CN105484052A - Preparation method for ecological anti-microbial microcapsule used for tidying silk quilt - Google Patents

Preparation method for ecological anti-microbial microcapsule used for tidying silk quilt Download PDF

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Publication number
CN105484052A
CN105484052A CN201510961302.XA CN201510961302A CN105484052A CN 105484052 A CN105484052 A CN 105484052A CN 201510961302 A CN201510961302 A CN 201510961302A CN 105484052 A CN105484052 A CN 105484052A
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China
Prior art keywords
silk quilt
preparation
ecological
cocoon silk
oil
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CN201510961302.XA
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Chinese (zh)
Inventor
潘世俊
胡小明
张立新
崔颖钊
王祥荣
石继均
梅德祥
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NAFUER GARMENT ORNAMENT CO LD NANTONG
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NAFUER GARMENT ORNAMENT CO LD NANTONG
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Priority to CN201510961302.XA priority Critical patent/CN105484052A/en
Publication of CN105484052A publication Critical patent/CN105484052A/en
Pending legal-status Critical Current

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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M23/00Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
    • D06M23/12Processes in which the treating agent is incorporated in microcapsules
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02Making microcapsules or microballoons
    • B01J13/06Making microcapsules or microballoons by phase separation
    • B01J13/14Polymerisation; cross-linking
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/10Animal fibres
    • D06M2101/12Keratin fibres or silk

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Medicinal Preparation (AREA)

Abstract

The invention discloses a preparation method for an ecological anti-microbial microcapsule used for tidying a silk quilt. According to the method, natural products are used as raw materials, gelatin and a cardanol polyoxyethylene ether aqueous solution are mixed to be uniform at the temperature of 50 DEG C, oil-soluble naturally extracted anti-microbial constituents are added, and the mixture is emulsified in a high-shear emulsifying machine; the prepared emulsion is poured into a chitosan-acetic acid solution on a stirring condition, and after the emulsion is dripped up, transglutaminase is dripped on a stirring condition, and the temperature is kept at 50 DEG C for a reaction for 4-8 hours; after the reaction is over, filtration and vacuum freeze-drying are performed to obtain the ecological anti-microbial microcapsule product. The ecological anti-microbial microcapsule prepared through the method is used for tidying the silk quilt to keep natural and ecological characteristics of the silk quilt, is ecological and safe, and increases the grade and added value of a silk quilt product.

Description

A kind of preparation method of cocoon silk quilt arrangement ecological antibiotic microcapsules
Technical field
The present invention relates to the preparation method of TEXTILE CHEMICALS, be related specifically to the preparation method of the ecological antibiotic microcapsules used when arranging cocoon silk quilt.
Background technology
Since ancient times, silk is that occurring in nature integrates light, soft, carefully natural fabric, have the good reputation of " human body second skin ", is called as " fiber queen " in textile material.Silk is pure natural animal protein fibre, containing the amino acid that 18 kinds of human bodies are necessary, have windproof, dehumidify, calm the nerves, nourish and effect of balanced human's skin.But cocoon silk quilt is often subject to the invasion and attack of bacterium, various bacterium can breed rapidly when condition is suitable for, not only can make fibre variable color, mouldy, degraded etc., also can produce abnormal stimulation to human body skin and bring out various skin disease, form all harm to human lives.In order to maintain the natural characteristic of cocoon silk quilt, the antibacterial finishing agent of exploitation pure natural becomes very important.Along with the progress of science and technology and improving constantly of people's living standard, the health care consciousness of people to self strengthens day by day, the antibiotic finish of textiles is more and more subject to people's attention, and particularly in the home textile products such as cocoon silk quilt, antibiotic finish is particularly important.
Antibacterial fabric originates from World War II, nineteen thirty-five uses quaternary ammonium salt cationic antibacterial finishing agent to process the textile product of process Military Clothing and FAMB through batch (-type) infusion process by G.Domak, to prevent the superinfection of injured soldier, certain effect is served to the bacteriological infection controlling the sick and wounded.Nineteen forty-seven American market has occurred, by commodity such as the diaper of quaternary ammonium salt process, bandage and towels, baby can being prevented to obtain ammonia dermatitis disease.The people such as nineteen fifty-two Britain Engel with softex kw process woollen blanket, bed (seat) pad, cushion fabric.20 century 70 Japan in mid-term are proposed the products such as antibacterial, deodorization socks, antibacterial fabric is made to enter the climax of exploitation, various antibacterial finishing agent releases one after another, except quaternary ammonium salt, phenol, organic nitrogen, diphenyl ether, also have metallic compound, carbamide compounds etc.Within 1975, Dow corning company releases organosilicon quaternary ammonium salt antibacterial finishing agent (commodity are called DC-5700), one of representative kind becoming modern anti-bacteium deodorization finishing agent.Recently during the last ten years, the developmental research of the anti-bacteium deodorization finishing agent of three aspects such as inorganic compound, the complex bound metallic compound of fiber and native compound and progress thereof attract people's attention.The eighties in 20th century starts to have occurred anti-bacterial fibre, particularly the developing rapidly of chemical fibre, becomes by chemical fiber modification the various antibacterial fabrics that anti-bacterial fibre produces, good endurance antibacterial with it and enjoy the favor of people.
The antiseptic used on the textile is at present mostly synthetic antibacterial agents, although solve the antibiotic property problem of textiles.But it also creates a series of problem, some antiseptic has certain harm equally to human body while antibacterial bacteriostatic, this becomes a textile printing and dyeing and chemical and medicine industry field technology worker's difficult problem, and internationally recognized Oeko-Tex Standard Oeko-Texstandardl00 also once specified the product arranged through antibacterial and mouldproof sanitary finish agent certification all off the docket
Summary of the invention
The technical problem to be solved in the present invention overcomes deficiency of the prior art, provides the preparation method of cocoon silk quilt arrangement ecological antibiotic microcapsules, maintains the natural characteristic of cocoon silk quilt, improves class and the surcharge of cocoon-fibre quilt product.
Technical scheme of the present invention is: a kind of preparation method of cocoon silk quilt arrangement ecological antibiotic microcapsules, and its preparation process is:
(1) aqueous gelatin solution and the cardanol polyoxyethylene ether aqueous solution are mixed under 50 DEG C of conditions, make gelatine content account for 3 ~ 5% of whole reactant gross mass, cardanol polyoxyethylene ether content accounts for 1 ~ 2% of whole reactant gross mass;
(2) add the natural extraction antimicrobial component of whole reactant gross mass 1 ~ 3% oil-soluble, in high-shear emulsion machine, carry out emulsification with the rotating speed of 3000 ~ 6000r/min;
(3) the above-mentioned emulsion prepared under agitation drips and pours in 0.5 ~ 1.5% chitosan-acetic acid solution, after emulsion droplets adds, under agitation drip and account for whole reaction system quality 2.0 ~ 8.0% glutamine transaminage, maintain 50 DEG C of reactions 4 ~ 8 hours;
(4) reaction terminates rear filtration, vacuum freeze drying, obtains ecological antibiotic microcapsule product;
The precedence of above-mentioned steps is represented with (1) ~ (4) at this.
Further technical scheme, to be percentage by weight be the natural extraction antimicrobial component of described oil-soluble: the litsea citrate oil of 40%, the archen of 30%, 30% the mixture of Turmeric P.E.
Further technical scheme, described gelatin is general food level gelatin product.
Further technical scheme, described chitosan molecule amount is 100,000 ~ 300,000, and degree of deacetylation is 85% ~ 90%.
Further technical scheme, the Mei Huo unit of described glutamine transaminage is 100U/g.
Described cardanol polyoxyethylene ether is the polyoxyethylene addition product of natural cashew nut shell oil extract, and described glutamine transaminage is a kind of biological cross-linking enzyme, all can commercially buy.
The raw material that the present invention prepares microcapsules all comes as natural products, and wall material gelatin and shitosan are natural polymer, and shitosan itself has certain antibacterial action; Emulsifying agent cardanol polyoxyethylene ether is the polyoxyethylene addition product of natural cashew nut shell oil extract; Antimicrobial component core is the mixture of the natural extraction antimicrobial component of oil-soluble.
Advantage of the present invention is: present invention employs a kind of new bio cross-linking enzyme-glutamine transaminage as crosslinking agent, between glutamine transaminage energy catalytic proteins molecule or the acyl group transfer reaction of inside, cross-linking reaction that can be amino in catalysis gelatin amino acid and chitosan molecule, complete the solidification of wall material, overcome the deficiency that microcapsules preparation in the past adopts chemical cross-linking agent; After the present invention adopts abovementioned technology, the ecological antibiotic microcapsules of preparation are used for the arrangement of cocoon silk quilt, keep natural, the ecological characteristic of cocoon silk quilt, ecological safety; Improve class and the surcharge of cocoon silk quilt product.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described:
Embodiment one: mix accounting for the aqueous solution of whole reaction system quality 3.5% gelatin with the cardanol polyoxyethylene ether accounting for whole reaction system quality 1.5% under 50 DEG C of conditions, add and account for the natural extraction antimicrobial component of whole reaction system quality 2% oil-soluble, in high-shear emulsion machine, carry out emulsification with the rotating speed of 4000r/min; The above-mentioned emulsion prepared under agitation is poured in 1.0% chitosan-acetic acid solution, after emulsion droplets adds, under agitation drips and account for whole reaction system quality 5.0% glutamine transaminage, maintain 50 DEG C of reactions 6 hours.Reaction terminates rear filtration, vacuum freeze drying, obtains ecological antibiotic microcapsule product.
The microcapsules drugloading rate adopting this method obtained is 20.5%, and average grain diameter is 10.2 μm.
Embodiment two: mix accounting for the aqueous solution of whole reaction system quality 3% gelatin with the cardanol polyoxyethylene ether accounting for whole reaction system quality 1% under 50 DEG C of conditions, add and account for the natural extraction antimicrobial component of whole reaction system quality 1% oil-soluble, in high-shear emulsion machine, carry out emulsification with the rotating speed of 3000r/min; The above-mentioned emulsion prepared under agitation is poured in 0.5% chitosan-acetic acid solution, after emulsion droplets adds, under agitation drips and account for whole reaction system quality 2% glutamine transaminage, maintain 50 DEG C of reactions 4 hours.Reaction terminates rear filtration, vacuum freeze drying, obtains ecological antibiotic microcapsule product.
The microcapsules drugloading rate adopting this method obtained is 18%, and average grain diameter is 9 μm.
Embodiment three: mix accounting for the aqueous solution of whole reaction system quality 5% gelatin with the cardanol polyoxyethylene ether accounting for whole reaction system quality 2% under 50 DEG C of conditions, add and account for the natural extraction antimicrobial component of whole reaction system quality 3% oil-soluble, in high-shear emulsion machine, carry out emulsification with the rotating speed of 6000r/min; The above-mentioned emulsion prepared under agitation is poured in 1.5% chitosan-acetic acid solution, after emulsion droplets adds, under agitation drips and account for whole reaction system quality 8% glutamine transaminage, maintain 50 DEG C of reactions 8 hours.Reaction terminates rear filtration, vacuum freeze drying, obtains ecological antibiotic microcapsule product.
The microcapsules drugloading rate adopting this method obtained is 25.5%, and average grain diameter is 15.2 μm.
Above-described is only the preferred embodiment of the present invention.It should be pointed out that for the person of ordinary skill of the art, under the premise without departing from the principles of the invention, can also make some modification and improvement, these also should be considered as belonging to protection scope of the present invention.

Claims (5)

1. cocoon silk quilt arranges the preparation method with ecological antibiotic microcapsules, it is characterized in that: its preparation process is:
(1) aqueous gelatin solution and the cardanol polyoxyethylene ether aqueous solution are mixed under 50 DEG C of conditions, make gelatine content account for 3 ~ 5% of whole reactant gross mass, cardanol polyoxyethylene ether content accounts for 1 ~ 2% of whole reactant gross mass;
(2) add and account for the natural extraction antimicrobial component of whole reactant gross mass 1 ~ 3% oil-soluble, in high-shear emulsion machine, carry out emulsification with the rotating speed of 3000 ~ 6000r/min;
(3) the above-mentioned emulsion prepared under agitation drips and pours in 0.5 ~ 1.5% chitosan-acetic acid solution, after emulsion droplets adds, under agitation drip and account for whole reaction system quality 2.0 ~ 8.0% glutamine transaminage, maintain 50 DEG C of reactions 4 ~ 8 hours;
(4) reaction terminates rear filtration, vacuum freeze drying, obtains ecological antibiotic microcapsule product;
The precedence of above-mentioned steps is represented with (1) ~ (4) at this.
2. the preparation method of a kind of cocoon silk quilt arrangement ecological antibiotic microcapsules according to claim 1, is characterized in that: described for the natural extraction antimicrobial component of oil-soluble is percentage by weight be: the litsea citrate oil of 40%, the archen of 30%, 30% the mixture of Turmeric P.E.
3. the preparation method of a kind of cocoon silk quilt arrangement ecological antibiotic microcapsules according to claim 1, is characterized in that: described gelatin is general food level gelatin product.
4. the preparation method of a kind of cocoon silk quilt arrangement ecological antibiotic microcapsules according to claim 1, it is characterized in that: described chitosan molecule amount is 100,000 ~ 300,000, degree of deacetylation is 85% ~ 90%.
5. the preparation method of a kind of cocoon silk quilt arrangement ecological antibiotic microcapsules according to claim 1, is characterized in that: the Mei Huo unit of described glutamine transaminage is 100U/g.
CN201510961302.XA 2015-12-18 2015-12-18 Preparation method for ecological anti-microbial microcapsule used for tidying silk quilt Pending CN105484052A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107190518A (en) * 2017-07-13 2017-09-22 江苏金太阳纺织科技股份有限公司 A kind of preparation method of antibacterial down feather
CN107385554A (en) * 2017-06-29 2017-11-24 王艳秋 A kind of preparation method of silk quilt silk material
CN115322613A (en) * 2022-08-23 2022-11-11 南京工业大学 Bio-based microcapsule and preparation method and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101708451A (en) * 2009-12-25 2010-05-19 陕西科技大学 Method for preparing high-temperature resistant essence microcapsules
CN102405941A (en) * 2011-08-10 2012-04-11 华南农业大学 Isatis root oil microcapsule and functional fabric finishing agent
CN102885378A (en) * 2012-09-29 2013-01-23 渤海大学 Preparation method of high-temperature resistant microencapsulation turmeric essential oil biological bacteriostatic agent
CN103127031A (en) * 2013-03-21 2013-06-05 黑龙江大学 Preparation method for oily and oil soluble drug nanocapsules

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101708451A (en) * 2009-12-25 2010-05-19 陕西科技大学 Method for preparing high-temperature resistant essence microcapsules
CN102405941A (en) * 2011-08-10 2012-04-11 华南农业大学 Isatis root oil microcapsule and functional fabric finishing agent
CN102885378A (en) * 2012-09-29 2013-01-23 渤海大学 Preparation method of high-temperature resistant microencapsulation turmeric essential oil biological bacteriostatic agent
CN103127031A (en) * 2013-03-21 2013-06-05 黑龙江大学 Preparation method for oily and oil soluble drug nanocapsules

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107385554A (en) * 2017-06-29 2017-11-24 王艳秋 A kind of preparation method of silk quilt silk material
CN107190518A (en) * 2017-07-13 2017-09-22 江苏金太阳纺织科技股份有限公司 A kind of preparation method of antibacterial down feather
WO2019011265A1 (en) * 2017-07-13 2019-01-17 江苏金太阳纺织科技股份有限公司 Method for preparing antibacterial down
CN115322613A (en) * 2022-08-23 2022-11-11 南京工业大学 Bio-based microcapsule and preparation method and application thereof
CN115322613B (en) * 2022-08-23 2023-04-07 南京工业大学 Bio-based microcapsule and preparation method and application thereof

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Address after: 1 East Lake Road, Haian Development Zone, Jiangsu, China (No. 226600 Silk Road, Nantong)

Applicant after: Nafuer Garment Ornament Co., Ld., Nantong

Address before: 226600 silk industrial park, East Lake Road, Nantong Development Zone, Jiangsu, China

Applicant before: Nafuer Garment Ornament Co., Ld., Nantong

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Application publication date: 20160413

RJ01 Rejection of invention patent application after publication