CN115233459B - Degreasing and degerming process for white duck velvet - Google Patents
Degreasing and degerming process for white duck velvet Download PDFInfo
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- CN115233459B CN115233459B CN202211016535.9A CN202211016535A CN115233459B CN 115233459 B CN115233459 B CN 115233459B CN 202211016535 A CN202211016535 A CN 202211016535A CN 115233459 B CN115233459 B CN 115233459B
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- 241000272525 Anas platyrhynchos Species 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 28
- 230000008569 process Effects 0.000 title claims abstract description 26
- 238000005238 degreasing Methods 0.000 title claims abstract description 25
- 229920001661 Chitosan Polymers 0.000 claims abstract description 56
- 239000007788 liquid Substances 0.000 claims abstract description 25
- 229940123208 Biguanide Drugs 0.000 claims abstract description 23
- 238000005406 washing Methods 0.000 claims abstract description 17
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 238000002791 soaking Methods 0.000 claims abstract description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 239000011787 zinc oxide Substances 0.000 claims description 15
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 14
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 7
- JHUFGBSGINLPOW-UHFFFAOYSA-N 3-chloro-4-(trifluoromethoxy)benzoyl cyanide Chemical compound FC(F)(F)OC1=CC=C(C(=O)C#N)C=C1Cl JHUFGBSGINLPOW-UHFFFAOYSA-N 0.000 claims description 7
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 7
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- 230000001954 sterilising effect Effects 0.000 claims description 7
- KSCAZPYHLGGNPZ-UHFFFAOYSA-N 3-chloropropyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)CCCCl KSCAZPYHLGGNPZ-UHFFFAOYSA-N 0.000 claims description 6
- YPCMISLZCVOUJB-UHFFFAOYSA-N 4-cyano-4-methyl-5-phenyl-5-sulfanylidenepentanoic acid Chemical compound OC(=O)CCC(C)(C#N)C(=S)C1=CC=CC=C1 YPCMISLZCVOUJB-UHFFFAOYSA-N 0.000 claims description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 6
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 claims description 6
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 239000012986 chain transfer agent Substances 0.000 claims description 3
- 238000006482 condensation reaction Methods 0.000 claims description 3
- 238000005886 esterification reaction Methods 0.000 claims description 3
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 3
- 239000003999 initiator Substances 0.000 claims description 2
- 239000000178 monomer Substances 0.000 claims description 2
- 230000000379 polymerizing effect Effects 0.000 claims description 2
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 18
- 210000003746 feather Anatomy 0.000 abstract description 13
- 230000006872 improvement Effects 0.000 abstract description 2
- 229910052710 silicon Inorganic materials 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- -1 silicon quaternary ammonium salt Chemical class 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000003242 anti bacterial agent Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- VHYFNPMBLIVWCW-UHFFFAOYSA-N 4-Dimethylaminopyridine Chemical compound CN(C)C1=CC=NC=C1 VHYFNPMBLIVWCW-UHFFFAOYSA-N 0.000 description 2
- 239000006087 Silane Coupling Agent Substances 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000005445 natural material Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 125000000542 sulfonic acid group Chemical group 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 210000002268 wool Anatomy 0.000 description 2
- YRIZYWQGELRKNT-UHFFFAOYSA-N 1,3,5-trichloro-1,3,5-triazinane-2,4,6-trione Chemical compound ClN1C(=O)N(Cl)C(=O)N(Cl)C1=O YRIZYWQGELRKNT-UHFFFAOYSA-N 0.000 description 1
- 229960000549 4-dimethylaminophenol Drugs 0.000 description 1
- 235000019737 Animal fat Nutrition 0.000 description 1
- 241000272814 Anser sp. Species 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 235000021120 animal protein Nutrition 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- PNHHVOISKCAJLC-UHFFFAOYSA-N benzaldehyde;methanol Chemical compound OC.O=CC1=CC=CC=C1 PNHHVOISKCAJLC-UHFFFAOYSA-N 0.000 description 1
- 150000004283 biguanides Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000006196 deacetylation Effects 0.000 description 1
- 238000003381 deacetylation reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000001877 deodorizing effect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 235000019197 fats Nutrition 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 description 1
- 244000000010 microbial pathogen Species 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229950009390 symclosene Drugs 0.000 description 1
Classifications
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M19/00—Treatment of feathers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
- C08G81/02—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers at least one of the polymers being obtained by reactions involving only carbon-to-carbon unsaturated bonds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/55—Design of synthesis routes, e.g. reducing the use of auxiliary or protecting groups
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Textile Engineering (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The scheme relates to a degreasing and degerming process for white duck velvet, which comprises the following steps of: pre-separating, ash removal, fine separation and primary washing; preparing finishing liquid: dispersing chitosan derivative and organosilicon quaternary ammonium salt in water according to the mass ratio of 1-3:1 to obtain 5g/L finishing liquid; and (3) fine washing: dewatering and soaking the pretreated white duck down in the finishing liquid, padding, rinsing with clear water, dewatering and drying; wherein the chitosan derivative comprises N-biguanide chitosan and p (AM-co-ALS) grafted chitosan, and the structural formula is as follows:
Description
Technical Field
The invention relates to the technical field of down feather processing, in particular to a degreasing and degerming process for white duck down feather.
Background
The down is a natural material with excellent heat retention, and compared with the natural material, the cotton, silk, chemical fiber and other fibers are linear, and the long-term use can cause hardening, thereby influencing the heat retention performance and comfort; the down feather is a mixture of feather and down feather, and the down feather is three-dimensional spherical and has no hardening problem. However, the down directly sources goose and duck body, is an animal protein fiber and is accompanied by animal fat, so that a large amount of stains and various pathogenic microorganisms are carried, and if the down cannot be treated cleanly, the health of people can be endangered.
The existing production process of the antibacterial down feather generally comprises the following steps: pre-separating, ash removal, fine separation, primary washing, dehydration, drying, cooling and packaging; in the traditional degreasing and antibacterial process of the down feather, the down feather is treated in the drying process by adopting agents such as trichloroisocyanuric acid and the like; although this method can effectively remove bacteria, the extremely strong oxidizing property can weaken the fluffy performance of the down. CN1023525688 discloses a finishing method of down with antibacterial function, which adopts chitosan to finish down fibers, so that the effects of antibacterial, mildew-proof, deodorizing and moisture absorption can be obtained, and meanwhile, the higher fluffiness of the down can be ensured. However, in reality, chitosan belongs to a dissolution type antibacterial finishing agent, and slowly dissolves to achieve an antibacterial effect. Thus, the antibacterial property of the chitosan-finished fabric is gradually lost after continuous use for a period of time.
Disclosure of Invention
Aiming at the defects in the prior art, the invention is based on the modification of chitosan to obtain N-biguanide chitosan and p (AM-co-ALS) grafted chitosan, and combines the organosilicon quaternary ammonium salt containing nano zinc oxide particles to finish down, thereby being capable of effectively sterilizing and degreasing.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a degreasing and degerming process for white duck down comprises the following steps:
s1, pretreatment of white duck velvet: pre-separating, ash removal, fine separation and primary washing;
s2, preparing finishing liquid: dispersing chitosan derivative and organosilicon quaternary ammonium salt in water according to the mass ratio of 1-3:1 to obtain 5g/L finishing liquid;
s3, fine washing: dewatering and soaking the pretreated white duck down in the finishing liquid, padding, rinsing with clear water, dewatering and drying;
wherein the chitosan derivative comprises N-biguanide chitosan and p (AM-co-ALS) grafted chitosan, and the structural formula is as follows:
m and n are each independently integers of 10 to 20 and 5 to 10.
Further, the preparation process of the p (AM-co-ALS) grafted chitosan comprises the following steps:
1) Polymerizing acrylamide and sodium allylsulfonate serving as monomers under the condition that 4-cyano-4 (thiobenzoyl) valeric acid serving as a chain transfer agent and azodiisobutyronitrile serving as an initiator to obtain p (AM-co-ALS);
2) The chitosan protects amino through condensation reaction of benzaldehyde and amino, then carries out esterification reaction with p (AM-co-ALS), and removes benzaldehyde after the reaction is finished to obtain p (AM-co-ALS) grafted chitosan.
Further, in the step S1, the molar ratio of the acrylamide to the sodium allylsulfonate to the 4-cyano-4 (thiobenzoyl) pentanoic acid to the azobisisobutyronitrile is 10-30:5-15:1:0.02.
Further, the mass ratio of the N-biguanide chitosan to the p (AM-co-ALS) grafted chitosan is 3-5:7-5.
Further, the preparation process of the organosilicon quaternary ammonium salt is as follows:
1) Dispersing nano zinc oxide in absolute ethyl alcohol, performing ultrasonic dispersion for 1h, adding gamma-chloropropyl triethoxysilane into the solution, heating the solution to 40-50 ℃, refluxing and stirring the solution for 2h, performing suction filtration, washing the solution by using absolute ethyl alcohol, and drying the solution to obtain ZnO/KH230;
2) Adding hexamethylenetetramine into a reaction bottle, and adding pyridine to dissolve completely; and (3) ultrasonically dispersing ZnO/KH230 in toluene solution, adding the solution into a reaction bottle, setting the temperature to 110 ℃, carrying out microwave heating reflux for 5-10 h, cooling and standing after the reaction is finished, and recrystallizing acetone to obtain the organosilicon quaternary ammonium salt.
Further, the mass ratio of the nano zinc oxide to the gamma-chloropropyl triethoxysilane is 2:1; the mass ratio of hexamethylenetetramine to ZnO/KH230 is 1:2.
Further, the temperature is set to 70-80 ℃ in the fine washing process, and the temperature is kept for 30-100 min.
The beneficial effects of the invention are as follows: according to the scheme, through improvement of a fine washing process in a conventional down feather treatment process, the self-made chitosan derivative and the organosilicon quaternary ammonium salt are used for preparing finishing liquid, so that the antibacterial property and the degreasing rate of the finished down feather can be effectively improved, and the treatment process is simple.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in connection with the embodiments, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In addition, the technical features of the different embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
Examples
The raw materials used in the scheme can be directly purchased from the market unless otherwise specified.
N-biguanide chitosan
Has stronger and spectral antibacterial activity than chitosan, has simple preparation method, and can be used for synthesizing chitosan biguanide derivatives and application thereof on wool, and is prepared by wool spinning technology, volume 37, phase 12.
4-cyano-4 (thiobenzoyl) pentanoic acid as chain transfer agent
For the usual RAFT reagents, reference is made to Macromolecules,2001,34:2248-2256, either synthetically or commercially available directly.
p (AM-co-ALS) grafted chitosan
The preparation process of (2) is as follows:
1) 20mmol of acrylamide, 10mmol of sodium allylsulfonate, 1mmol of 4-cyano-4 (thiobenzoyl) pentanoic acid and 0.2mmol of azodiisobutyronitrile are added into a reaction bottle, and the freezing, the air extraction and the nitrogen filling are repeated for three times to react for 2 hours at 60 ℃; p (AM-co-ALS) 1, mn=3100 g/mol, m=17, n=6;
changing the reaction feeding ratio to obtain the following components:
p(AM-co-ALS)2，Mn＝2200g/mol，m＝6，n＝15；
p(AM-co-ALS)3，Mn＝2700g/mol，m＝13，n＝8；
p(AM-co-ALS)4，Mn＝4400g/mol，m＝25，n＝7；
2) Chitosan (deacetylation degree 91.5%, average molecular weight 3000) protects amino group by condensation reaction of benzaldehyde and amino group, 4g chitosan is dispersed in methanol water solution, 15ml benzaldehyde methanol solution is added dropwise, temperature is raised to 50 ℃, reflux reaction is carried out for 4h, and amino protective shell glycan is obtained by ethanol cable extraction; 2g of the mixture is dispersed in DMF, DCC (binary solid) and nitrogen protection are added, equal mass of p (AM-co-ALS) is added, the mixture is stirred at low speed, DMF solution dissolved with DMAP is dripped, the mixture is stirred at normal temperature for 48 hours for esterification reaction, benzaldehyde is removed after the reaction is finished to obtain p (AM-co-ALS) grafted chitosan, p (AM-co-ALS) 1-4 is corresponded, and the final products are numbered as p (AM-co-ALS)/CS-1, p (AM-co-ALS)/CS-2, p (AM-co-ALS)/CS-3 and p (AM-co-ALS)/CS-4.
In the scheme, the chitosan is modified, and firstly N-biguanide chitosan is prepared, and compared with chitosan, the N-biguanide chitosan has higher antibacterial property, so that the N-biguanide chitosan can keep positive electricity in a larger pH value range, and the stability of molecules is improved; in addition, the polymer grafting modification chitosan of sodium allylsulfonate and acrylamide can also improve the antibacterial property, and the electronegativity of the sulfonic acid group and the N-biguanide chitosan are subjected to electrostatic adsorption, so that the combination degree is high, and the durability is improved. The chitosan with the introduced sulfonic group has a surface active function to a certain extent, and further plays a role in removing the content of oil in the down in the process of fine washing, so that the residual fat rate in the down is reduced.
The preparation process of the organosilicon quaternary ammonium salt comprises the following steps:
1) Dispersing 2g of nano zinc oxide in 50ml of absolute ethyl alcohol, performing ultrasonic dispersion for 1h, adding 1g of gamma-chloropropyl triethoxysilane into the solution, heating to 40-50 ℃, refluxing and stirring for 2h, performing suction filtration, washing with absolute ethyl alcohol, and drying to obtain ZnO/KH230;
2) 1.5g of hexamethylenetetramine is added into a reaction bottle, and 30ml of pyridine is added to dissolve the hexamethylenetetramine completely; 3g ZnO/KH230 is dispersed in toluene solution by ultrasonic, then added into a reaction bottle, the temperature is set at 110 ℃, microwave heating reflux is carried out for 5-10 h, cooling and standing are carried out after the reaction is finished, and acetone recrystallization is carried out, thus obtaining the organosilicon quaternary ammonium salt.
The organosilicon quaternary ammonium salt antibacterial agent belongs to a non-leaching antibacterial agent, has good durability, can effectively make up the problem of poor durability of chitosan, and further avoids the problem of antibacterial failure; in the scheme, hexamethylenetetramine and a silane coupling agent are used for synthesizing a multi-head organosilicon quaternary ammonium salt, so that the antibacterial effect is good, and in the reaction process, the gamma-chloropropyl triethoxy silane coupling agent plays a bridging role to wrap nano zinc oxide particles in organosilicon, so that the antibacterial property is further improved due to the inorganic and organic compounding, and the down has a longer-lasting antibacterial effect. The finishing liquid formed by the compounded antibacterial agent has good effect of sterilizing down, and is less in use amount, more economical and efficient.
A degreasing and degerming process for white duck down comprises the following steps:
s1, pretreatment of white duck velvet: pre-separating, ash removal, fine separation and primary washing;
s2, preparing finishing liquid: dispersing chitosan derivative and organosilicon quaternary ammonium salt in water according to the mass ratio of 1-3:1 to obtain 5g/L finishing liquid;
s3, fine washing: dewatering and soaking pretreated white duck down in finishing liquid, setting the temperature to 70-80 ℃, preserving heat for 30-100 min, rinsing with clear water, dewatering and drying;
example 1:
according to the degreasing and degerming process for the white duck down, the mass ratio of the N-biguanide chitosan to p (AM-co-ALS)/CS-1 in the finishing liquid is 3:7, and the mass ratio of the N-biguanide chitosan to the organic silicon quaternary ammonium salt is 1:1.
Example 2:
according to the degreasing and degerming process for the white duck down, the mass ratio of the N-biguanide chitosan to p (AM-co-ALS)/CS-1 in the finishing liquid is 5:5, and the mass ratio of the N-biguanide chitosan to the organic silicon quaternary ammonium salt is 2:1.
Example 3:
according to the degreasing and degerming process for the white duck down, the mass ratio of the N-biguanide chitosan to p (AM-co-ALS)/CS-2 in the finishing liquid is 3:7, and the mass ratio of the N-biguanide chitosan to the organic silicon quaternary ammonium salt is 1:1.
Example 4:
according to the degreasing and degerming process for the white duck down, the mass ratio of the N-biguanide chitosan to p (AM-co-ALS)/CS-3 in the finishing liquid is 3:7, and the mass ratio of the N-biguanide chitosan to the organic silicon quaternary ammonium salt is 1:1.
Example 5:
according to the degreasing and degerming process for the white duck down, the mass ratio of the N-biguanide chitosan to p (AM-co-ALS)/CS-4 in the finishing liquid is 3:7, and the mass ratio of the N-biguanide chitosan to the organic silicon quaternary ammonium salt is 1:1.
Example 6:
according to the degreasing and degerming process for the white duck down, the mass ratio of the N-biguanide chitosan to the p (AM-co-ALS)/CS-1 in the finishing liquid is 3:7, and the finishing liquid does not contain organic silicon quaternary ammonium salt.
Example 7:
according to the degreasing and degerming process for the white duck down, the mass ratio of the N-biguanide chitosan to the organic silicon quaternary ammonium salt in the finishing liquid is 1:1, and the finishing liquid does not contain p (AM-co-ALS)/CS.
The residual lipid fraction of down was measured according to GB/T14272-2011, and the antimicrobial properties were measured according to FZ/T73023-2006, and are recorded in Table 1.
TABLE 1
The table shows that the treatment process of the white duck down can effectively degrease and degerming down, p (AM-co-ALS)/CS-4 in finishing liquid plays a decisive role in the degreasing effect, the number of repeated units of sodium allylsulfonate in the structural formula is within 10-20, the effect is optimal, the antibacterial property is lower than 10, and the degreasing effect is weakened; however, if the amount is more than 20, the sulfonic acid group is rich, electronegativity is increased, repulsive effect is increased, and antibacterial property is lowered.
Although embodiments of the present invention have been disclosed above, it is not limited to the use of the description and embodiments, it is well suited to various fields of use for the invention, and further modifications may be readily apparent to those skilled in the art, and accordingly, the invention is not limited to the particular details without departing from the general concepts defined in the claims and the equivalents thereof.
Claims (6)
1. The degreasing and sterilizing process for the white duck down is characterized by comprising the following steps of:
s1, pretreatment of white duck velvet: pre-separating, ash removal, fine separation and primary washing;
s2, preparing finishing liquid: dispersing chitosan derivative and organosilicon quaternary ammonium salt in water according to the mass ratio of 1-3:1 to obtain 5g/L finishing liquid;
s3, fine washing: dewatering and soaking the pretreated white duck down in the finishing liquid, padding, rinsing with clear water, dewatering and drying;
wherein the chitosan derivative comprises N-biguanide chitosan and p (AM-co-ALS) grafted chitosan, and the structural formula is as follows:
m and n are each independently integers of 10 to 20 and 5 to 10;
the preparation process of the organosilicon quaternary ammonium salt comprises the following steps:
1) Dispersing nano zinc oxide in absolute ethyl alcohol, performing ultrasonic dispersion for 1h, adding gamma-chloropropyl triethoxysilane into the solution, heating the solution to 40-50 ℃, refluxing and stirring the solution for 2h, performing suction filtration, washing the solution by using absolute ethyl alcohol, and drying the solution to obtain ZnO/KH230;
2) Adding hexamethylenetetramine into a reaction bottle, and adding pyridine to dissolve completely; and (3) ultrasonically dispersing ZnO/KH230 in toluene solution, adding the solution into a reaction bottle, setting the temperature to 110 ℃, carrying out microwave heating reflux for 5-10 h, cooling and standing after the reaction is finished, and recrystallizing acetone to obtain the organosilicon quaternary ammonium salt.
2. The degreasing and sterilizing process for white duck down according to claim 1, wherein the preparation process of the p (AM-co-ALS) grafted chitosan comprises the following steps:
1) Polymerizing acrylamide and sodium allylsulfonate serving as monomers under the condition that 4-cyano-4 (thiobenzoyl) valeric acid serving as a chain transfer agent and azodiisobutyronitrile serving as an initiator to obtain p (AM-co-ALS);
2) The chitosan protects amino through condensation reaction of benzaldehyde and amino, then carries out esterification reaction with p (AM-co-ALS), and removes benzaldehyde after the reaction is finished to obtain p (AM-co-ALS) grafted chitosan.
3. The degreasing and sterilizing process for white duck down according to claim 2, wherein in the step S1, the molar ratio of the acrylamide, the sodium allylsulfonate, the 4-cyano-4 (thiobenzoyl) pentanoic acid and the azobisisobutyronitrile is 10-30:5-15:1:0.02.
4. The degreasing and sterilizing process for white duck down according to claim 1, wherein the mass ratio of the N-biguanide chitosan to the p (AM-co-ALS) grafted chitosan is 3-5:7-5.
5. The degreasing and degerming process for white duck down according to claim 1, wherein the mass ratio of the nano zinc oxide to gamma-chloropropyl triethoxysilane is 2:1; the mass ratio of hexamethylenetetramine to ZnO/KH230 is 1:2.
6. The degreasing and sterilizing process for white duck down according to claim 1, wherein the temperature is set to 70-80 ℃ in the fine washing process, and the temperature is kept for 30-100 min.
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Denomination of invention: A degreasing and sterilization process for white duck down Granted publication date: 20230425 Pledgee: Yangzhou Branch of Bank of Jiangsu Co.,Ltd. Pledgor: Yangzhou Junxiang Down Products Co.,Ltd. Registration number: Y2024980016089 |