements are not excluded outside the claim as entirety.
Equivalent, concentration or other values or parameter are excellent with scope, preferred scope or a series of upper limit preferred values and lower limit
During the Range Representation that choosing value limits, this, which is appreciated that, specifically discloses by any range limit or preferred value and any scope
All scopes that any pairing of lower limit or preferred value is formed, regardless of whether the scope separately discloses.For example, when open
During scope " 1 to 5 ", described scope should be interpreted as including scope " 1 to 4 ", " 1 to 3 ", " 1 to 2 ", " 1 to 2 and 4 to
5 ", " 1 to 3 and 5 " etc..When number range is described herein, unless otherwise indicated, otherwise the scope is intended to include its end
Value and all integers and fraction within the range.
Singulative includes plural number and object is discussed, unless the context clearly dictates otherwise." optional " or it is " any
It is a kind of " refer to that the item that describes thereafter or event may or may not occur, and the description include situation that event occurs and
The situation that event does not occur.
Approximate term in specification and claims is used for modifying quantity, and it is specific to represent that the present invention is not limited to this
Quantity, include the part of the amendment of the acceptable change without cause related basic function close to the quantity.Phase
Answer, modify a numerical value with " about ", " about " etc., mean that the invention is not restricted to the exact numerical.It is approximate in some examples
Term likely corresponds to the precision of the instrument of measured value.In present specification and claims, scope limits can be with
Combine and/or exchange, these scopes include all subranges contained therebetween if not stated otherwise.
In addition, indefinite article " one kind " before key element of the present invention or component and "one" to key element or the quantitative requirement of component
(i.e. occurrence number) unrestriction.Therefore "one" or " one kind " should be read as including one or at least one, and odd number
The key element or component of form also include plural form, unless the obvious purport of the quantity refers to singulative.
" polymer " means by the polymerizable compound prepared by the monomer that polymerize identical or different type.Generic term
" polymer " includes term " homopolymer ", " copolymer ", " terpolymer " and " EVA ".
In order to solve the above-mentioned technical problem, it is fine to provide a kind of functional poly carbamate for the first aspect of the invention
Dimension, the preparing raw material of the functional poly carbamate fibre, in parts by weight, is comprised at least：Polyalcohol 30~55, isocyanide
Acid esters 8~25, chain extender 1~4, nano silver additive 0.1~1.5, catalyst 0.1~0.8, solvent 70~110.
In the present invention, the polyalcohol is not particularly limited, and can be small molecule polyol, such as：Ethylene glycol, third
Glycol, 1,3-PD, BDO, 1,3-BDO, 1,2- butanediols, 1,5-PD, 1,6- hexylene glycols, new penta 2
Alcohol, alkane (7~22) glycol, diethylene glycol (DEG), triethylene glycol, dipropylene glycol, 3- methyl isophthalic acids, 5- pentanediols, alkane -1,2- glycol (C17
~20), 1,3- or 1,4-CHDM and their mixture, Isosorbide-5-Nitrae-cyclohexanediol, hydrogenated bisphenol A, Isosorbide-5-Nitrae-dihydroxy-
The dihydric alcohols such as 2- butylene, 2,6- dimethyl -1- octenes -3,8- glycol, bisphenol-A；Can also be polymer polyatomic alcohol, for example, poly-
Ethoxylated polyhydric alcohol, PEPA, polycarbonate polyol, polyurethane polyol, epoxy polyol, vegetable oil polyol, polyene
Hydrocarbon polyalcohol, acrylic polyol and vinyl monomer modified polyalcohol.
As PPG, such as polypropylene glycol, polytetramethylene ether diol etc. can be enumerated.
As PEPA, such as it can enumerate and make above-mentioned low molecular weight polyols (preferably binary under the conditions of known
Alcohol) with polynary acid reaction obtained by condensation polymer.
As polycarbonate polyol, such as can enumerate using above-mentioned low molecular weight polyols (preferably dihydric alcohol) as drawing
Send out agent ethylene carbonate ring-opening polymerization polymer, and will such as BDO, 1,5-PD, 3- methyl isophthalic acids, 5- penta 2
The dihydric alcohol such as alcohol or 1,6- hexylene glycol is copolymerized amorphous poly carbonate polyol of gained etc. with ring-opening polymerization polymer.
In addition, polyurethane polyol can be as obtained by will be above-mentioned PEPA, PPG and/or poly- carbonic acid
Ester polyol (is contained with hydroxyl relative to ratio of the equivalent proportion (OH/NCO) of NCO more than 1 with above-mentioned polyisocyanates
There is Isosorbide-5-Nitrae-bis- (isocyanatomethyls) hexamethylene.Reaction same as below, it is polynary as polyester polyurethane polyol, polyether-polyurethane
Alcohol, polycarbonate polyurethane polyalcohol or polyester polyether-polyurethane polyalcohol etc. are obtained.
As epoxy polyol, such as can enumerate by above-mentioned low molecular weight polyols and such as epichlorohydrin, Beta-methyl
The multifunctional halohydrin such as epichlorohydrin reacts obtained epoxy polyol.
As vegetable oil polyol, such as vegetable oil containing hydroxyl such as castor oil, coconut oil etc. can be enumerated.Such as can
It is polynary to enumerate castor oil polyhydric alcohol or ester modified castor oil as obtained by castor oil polyhydric alcohol with polypropylene polyol reaction
Alcohol etc..
As polyolefin polyhydric alcohol, such as polyvinyl alcohol, polyethylene glycol, polybutadiene polyol, part soap can be enumerated
Change vinyl-vinyl acetate copolymer etc..
As acrylic polyol, for example, can enumerate by make acrylate with hydroxyl and can with hydroxyl
Copolymer obtained from the copolymerizable vinyl monomer copolymerization of the acrylic ester copolymer of base.
In a preferred embodiment, the polyalcohol is selected from：PPG, PEPA, makrolon
It is any in polyalcohol, polyurethane polyol, epoxy polyol, vegetable oil polyol, polyolefin polyhydric alcohol, acrylic polyol
One or more of mixing.
In a preferred embodiment, the polyalcohol is polytetramethylene ether diol.
In a preferred embodiment, the equal molecular mass of the number of the polytetramethylene ether diol is 2000.
In the present invention, the isocyanates is not particularly limited, and what can be enumerated has：Aliphatic diisocyanate,
Alicyclic diisocyanate, aromatic diisocyanate, aliphatic triisocyanate, polyisocyanates etc..
As aliphatic diisocyanate, such as trimethylene diisocyanate, tetramethylene diisocyanate, Asia can be enumerated
Amyl group diisocyanate, 1, hexamethylene-diisocyanate, 1,2- trimethylene diisocyanates, 1,2- tetramethylene diisocyanates, 2,
3- tetramethylene diisocyanates, 1,3- tetramethylene diisocyanates, 2,4,4- or 2,2,4- trimethyls 1, hexamethylene-diisocyanate,
2,6- bis- isocyanate group methyl caproates etc..
As the example of alicyclic diisocyanate, 1,3- pentamethylene diisocyanate, Isosorbide-5-Nitrae-hexamethylene can be included
Diisocyanate, 1,3- cyclohexane diisocyanates, 3- isocyanatomethyls -3,5,5- tri-methyl cyclohexane diisocyanates are (not
Name：IPDI), 4,4 '-methylene two (cyclohexyl isocyanate), the isocyanic acid of methyl -2,4- hexamethylene two
Double (isocyanatomethyl) hexamethylenes of ester, methyl -2,6- cyclohexane diisocyanate, 1,3-, 1,3- are double (ethyl isocyanate base)
Hexamethylene, Isosorbide-5-Nitrae-bis- (ethyl isocyanate bases) hexamethylene, 2,5- or 2,6- bis- (isocyanatomethyl) norbornane (NBDI) and
Its mixture etc..
As the example of aromatic diisocyanate, can include：2,4- toluene di-isocyanate(TDI)s and 2,6- toluene two
The isomer mixture of isocyanates and the toluene di-isocyanate(TDI), 4,4 '-'-diphenylmethane diisocyanate, 2,4 '-two
Phenylmethane diisocyanate and 2,2 '-'-diphenylmethane diisocyanate and the '-diphenylmethane diisocyanate it is arbitrary
Isomer mixture, toluene di-isocyanate(TDI), to phenylene diisocyanate, naphthalene diisocyanate etc..
As the example of aliphatic triisocyanate, 1,3,6- triisocyanate methyl hexanes etc. can be included.
As polyisocyanates, poly methylene poly phenyl poly isocyanate can be included, by above-mentioned diisocyanate
Polyisocyanates derived from compound.As the polyisocyanates as derived from above-mentioned diisocyanate, there is isocyanuric acid esters polyisocyanate
Cyanate, biuret class polyisocyanates, carbamates polyisocyanates, allophanic acid esters polyisocyanates, carbon two
Acid imide polyisocyanates etc..
In a preferred embodiment, the isocyanates is the arbitrary isomers of '-diphenylmethane diisocyanate
Mixture.
In the present invention, the chain extender is not particularly limited, and can be ethylene glycol, 1,3-PD, Isosorbide-5-Nitrae-fourth two
Alcohol, ethylenediamine, propane diamine, diglycol, glycerine, trimethylolpropane, hydrogenation double A, diethanol amine, three ethanol
Amine, diethyl toluene diamine.
In a preferred embodiment, the chain extender is propane diamine.
In the present invention, the catalyst is organic tin catalyst, including but not limited to dibutyl tin laurate.
Dibutyl tin laurate is a kind of organotin additive, can be dissolved in benzene, toluene, carbon tetrachloride, ethyl acetate, chlorine
Organic solvent and all industrial plasticizer such as imitative, acetone, petroleum ether.The higher boiling multipurpose organotin catalysts to circulate on the market
Dibutyl tin laurate is handled by special liquefaction, is light yellow under normal temperature or colourless oil liquid, low temperature
Into white crystalline body, available for igelite auxiliary agent, there is excellent lubricity, transparent, weatherability.Halophile pollutes
Preferably.The used as stabilizers in soft transparent product, make highly-efficient lubricant in hard transparent product, also act as acrylate rubber
The catalyst of glue and carboxylic rubber cross-linking reaction, polyurethane foam plastics synthesis and polyester synthesis, room temperature vulcanized silicone rubber catalysis
Agent.
Dibutyl tin laurate in the present invention is as catalyst, catalysis NCO and hydroxyl, amino groups
Between reaction.
The preparing raw material of heretofore described functional poly carbamate fibre also includes binary oxime.
The organic compound that oxime (oxime) is the aldehyde containing carbonyl, ketone compounds and azanol effect and is generated, formula
All there is C=NOH groups.The oxime obtained by aldehyde reaction claims aldoxime, and the oxime obtained by reactive ketone claims ketoxime, and oxime can obtain through hydrolysis
To original aldehydes or ketones.Binary oxime is the oxime compound containing two C=NOH groups in structure.
In a preferred embodiment, the binary oxime is binary ketoxime.
In a preferred embodiment, the binary ketoxime is selected from：2,4- pentanes dione dioxime, 1,2- cyclohexanediones
Dioxime, 5,5- dimethyl -1,3- cyclohexanedione dioximes, 1,4- benzoquinones dioxime, 4- methyl isophthalic acids, in 2- cyclohexanedione dioximes
It is one or more.
In a preferred embodiment, the binary oxime is 2,4- pentane dione dioximes.
A part of binary oxime is introduced in the present invention, is reacted instead of polyalcohol and isocyanates so that the function of finally giving
There is invertibity in the bonding and fracture for changing chemical bond in the strand of polyurethane fibre, this is due to a certain extent
Oxime ammonia ester bond is broken under the conditions of certain temperature, ultraviolet lighting etc., and removes these conditions and isocyanates bond
Bonding.This is advantageous to the degraded of the functional poly carbamate fibre fabric, this kind fabric is returned to a certain extent
Receive and utilize.
Nano silver additive in the present invention is to include protective agent and nano silver particles.Because Nano Silver particle diameter is small, have
The characteristics such as skin effect, quantum size effect, surface electrostatic effect is strong, is easy to reunite, the bad dispersibility in solvent or solution,
Therefore need to improve the dispersiveness of nano silver particles using protective agent, therefore the nano silver additive in the present invention includes protection
Agent and nano silver particles.
In a preferred embodiment, the protective agent is dissaving polymer；The end of the dissaving polymer
Base is at least one of hydroxyl, sulfydryl, amino.
Contain substantial amounts of cavity inside dissaving polymer in the present invention, and flank attack contains carbonyl, tertiary amine groups, hydroxyl etc.
Active group, these groups can capture the anion in solution by complexing, so as to make Argent grain former in spinning
Disperse well in liquid.The preparing raw material of dissaving polymer in the present invention comprises at least the first function monomer, the second function
Monomer, catalyst, solvent.
In a preferred embodiment, first function monomer is selected from 3,4- epoxies methyl butyrate, acrylic acid -2,
3- polyglycidyls, oxirane -2- carboxylate methyl esters, 4- (2- Oxiranylmethoxies) butyl propyleneglycol acid esters, 4- (2- epoxy second
Alkyl)-methyl phenylpropionate, methyl acrylate, the one or more in 4,5- epoxy -2- glycidyl methyl valerates.
When containing epoxide group in the first function monomer hydroxyl, therefore obtained centre are generated with the reaction of the second function monomer
Contain three active groups and ester group in body, these intermediates at high temperature polycondensation when the dissaving polymer that is formed formed
Cavity size it is small.It is also small that silver ion is reduced the crystal particle diameter to be formed in the cavity, is distributed to functional poly carbamic acid
Good antimicrobial effect after in ester fiber.In addition, in some the first function monomers (such as 4- (2- Oxiranylmethoxies) butyl third
Olefin(e) acid ester) strand is long, and contains ehter bond, and it is flexible big, when being second comonomer reaction generation dissaving polymer
The cavity of formation is bigger, and the size that silver ion is formed after being reduced is larger, and fungistatic effect is relatively weak.
In a preferred embodiment, second function monomer is selected from diethanol amine, AEEA, diethyl
One or more in alkene triamine, 3- amino-N- (2- mercaptoethyls) propionamide.
When containing hydroxyl and amino (such as AEEA) in the second function monomer structure simultaneously, or contain simultaneously
When sulfydryl and amino (such as 3- amino-N- (2- mercaptoethyls) propionamide), because its cloud density is different, cause itself and the
The reactivity of one function monomer is different, is reacted when reaction generates super branched polyurethane and first occurs at the high functional group of activity
Position, the degree of branching of dissaving polymer is also caused to reduce, the cavity structure size of formation is small, influences fungistatic effect.In addition, the
Active group hyperactivity on two function monomers, also cause the crosslinking of dissaving polymer, form the elasticity insoluble in solvent
Body, it is impossible to be distributed in functional poly carbamate spinning solution, even and if can dissolve, can also spin polyurethanes
The viscosity of silk stock solution is too high, influences its processing technology.
In a preferred embodiment, the preparation method of the nano silver additive comprises at least following steps：
(1) the second function monomer is added in container in the case where being passed through nitrogen, and is stirred under ice-water bath
(2) methanol solution with the first function monomer of the second function monomer equimolar amounts is added dropwise, and system is moved on into room
Stirred under warm environment 2~6 hours, be then concentrated by evaporation and obtain intermediate；
(3) system is warming up to 100~150 DEG C, adds p-methyl benzenesulfonic acid, stirred lower reaction 2~6 hours, be concentrated by evaporation
Obtain the dissaving polymer；
(4) silver nitrate powder is dissolved in DMSO under normal temperature, and adds the dissaving polymer that the 3rd step obtains, control
The amount of silver nitrate powder and dissaving polymer, the concentration for making dissaving polymer are 0.1g/mL, concentration of silver ions 0.01g/
ML, 30~60min is stirred, and 0.1~0.5ml reducing agents are added dropwise again, 30~120min of reaction can obtain the Nano Silver and add
Add agent.
In the present invention, the first function monomer and the second function monomer react in the preparation process of dissaving polymer
To intermediate, amino and imino group during this in the second function monomer have compatibility because cloud density is big, can be with
Ring-opening reaction occurs for the epoxide group or vinyl of the first function monomer.When the first function monomer epoxide group or vinyl with
One end is obtained when imino group reacts has ester group, and the other end has two active groups (two in amino, hydroxyl, sulfydryl
It is individual) intermediate；And when the epoxide group or the amino or sulfydryl of vinyl and the second function monomer of the first function monomer occur
During reaction, obtaining one end and contain ester group, amino or hydroxyl, sulfydryl are contained in two one end, and in middle linear also containing imino group
Mesosome, thus in the present invention in the building-up process of dissaving polymer because selection the first and second function monomers difference, institute
Obtained intermediate structure is also different, and these intermediates are likely to be formed during the course of the reaction, is a mixture system.
And when the temperature of system rises to 100~~150 DEG C when, due between amino, sulfydryl or hydroxyl and ester group between these intermediates
Condensation reaction and form the wide dissaving polymer of molecular weight distribution.
The DMSO solution of silver nitrate is added in dissaving polymer, makes its mixed dissolution, silver ion quickly with hyperbranched poly
Amino, hydroxyl, sulfydryl isoreactivity group in compound are complexed, and are distributed in the cavity of dissaving polymer.And work as and be somebody's turn to do
When material (such as sodium borohydride etc.) with reproducibility being added dropwise in system, it is brilliant that the silver ion in system is reduced into silver-colored simple substance
Body, and because the cavity size of dissaving polymer is certain, it is possible to regulate and control the size of silver-colored elemental crystal with this, obtain
The Argent grain of different size size.At the same time, can also solve the problems, such as silver-colored bad dispersibility.
In addition not only have in the intermediate that the functional group reactionses of epoxide epoxy group group of the present invention and the second function monomer obtain
The groups such as the original hydroxyl of the second function monomer, amino, sulfydryl and the original ester group of the first function monomer, go back epoxide group open loop
A newly-generated hydroxyl, because the hydroxyl is located on main chain, do not lie on end group, therefore activity is relative to the active weak of end group,
It is big in the possibility for occurring to remain during condensation reaction, therefore obtained dissaving polymer end group is amino, hydroxyl or mercapto
Base, and also have hydroxyl on its side chain, it is scattered in functional poly carbamate fibre spinning solution to be advantageous to Argent grain
Property and the adhesive force to spinning solution strand, improve the resistance to jail property of Argent grain.
The second aspect of the invention provides the preparation method of functional poly carbamate fibre, including at least as follows
Step：
(1) preparing raw material of functional poly carbamate fibre is weighed by defined parts by weight, and is being passed through nitrogen
In the case of polyalcohol, isocyanates, catalyst are added in reactor, controlling reaction temperature at 70~80 DEG C, reaction 2~4
Hour, polyurethane prepolymer；
(2) in a solvent, chain extender is then added dropwise in the prepolymer dissolving obtained the first step, and stirring reaction 10~
30min, controlling the dosage of solvent makes the concentration of the reaction product in system be 30~35wt%；
(3) nano silver additive is added dropwise in the system obtained toward second step, 30~45min of stirring reaction, obtains functionalization
Polyurethanes spinning solution；
(4) the functional poly carbamate spinning solution for obtaining the 3rd step filters deaeration, using dry spinning method, system
It is standby to obtain functional poly carbamate fibre.
In the present invention, when preparing functional poly carbamate fibre spinning solution, using excess isocyanates with
Polyol reaction obtains the polyester-urethane prepolymer that end group is isocyanates, adds the molecule that chain extender improves polymer
Amount, control the amount of chain extender to make to obtain in spinning solution and retain a certain amount of unreacted NCO, add Nano Silver and add
End group reaction in isocyanates and protective agent when adding agent blended in spinning solution, makes protective agent be connected with Argent grain
Into polyurethanes spinning solution so that Argent grain is uniformly dispersed in spinning solution, and with the effect of spinning solution
Power is sufficiently strong, is not easy to be desorbed.
Further, since the hydroxyl that the epoxide group open loop of the first function monomer generates during dissaving polymer is prepared
Hydrogen bond can be formed with the ammonia ester bond on polyurethanes strand, improve the concentration of spinning solution so that finally give
Functional poly carbamate fibre elasticity and intensity are improved.Moreover, the over-expense in nano silver additive in the present invention
Fluidized polymer protective agent plays a part of chain extender, can be with the remaining isocyanates in polyurethane fibre spinning solution
Base is reacted, and makes a certain degree of crosslinking of System forming, and the elastic and strong of fiber can be improved while spinning parameter is not influenceed
Degree.
The third aspect of the invention provides a kind of antimicrobial fabric with nano silver particles, described antimicrobial
Fabric is formed by functional poly carbamate fibre and chitin fiber mixed weaving.
In a preferred embodiment, the mixing of the functional poly carbamate fibre and chitin fiber is compiled
The mode of knitting is, using functional poly carbamate fibre as warp, is woven by parallel of chitin fiber；The warp and parallel
Tension force ratio be 5：1.
There is longitudinal stripe on chitin fiber surface, while wet spinning causes fiber surface has irregular holes.This
The fine small structure of kind, can form capillary effect, can absorb the sweat of human body surface and spread out rapidly, thus
It is not easy breed bacteria so that chitin fiber possesses certain antibacterial effect.
Functional poly carbamate fibre and chitin fiber are with 5 in the present invention：1 tension force carries out shuffling, is knitted
Thing is not only antimicrobial, good anti-bacterial effect, and with elasticity, pliability and comfort sense well.Mixed using different tension force
Compile, the good elasticity of functional poly carbamate fibre is not affected because of the bad elasticity of chitin fiber, it is resulting
Fabric property more preferably.
The fourth aspect of the invention provides the application of the antimicrobial fabric with nano silver particles, can be applied to cure
With uniform, underwear for men and women, feminine hygiene products field.
The present invention is specifically described below by embodiment.It is necessarily pointed out that following examples are only used
In the invention will be further described, it is impossible to be interpreted as limiting the scope of the invention, professional and technical personnel in the field
Some the nonessential modifications and adaptations made according to the content of the invention described above, still fall within protection scope of the present invention.
In addition, same materials specification used in embodiment, source etc. are identical, if without other explanations, original used
Material is all commercially available, is purchased from traditional Chinese medicines chemical reagent.
Embodiment
Embodiment 1
Embodiment 1 provides a kind of functional poly carbamate fibre, the functional poly carbamate fibre
Preparing raw material, in parts by weight, including：Polyalcohol 30, isocyanates 8, chain extender 1, nano silver additive 0.1, catalyst
0.1st, solvent 70.
The polyalcohol is polytetramethylene ether diol, purchased from traditional Chinese medicines chemical reagent；The isocyanates is diphenylmethyl
Alkane diisocyanate, purchased from traditional Chinese medicines chemical reagent；The chain extender is propane diamine, purchased from traditional Chinese medicines chemical reagent；The catalyst
For dibutyl tin laurate, purchased from traditional Chinese medicines chemical reagent, the solvent is DMSO.
The preparation method of the nano silver additive comprises the following steps：
(1) 0.5mol the second function monomer diethylenetriamine (CAS is added in container in the case where being passed through nitrogen：
111-40-0), and under ice-water bath stir
(2) 0.5mol the first function monomer 3,4- epoxy methyl butyrates (CAS is added dropwise:4509-09-5, purchased from Chemos
GmbH 50ml methanol solutions), and system is moved on to and stirred under room temperature environment 2 hours, then it is concentrated by evaporation and obtains intermediate；
(3) system is warming up to 100 DEG C, adds 0.8g p-methyl benzenesulfonic acid, stir lower reaction 2 hours, evaporation and concentration obtains
The dissaving polymer；
(4) silver nitrate powder is dissolved in DMSO under normal temperature, it is 0.01g/mL to make concentration of silver ions, and adds the 3rd step
Obtained dissaving polymer, the concentration for making dissaving polymer are 0.1g/mL, stir 30min, and 0.1ml boron hydrogen is added dropwise again
Change sodium (CAS：16940-66-2), react 30min and can obtain the nano silver additive.
The preparation method of functional poly carbamate fibre, comprises the following steps：
(1) preparing raw material of functional poly carbamate fibre is weighed by defined parts by weight, and is being passed through nitrogen
In the case of polyalcohol, isocyanates, catalyst are added in reactor, controlling reaction temperature at 70 DEG C, react 2 hours, gather
Urethane prepolymer；
(2) the prepolymer dissolving obtained the first step in a solvent, is then added dropwise chain extender, and stirring reaction 10min, controlled
The dosage of solvent processed makes the concentration of the reaction product in system be 30wt%；
(3) nano silver additive is added dropwise in the system obtained toward second step, stirring reaction 30min, obtains functional poly ammonia
Carbamate spinning solution；
(4) the functional poly carbamate spinning solution for obtaining the 3rd step filters deaeration, using dry spinning method, system
It is standby to obtain functional poly carbamate fibre.
Antimicrobial fabric preparation method with nano silver particles：
The antimicrobial fabric with nano silver particles is warp by functional poly carbamate fibre, with crust
Cellulose fiber weaves for parallel, with 5：1 tension force ratio mixed weaving forms.
Embodiment 2
Embodiment 2 provides a kind of functional poly carbamate fibre, the functional poly carbamate fibre
Preparing raw material, in parts by weight, including：Polyalcohol 55, isocyanates 25, chain extender 4, nano silver additive 1.5, catalyst
0.8th, solvent 110.
The polyalcohol is polytetramethylene ether diol, purchased from traditional Chinese medicines chemical reagent；The isocyanates is diphenylmethyl
Alkane diisocyanate, purchased from traditional Chinese medicines chemical reagent；The chain extender is propane diamine, purchased from traditional Chinese medicines chemical reagent；The catalyst
For dibutyl tin laurate, purchased from traditional Chinese medicines chemical reagent；The solvent is DMSO.
The preparation method of the nano silver additive comprises the following steps：
(1) 0.5mol the second function monomer diethanol amine (CAS is added in container in the case where being passed through nitrogen：111-
42-2), and under ice-water bath stir
(2) 0.5mol the first function monomer 3, the 50ml methanol solutions of 4- epoxy methyl butyrates is added dropwise, and system is moved
Stirred under to room temperature environment 6 hours, be then concentrated by evaporation and obtain intermediate；
(3) system is warming up to 150 DEG C, adds 0.8g p-methyl benzenesulfonic acid (CAS：104-15-4), the lower reaction 6 of stirring is small
When, evaporation and concentration obtains the dissaving polymer；
(4) silver nitrate powder is dissolved in DMSO under normal temperature, it is 0.01g/mL to make concentration of silver ions, and adds the 3rd step
Obtained dissaving polymer, the concentration for making dissaving polymer are 0.1g/mL, stir 60min, and 0.5ml boron hydrogen is added dropwise again
Change sodium, reaction 120min can obtain the nano silver additive.
The preparation method of functional poly carbamate fibre, comprises the following steps：
(1) preparing raw material of functional poly carbamate fibre is weighed by defined parts by weight, and is being passed through nitrogen
In the case of polyalcohol, isocyanates, catalyst are added in reactor, controlling reaction temperature at 80 DEG C, react 2 hours, gather
Urethane prepolymer；
(2) the prepolymer dissolving obtained the first step in a solvent, is then added dropwise chain extender, and stirring reaction 30min, controlled
The dosage of solvent processed makes the concentration of the reaction product in system be 35wt%；
(3) nano silver additive is added dropwise in the system obtained toward second step, stirring reaction 45min, obtains functional poly ammonia
Carbamate spinning solution；
(4) the functional poly carbamate spinning solution for obtaining the 3rd step filters deaeration, using dry spinning method, system
It is standby to obtain functional poly carbamate fibre.
Antimicrobial fabric preparation method with nano silver particles：
The antimicrobial fabric with nano silver particles is warp by functional poly carbamate fibre, with crust
Cellulose fiber weaves for parallel, with 5：1 tension force ratio mixed weaving forms.
Embodiment 3
Embodiment 3 provides a kind of functional poly carbamate fibre, the functional poly carbamate fibre
Preparing raw material, in parts by weight, including：Polyalcohol 40, binary oxime 2, isocyanates 10, chain extender 1.2, nano silver additive
0.8th, catalyst 0.3, solvent 95.
The polyalcohol is polytetramethylene ether diol, purchased from traditional Chinese medicines chemical reagent；The isocyanates is diphenylmethyl
Alkane diisocyanate, purchased from traditional Chinese medicines chemical reagent；The chain extender is propane diamine, purchased from traditional Chinese medicines chemical reagent；The catalyst
For dibutyl tin laurate, purchased from traditional Chinese medicines chemical reagent；The solvent is DMSO；The binary oxime is 2,4- pentanes diketone two
Oxime (CAS：2157-56-4, purchased from Wuhan profit is micro- can Science and Technology Ltd.).
The preparation method of the nano silver additive comprises the following steps：
(1) 0.5mol the second function monomer 3- amino-N- (2- sulfydryl second is added in container in the case where being passed through nitrogen
Base) propionamide (CAS：539-83-3 is purchased from Ivy Fine Chemicals), and stirred under ice-water bath
(2) 0.5mol the first function monomer 3, the 50ml methanol solutions of 4- epoxy methyl butyrates is added dropwise, and system is moved
Stirred under to room temperature environment 3 hours, be then concentrated by evaporation and obtain intermediate；
(3) system is warming up to 130 DEG C, adds 0.8g p-methyl benzenesulfonic acid, stir lower reaction 4 hours, evaporation and concentration obtains
The dissaving polymer；
(4) silver nitrate powder is dissolved in DMSO under normal temperature, it is 0.01g/mL to make concentration of silver ions, and adds the 3rd step
Obtained dissaving polymer, the concentration for making dissaving polymer are 0.1g/mL, stir 45min, and 0.2ml boron hydrogen is added dropwise again
Change sodium, reaction 60min can obtain the nano silver additive.
The preparation method of functional poly carbamate fibre, comprises the following steps：
(1) preparing raw material of functional poly carbamate fibre is weighed by defined parts by weight, and is being passed through nitrogen
In the case of polyalcohol, isocyanates, catalyst are added in reactor, controlling reaction temperature at 80 DEG C, react 2 hours, gather
Urethane prepolymer；
(2) the prepolymer dissolving obtained the first step in a solvent, is then added dropwise chain extender, and stirring reaction 30min, controlled
The dosage of solvent processed makes the concentration of the reaction product in system be 33wt%；
(3) nano silver additive is added dropwise in the system obtained toward second step, stirring reaction 45min, obtains functional poly ammonia
Carbamate spinning solution；
(4) the functional poly carbamate spinning solution for obtaining the 3rd step filters deaeration, using dry spinning method, system
It is standby to obtain functional poly carbamate fibre.
Antimicrobial fabric preparation method with nano silver particles：
The antimicrobial fabric with nano silver particles is warp by functional poly carbamate fibre, with crust
Cellulose fiber weaves for parallel, with 5：1 tension force ratio mixed weaving forms.
Embodiment 4
Embodiment 4 provides a kind of functional poly carbamate fibre, the functional poly carbamate fibre
Preparing raw material, in parts by weight, including：Polyalcohol 40, binary oxime 2, isocyanates 10, chain extender 1.2, nano silver additive
0.8th, catalyst 0.3, solvent 95.
The polyalcohol is polytetramethylene ether diol, purchased from traditional Chinese medicines chemical reagent；The isocyanates is diphenylmethyl
Alkane diisocyanate, purchased from traditional Chinese medicines chemical reagent；The chain extender is propane diamine, purchased from traditional Chinese medicines chemical reagent；The catalyst
For dibutyl tin laurate, purchased from traditional Chinese medicines chemical reagent；The solvent is DMSO；The binary oxime is 2,4- pentanes diketone two
Oxime (CAS：2157-56-4, purchased from Wuhan profit is micro- can Science and Technology Ltd.).
The preparation method of the nano silver additive is that the second function monomer selects with the step difference in embodiment 3
With AEEA (CAS：111-41-1, purchased from traditional Chinese medicines chemical reagent).
The preparation method of functional poly carbamate fibre is same as Example 3.
Antimicrobial fabric preparation method with nano silver particles is same as Example 3.
Embodiment 5
Embodiment 5 provides a kind of functional poly carbamate fibre, the functional poly carbamate fibre
Preparing raw material, in parts by weight, including：Polyalcohol 40, binary oxime 2, isocyanates 10, chain extender 1.2, nano silver additive
0.8th, catalyst 0.3, solvent 95.
The polyalcohol is polytetramethylene ether diol, purchased from traditional Chinese medicines chemical reagent；The isocyanates is diphenylmethyl
Alkane diisocyanate, purchased from traditional Chinese medicines chemical reagent；The chain extender is propane diamine, purchased from traditional Chinese medicines chemical reagent；The catalyst
For dibutyl tin laurate, purchased from traditional Chinese medicines chemical reagent；The solvent is DMSO；The binary oxime is 2,4- pentanes diketone two
Oxime (CAS：2157-56-4, purchased from Wuhan profit is micro- can Science and Technology Ltd.).
The preparation method of the nano silver additive is that the second function monomer selects with the step difference in embodiment 3
With diethylenetriamine, the first function monomer methyl acrylate (CAS：96-33-3, purchased from traditional Chinese medicines chemical reagent).
The preparation method of functional poly carbamate fibre is same as Example 3.
Antimicrobial fabric preparation method with nano silver particles is same as Example 3.
Embodiment 6
Embodiment 6 provides a kind of functional poly carbamate fibre, the functional poly carbamate fibre
Preparing raw material, in parts by weight, including：Polyalcohol 40, binary oxime 2, isocyanates 10, chain extender 1.2, nano silver additive
0.8th, catalyst 0.3, solvent 95.
The polyalcohol is polytetramethylene ether diol, purchased from traditional Chinese medicines chemical reagent；The isocyanates is diphenylmethyl
Alkane diisocyanate, purchased from traditional Chinese medicines chemical reagent；The chain extender is propane diamine, purchased from traditional Chinese medicines chemical reagent；The catalyst
For dibutyl tin laurate, purchased from traditional Chinese medicines chemical reagent；The solvent is DMSO；The binary oxime is 2,4- pentanes diketone two
Oxime (CAS：2157-56-4, purchased from Wuhan profit is micro- can Science and Technology Ltd.).
The preparation method of the nano silver additive is that the second function monomer selects with the step difference in embodiment 5
Use diethanol amine.
The preparation method of functional poly carbamate fibre is same as Example 5.
Antimicrobial fabric preparation method with nano silver particles is same as Example 5.
Embodiment 7
Embodiment 7 provides a kind of functional poly carbamate fibre, the functional poly carbamate fibre
Preparing raw material, in parts by weight, including：Polyalcohol 40, binary oxime 2, isocyanates 10, chain extender 1.2, nano silver additive
0.8th, catalyst 0.3, solvent 95.
The polyalcohol is polytetramethylene ether diol, purchased from traditional Chinese medicines chemical reagent；The isocyanates is diphenylmethyl
Alkane diisocyanate, purchased from traditional Chinese medicines chemical reagent；The chain extender is propane diamine, purchased from traditional Chinese medicines chemical reagent；The catalyst
For dibutyl tin laurate, purchased from traditional Chinese medicines chemical reagent；The solvent is DMSO；The binary oxime is 2,4- pentanes diketone two
Oxime (CAS：2157-56-4, purchased from Wuhan profit is micro- can Science and Technology Ltd.).
The preparation method of the nano silver additive is that the second function monomer selects with the step difference in embodiment 5
With 3- amino-N- (2- mercaptoethyls) propionamide.
The preparation method of functional poly carbamate fibre is same as Example 5.
Antimicrobial fabric preparation method with nano silver particles is same as Example 5.
Embodiment 8
Embodiment 8 provides a kind of functional poly carbamate fibre, the functional poly carbamate fibre
Preparing raw material, in parts by weight, including：Polyalcohol 40, binary oxime 2, isocyanates 10, chain extender 1.2, nano silver additive
0.8th, catalyst 0.3, solvent 95.
The polyalcohol is polytetramethylene ether diol, purchased from traditional Chinese medicines chemical reagent；The isocyanates is diphenylmethyl
Alkane diisocyanate, purchased from traditional Chinese medicines chemical reagent；The chain extender is propane diamine, purchased from traditional Chinese medicines chemical reagent；The catalyst
For dibutyl tin laurate, purchased from traditional Chinese medicines chemical reagent；The solvent is DMSO；The binary oxime is 2,4- pentanes diketone two
Oxime (CAS：2157-56-4, purchased from Wuhan profit is micro- can Science and Technology Ltd.).
The preparation method of the nano silver additive is that the second function monomer selects with the step difference in embodiment 5
Use AEEA.
The preparation method of functional poly carbamate fibre is same as Example 5.
Antimicrobial fabric preparation method with nano silver particles is same as Example 5.
Embodiment 9
Embodiment 9 provides a kind of functional poly carbamate fibre, the functional poly carbamate fibre
Preparing raw material, in parts by weight, including：Polyalcohol 40, binary oxime 2, isocyanates 10, chain extender 1.2, nano silver additive
0.8th, catalyst 0.3, solvent 95.
The polyalcohol is polytetramethylene ether diol, purchased from traditional Chinese medicines chemical reagent；The isocyanates is diphenylmethyl
Alkane diisocyanate, purchased from traditional Chinese medicines chemical reagent；The chain extender is propane diamine, purchased from traditional Chinese medicines chemical reagent；The catalyst
For dibutyl tin laurate, purchased from traditional Chinese medicines chemical reagent；The solvent is DMSO；The binary oxime is 2,4- pentanes diketone two
Oxime (CAS：2157-56-4, purchased from Wuhan profit is micro- can Science and Technology Ltd.).
The preparation method of the nano silver additive is that the first function monomer selects with the step difference in embodiment 5
With 4- (2- Oxyranyles)-methyl phenylpropionate (CAS：6304-01-4, purchased from Leancare Ltd.).
The preparation method of functional poly carbamate fibre is same as Example 5.
Antimicrobial fabric preparation method with nano silver particles is same as Example 5.
Embodiment 10
Embodiment 10 provides a kind of functional poly carbamate fibre, the functional poly carbamate fibre
Preparing raw material, in parts by weight, including：Polyalcohol 40, binary oxime 2, isocyanates 10, chain extender 1.2, nano silver additive
0.8th, catalyst 0.3, solvent 95.
The polyalcohol is polytetramethylene ether diol, purchased from traditional Chinese medicines chemical reagent；The isocyanates is diphenylmethyl
Alkane diisocyanate, purchased from traditional Chinese medicines chemical reagent；The chain extender is propane diamine, purchased from traditional Chinese medicines chemical reagent；The catalyst
For dibutyl tin laurate, purchased from traditional Chinese medicines chemical reagent；The solvent is DMSO；The binary oxime is 2,4- pentanes diketone two
Oxime (CAS：2157-56-4, purchased from Wuhan profit is micro- can Science and Technology Ltd.).
The preparation method of the nano silver additive is that the second function monomer selects with the step difference in embodiment 9
Use diethanol amine.
The preparation method of functional poly carbamate fibre is same as Example 9.
Antimicrobial fabric preparation method with nano silver particles is same as Example 9.
Embodiment 11
Embodiment 11 provides a kind of functional poly carbamate fibre, the functional poly carbamate fibre
Preparing raw material, in parts by weight, including：Polyalcohol 40, binary oxime 2, isocyanates 10, chain extender 1.2, nano silver additive
0.8th, catalyst 0.3, solvent 95.
The polyalcohol is polytetramethylene ether diol, purchased from traditional Chinese medicines chemical reagent；The isocyanates is diphenylmethyl
Alkane diisocyanate, purchased from traditional Chinese medicines chemical reagent；The chain extender is propane diamine, purchased from traditional Chinese medicines chemical reagent；The catalyst
For dibutyl tin laurate, purchased from traditional Chinese medicines chemical reagent；The solvent is DMSO；The binary oxime is 2,4- pentanes diketone two
Oxime (CAS：2157-56-4, purchased from Wuhan profit is micro- can Science and Technology Ltd.).
The preparation method of the nano silver additive is that the second function monomer selects with the step difference in embodiment 9
Use AEEA.
The preparation method of functional poly carbamate fibre is same as Example 9.
Antimicrobial fabric preparation method with nano silver particles is same as Example 9.
Embodiment 12
Embodiment 12 provides a kind of functional poly carbamate fibre, the functional poly carbamate fibre
Preparing raw material, in parts by weight, including：Polyalcohol 40, binary oxime 2, isocyanates 10, chain extender 1.2, nano silver additive
0.8th, catalyst 0.3, solvent 95.
The polyalcohol is polytetramethylene ether diol, purchased from traditional Chinese medicines chemical reagent；The isocyanates is diphenylmethyl
Alkane diisocyanate, purchased from traditional Chinese medicines chemical reagent；The chain extender is propane diamine, purchased from traditional Chinese medicines chemical reagent；The catalyst
For dibutyl tin laurate, purchased from traditional Chinese medicines chemical reagent；The solvent is DMSO；The binary oxime is 2,4- pentanes diketone two
Oxime (CAS：2157-56-4, purchased from Wuhan profit is micro- can Science and Technology Ltd.).
The preparation method of the nano silver additive is that the first function monomer selects with the step difference in embodiment 9
With 4- (2- Oxiranylmethoxies) butyl propyleneglycol acid esters (CAS：119692-59-0, it is limited to open up gram chemistry science and technology purchased from Shanghai
Company).
The preparation method of functional poly carbamate fibre is same as Example 9.
Antimicrobial fabric preparation method with nano silver particles is same as Example 9.
Embodiment 13
Embodiment 13 provides a kind of functional poly carbamate fibre, the functional poly carbamate fibre
Preparing raw material, in parts by weight, including：Polyalcohol 40, binary oxime 2, isocyanates 10, chain extender 1.2, nano silver additive
0.8th, catalyst 0.3, solvent 95.
The polyalcohol is polytetramethylene ether diol, purchased from traditional Chinese medicines chemical reagent；The isocyanates is diphenylmethyl
Alkane diisocyanate, purchased from traditional Chinese medicines chemical reagent；The chain extender is propane diamine, purchased from traditional Chinese medicines chemical reagent；The catalyst
For dibutyl tin laurate, purchased from traditional Chinese medicines chemical reagent；The solvent is DMSO；The binary oxime is 2,4- pentanes diketone two
Oxime (CAS：2157-56-4, purchased from Wuhan profit is micro- can Science and Technology Ltd.).
The preparation method of the nano silver additive is the second function monomer with the step difference in embodiment 12
From diethanol amine.
The preparation method of functional poly carbamate fibre is identical with embodiment 12.
Antimicrobial fabric preparation method with nano silver particles is identical with embodiment 12.
Embodiment 14
Embodiment 14 provides a kind of functional poly carbamate fibre, the functional poly carbamate fibre
Preparing raw material, in parts by weight, including：Polyalcohol 40, binary oxime 2, isocyanates 10, chain extender 1.2, nano silver additive
0.8th, catalyst 0.3, solvent 95.
The polyalcohol is polytetramethylene ether diol, purchased from traditional Chinese medicines chemical reagent；The isocyanates is diphenylmethyl
Alkane diisocyanate, purchased from traditional Chinese medicines chemical reagent；The chain extender is propane diamine, purchased from traditional Chinese medicines chemical reagent；The catalyst
For dibutyl tin laurate, purchased from traditional Chinese medicines chemical reagent；The solvent is DMSO；The binary oxime is 2,4- pentanes diketone two
Oxime (CAS：2157-56-4, purchased from Wuhan profit is micro- can Science and Technology Ltd.).
The preparation method of the nano silver additive is the second function monomer with the step difference in embodiment 12
From AEEA.
The preparation method of functional poly carbamate fibre is identical with embodiment 12.
Antimicrobial fabric preparation method with nano silver particles is identical with embodiment 12.
Embodiment 15
Embodiment 15 provides a kind of functional poly carbamate fibre, the functional poly carbamate fibre
Preparing raw material, in parts by weight, including：Polyalcohol 40, binary oxime 2, isocyanates 10, chain extender 1.2, nano silver additive
0.8th, catalyst 0.3, solvent 95.
The polyalcohol is polytetramethylene ether diol, purchased from traditional Chinese medicines chemical reagent；The isocyanates is diphenylmethyl
Alkane diisocyanate, purchased from traditional Chinese medicines chemical reagent；The chain extender is propane diamine, purchased from traditional Chinese medicines chemical reagent；The catalyst
For dibutyl tin laurate, purchased from traditional Chinese medicines chemical reagent；The solvent is DMSO；The binary oxime is 2,4- pentanes diketone two
Oxime (CAS：2157-56-4, purchased from Wuhan profit is micro- can Science and Technology Ltd.).
The preparation method of the nano silver additive is the first function monomer with the step difference in embodiment 12
From 4,5- epoxy -2- glycidyl methyl valerates (CAS：63041-05-4).
The preparation method of functional poly carbamate fibre is identical with embodiment 12.
Antimicrobial fabric preparation method with nano silver particles is identical with embodiment 12.
Embodiment 16
Embodiment 16 provides a kind of functional poly carbamate fibre, the functional poly carbamate fibre
Preparing raw material, in parts by weight, including：Polyalcohol 40, binary oxime 2, isocyanates 10, chain extender 1.2, nano silver additive
0.8th, catalyst 0.3, solvent 95.
The polyalcohol is polytetramethylene ether diol, purchased from traditional Chinese medicines chemical reagent；The isocyanates is diphenylmethyl
Alkane diisocyanate, purchased from traditional Chinese medicines chemical reagent；The chain extender is propane diamine, purchased from traditional Chinese medicines chemical reagent；The catalyst
For dibutyl tin laurate, purchased from traditional Chinese medicines chemical reagent；The solvent is DMSO；The binary oxime is 2,4- pentanes diketone two
Oxime (CAS：2157-56-4, purchased from Wuhan profit is micro- can Science and Technology Ltd.).
The preparation method of the nano silver additive is the second function monomer with the step difference in embodiment 15
From diethanol amine.
The preparation method of functional poly carbamate fibre is identical with embodiment 15.
Antimicrobial fabric preparation method with nano silver particles is identical with embodiment 15.
Embodiment 17
Embodiment 17 provides a kind of functional poly carbamate fibre, the functional poly carbamate fibre
Preparing raw material, in parts by weight, including：Polyalcohol 40, binary oxime 2, isocyanates 10, chain extender 1.2, nano silver additive
0.8th, catalyst 0.3, solvent 95.
The polyalcohol is polytetramethylene ether diol, purchased from traditional Chinese medicines chemical reagent；The isocyanates is diphenylmethyl
Alkane diisocyanate, purchased from traditional Chinese medicines chemical reagent；The chain extender is propane diamine, purchased from traditional Chinese medicines chemical reagent；The catalyst
For dibutyl tin laurate, purchased from traditional Chinese medicines chemical reagent；The solvent is DMSO；The binary oxime is 2,4- pentanes diketone two
Oxime (CAS：2157-56-4, purchased from Wuhan profit is micro- can Science and Technology Ltd.).
The preparation method of the nano silver additive is the second function monomer with the step difference in embodiment 15
From AEEA.
The preparation method of functional poly carbamate fibre is identical with embodiment 15.
Antimicrobial fabric preparation method with nano silver particles is identical with embodiment 15.
Comparative example 1
Comparative example 1 provides a kind of functional poly carbamate fibre, the functional poly carbamate fibre
Preparing raw material, in parts by weight, including：Polyalcohol 40, binary oxime 2, isocyanates 10, chain extender 1.2, additive 0.8, catalysis
Agent 0.3, solvent 95.
The polyalcohol is polytetramethylene ether diol, purchased from traditional Chinese medicines chemical reagent；The isocyanates is diphenylmethyl
Alkane diisocyanate, purchased from traditional Chinese medicines chemical reagent；The chain extender is propane diamine, purchased from traditional Chinese medicines chemical reagent；The catalyst
For dibutyl tin laurate, purchased from traditional Chinese medicines chemical reagent；The solvent is DMSO；The binary oxime is 2,4- pentanes diketone two
Oxime (CAS：2157-56-4, purchased from Wuhan profit is micro- can Science and Technology Ltd.).
The difference of the preparation method of the additive and the preparation process of nano silver additive in embodiment 15 is
Without (4) step, i.e., without addition silver particles.
The preparation method of functional poly carbamate fibre is identical with embodiment 15.
Antimicrobial fabric preparation method is identical with embodiment 15.
Comparative example 2
Comparative example 2 provides a kind of functional poly carbamate fibre, the functional poly carbamate fibre
Preparing raw material, in parts by weight, including：Polyalcohol 40, binary oxime 2, isocyanates 10, chain extender 1.2, additive 0.8, catalysis
Agent 0.3, solvent 95.
The polyalcohol is polytetramethylene ether diol, purchased from traditional Chinese medicines chemical reagent；The isocyanates is diphenylmethyl
Alkane diisocyanate, purchased from traditional Chinese medicines chemical reagent；The chain extender is propane diamine, purchased from traditional Chinese medicines chemical reagent；The catalyst
For dibutyl tin laurate, purchased from traditional Chinese medicines chemical reagent；The solvent is DMSO；The binary oxime is 2,4- pentanes diketone two
Oxime (CAS：2157-56-4, purchased from Wuhan profit is micro- can Science and Technology Ltd.).The additive is molten for the DMSO of silver nitrate powder
Liquid, wherein concentration of silver ions are 0.01g/mL, i.e., without addition dissaving polymer protective agent.
The preparation method of functional poly carbamate fibre comprises the following steps：
(1) preparing raw material of functional poly carbamate fibre is weighed by defined parts by weight, and is being passed through nitrogen
In the case of polyalcohol, isocyanates, catalyst are added in reactor, controlling reaction temperature at 80 DEG C, react 2 hours, gather
Urethane prepolymer；
(2) the prepolymer dissolving obtained the first step in a solvent, is then added dropwise chain extender, and stirring reaction 30min, controlled
The dosage of solvent processed makes the concentration of the reaction product in system be 33wt%；
(3) additive solution is added dropwise in the system obtained toward second step, 0.2ml sodium borohydrides, stirring reaction is being added dropwise
45min, obtain functional poly carbamate spinning solution；
(4) the functional poly carbamate spinning solution for obtaining the 3rd step filters deaeration, using dry spinning method, system
It is standby to obtain functional poly carbamate fibre.
Antimicrobial fabric preparation method with nano silver particles is identical with embodiment 15.
Comparative example 3
Comparative example 3 provides a kind of functional poly carbamate fibre, the functional poly carbamate fibre
Preparing raw material, in parts by weight, including：Polyalcohol 40, binary oxime 2, isocyanates 10, chain extender 1.2, nano silver additive
0.8th, catalyst 0.3, solvent 95.
The polyalcohol is polytetramethylene ether diol, purchased from traditional Chinese medicines chemical reagent；The isocyanates is diphenylmethyl
Alkane diisocyanate, purchased from traditional Chinese medicines chemical reagent；The chain extender is propane diamine, purchased from traditional Chinese medicines chemical reagent；The catalyst
For dibutyl tin laurate, purchased from traditional Chinese medicines chemical reagent；The solvent is DMSO；The binary oxime is 2,4- pentanes diketone two
Oxime (CAS：2157-56-4, purchased from Wuhan profit is micro- can Science and Technology Ltd.).
The preparation method of functional poly carbamate fibre is identical with embodiment 15.
Antimicrobial fabric preparation method with nano silver particles：
The antimicrobial fabric with nano silver particles is warp by functional poly carbamate fibre, with crust
Cellulose fiber is parallel, is formed with identical tension force mixed weaving.
Comparative example 4
Comparative example 4 provides a kind of functional poly carbamate fibre, the functional poly carbamate fibre
Preparing raw material, in parts by weight, including：Polyalcohol 40, binary oxime 2, isocyanates 10, chain extender 1.2, nano silver additive
0.8th, catalyst 0.3, solvent 95.
The polyalcohol is polytetramethylene ether diol, purchased from traditional Chinese medicines chemical reagent；The isocyanates is diphenylmethyl
Alkane diisocyanate, purchased from traditional Chinese medicines chemical reagent；The chain extender is propane diamine, purchased from traditional Chinese medicines chemical reagent；The catalyst
For dibutyl tin laurate, purchased from traditional Chinese medicines chemical reagent；The solvent is DMSO；The binary oxime is 2,4- pentanes diketone two
Oxime (CAS：2157-56-4, purchased from Wuhan profit is micro- can Science and Technology Ltd.).
The preparation method of functional poly carbamate fibre is identical with embodiment 15.
Antimicrobial fabric is formed by the braiding of functional poly carbamate fibre.
Comparative example 5
Comparative example 5 provides a kind of functional poly carbamate fibre, the functional poly carbamate fibre
Preparing raw material, in parts by weight, including：Polyalcohol 40, isocyanates 10, chain extender 1.2, nano silver additive 0.8, catalyst
0.3rd, solvent 95.
The polyalcohol is polytetramethylene ether diol, purchased from traditional Chinese medicines chemical reagent；The isocyanates is diphenylmethyl
Alkane diisocyanate, purchased from traditional Chinese medicines chemical reagent；The chain extender is propane diamine, purchased from traditional Chinese medicines chemical reagent；The catalyst
For dibutyl tin laurate, purchased from traditional Chinese medicines chemical reagent；The solvent is DMSO.
The preparation method of functional poly carbamate fibre is identical with embodiment 15.
Antimicrobial fabric preparation method with nano silver particles is identical with embodiment 15.
Performance evaluation
1. the anti-microbial property test of antimicrobial fabric
From Escherichia coli (E.coli), staphylococcus aureus (S.aureus) as test strain.Reference
GB15979-2002《Disposable Sanitary Accessory sanitary standard》, anti-(suppression) the bacterium product bacteriostasis property examination of 5 non-stripping property of appendix C
Proved recipe method.
2. antimicrobial fabric tension failure strength test
The chitin fabric sample that length is 30cm is pulled into trimming yarn width (10cm), clamping length as defined in is
350mm, pre-tension 5N, each three through broadwise.
3. the degradation property of antimicrobial fabric
The antimicrobial fabric of a block length cube shape is cut, with diethyl ether solution soaking flushing, wipes dry solvent and at 60 DEG C
Lower vacuum drying 4h, it is referred to as m to then take out its weight1.Then under illumination condition, the material is put into the training for filling distilled water
Support and soaked eight weeks in ware, distillation coolant-temperature gage is 40 DEG C, wipes dry solvent and is dried in vacuo 4h at 60 DEG C, then takes out and claims its weight
For m2.The mass loss rate of environment-friendly type degradable material is calculated in the following manner.
4. silver particles turnover rate
The fiber of gained is cleaned 30 minutes clear 3 times at 40 DEG C using same method, with ICP-MS testers
The ratio (%) that silver particles are lost in fiber is tested using identical method.
The performance test table of table 1
As can be seen from Table 1, the antimicrobial fabric with nano silver particles in the present invention is with good biocidal property
Energy, ultimate strength, elongation at break, and degradability, it can thus be seen that the nano silver additive in the present invention can be very
Good is distributed in fiber, plays good fungistatic effect.Moreover, the silver particles in fabric can be deposited in fabric for a long time,
Play antibacterial, antimicrobial effect.
Foregoing example is merely illustrative, for explaining some features of the method for the invention.Appended right will
Ask and be intended to require the scope as wide as possible being contemplated that, and embodiments as presented herein is only according to all possible implementation
The explanation of the embodiment of the selection of the combination of example.Therefore, the purpose of applicant is that appended claim is not illustrated this hair
The selectional restriction of the example of bright feature.Some number ranges used also include sub- model within the claims
Enclose, the change in these scopes should be also construed to by appended claim covering in the conceived case.
Claims (10)
- A kind of 1. functional poly carbamate fibre, it is characterised in that the preparation of the functional poly carbamate fibre Raw material, in parts by weight, comprise at least：Polyalcohol 30~55, isocyanates 8~25, chain extender 1~4, nano silver additive 0.1~1.5, catalyst 0.1~0.8, solvent 70~110.
- 2. functional poly carbamate fibre as claimed in claim 1, it is characterised in that the nano silver additive includes Protective agent and nano silver particles；The protective agent is dissaving polymer；The end group of the dissaving polymer is hydroxyl, mercapto At least one of base, amino.
- 3. functional poly carbamate fibre as claimed in claim 2, it is characterised in that the system of the dissaving polymer Standby raw material comprises at least the first function monomer, the second function monomer, catalyst, solvent.
- 4. functional poly carbamate fibre as claimed in claim 3, it is characterised in that first function monomer is selected from 3,4- epoxies methyl butyrate, acrylic acid -2,3- polyglycidyls, oxirane -2- carboxylate methyl esters, 4- (2- oxiranylmethoxies Base) butyl propyleneglycol acid esters, 4- (2- Oxyranyles)-methyl phenylpropionate, methyl acrylate, 4,5- epoxy -2- glycidyls One or more in methyl valerate.
- 5. functional poly carbamate fibre as claimed in claim 3, it is characterised in that second function monomer is selected from One or more in diethanol amine, AEEA, diethylenetriamine, 3- amino-N- (2- mercaptoethyls) propionamide.
- 6. functional poly carbamate fibre as claimed in claim 2, it is characterised in that the system of the nano silver additive Preparation Method comprises at least following steps：(1) the second function monomer is added in container in the case where being passed through nitrogen, and is stirred under ice-water bath(2) methanol solution with the first function monomer of the second function monomer equimolar amounts is added dropwise, and system is moved on into room temperature ring Stirred under border 2~6 hours, be then concentrated by evaporation and obtain intermediate；(3) system is warming up to 100~150 DEG C, adds p-methyl benzenesulfonic acid, stir lower reaction 2~6 hours, evaporation and concentration obtains The dissaving polymer；(4) silver nitrate powder is dissolved in DMSO under normal temperature, and adds the dissaving polymer that the 3rd step obtains, control nitric acid The amount of silver powder and dissaving polymer, the concentration for making dissaving polymer are 0.1g/mL, concentration of silver ions 0.01g/mL, 30~60min is stirred, and 0.1~0.5ml reducing agents are added dropwise again, 30~120min of reaction can obtain the Nano Silver addition Agent.
- 7. the preparation method of the functional poly carbamate fibre as described in claim 1~6, it is characterised in that at least wrap Include following steps：(1) preparing raw material of functional poly carbamate fibre is weighed by defined parts by weight, and is being passed through the situation of nitrogen Lower that polyalcohol, isocyanates, catalyst are added in reactor, controlling reaction temperature is reacted 2~4 hours at 70~80 DEG C, Polyurethane prepolymer；(2) the prepolymer dissolving obtained the first step in a solvent, is then added dropwise chain extender, and 10~30min of stirring reaction, controlled The dosage of solvent processed makes the concentration of the reaction product in system be 30~35wt%；(3) nano silver additive is added dropwise in the system obtained toward second step, 30~45min of stirring reaction, obtains functional poly ammonia Carbamate spinning solution；(4) the functional poly carbamate spinning solution for obtaining the 3rd step filters deaeration, using dry spinning method, is prepared into To functional poly carbamate fibre.
- 8. a kind of antimicrobial fabric with nano silver particles, it is characterised in that the antimicrobial fabric will by such as right The functional poly carbamate fibre described in 1~6 any one and chitin fiber mixed weaving is asked to form.
- 9. there is the antimicrobial fabric of nano silver particles as claimed in claim 8, it is characterised in that the functional poly ammonia The mixed weaving mode of carbamate fiber and chitin fiber is, using functional poly carbamate fibre as warp, with first Shell cellulose fiber weaves for parallel；The tension force ratio of the warp and parallel is 5：1.
- 10. the application of the antimicrobial fabric with nano silver particles as claimed in claim 8, it is characterised in that can apply In medical garments, underwear for men and women, feminine hygiene products field.
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