CN107326685A - The preparation of Korean pine phytocide finishing agent and its fabric and method for sorting arranged - Google Patents
The preparation of Korean pine phytocide finishing agent and its fabric and method for sorting arranged Download PDFInfo
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- CN107326685A CN107326685A CN201710663699.3A CN201710663699A CN107326685A CN 107326685 A CN107326685 A CN 107326685A CN 201710663699 A CN201710663699 A CN 201710663699A CN 107326685 A CN107326685 A CN 107326685A
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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
- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
- D06M23/12—Processes in which the treating agent is incorporated in microcapsules
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
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- 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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
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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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/02—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with hydrocarbons
- D06M13/03—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with hydrocarbons with unsaturated hydrocarbons, e.g. alkenes, or alkynes
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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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/02—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with hydrocarbons
- D06M13/03—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with hydrocarbons with unsaturated hydrocarbons, e.g. alkenes, or alkynes
- D06M13/07—Aromatic hydrocarbons
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- 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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/39—Aldehyde resins; Ketone resins; Polyacetals
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
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Abstract
The present invention relates to a kind of preparation of Korean pine phytocide finishing agent and its fabric and method for sorting that arrange, the formula of the finishing agent is:10~40g/L of Korean pine phytocide microcapsules, chitosan crosslinked dose of 10~35g/L, 1~3g/L of 2~5g/L of organosilicon flexible finishing agent and penetrating agent JFC;The finishing agent is to prepare production Korean pine phytocide finishing agent by extracting the process of Korean pine phytocide, preparation Korean pine phytocide microcapsules, preparation Korean pine phytocide finishing agent and bottling and packaging, then the finishing agent is applied to in the arrangement of bafta, the bafta is to staphylococcus aureus bacteriostasis rate>98.2%, to Escherichia coli bacteriostasis rate>92.3%, to Candida albicans bacteriostasis rate>90.5%, deodorizing rate>97.2%, anti-mite rate>90.6%, and scrubbed more than 20 times sterilizations, deodorization and anti-mite effect reduced rate are less than 10%.
Description
Technical field
The present invention relates to fabric finishing agent and Final finishing field, and in particular to a kind of system of Korean pine phytocide finishing agent
Fabric and method for sorting standby and its arrange.
Background technology
Phytocide is plant resistant pathogen, insect, mould and a kind of material secreted, and passes through Forest Bath and absorbs and plants
Thing bacteriocidin can slow down pressure, make happy, reinforcing enteron aisle and cardio-pulmonary function and the effect for effectively playing sterilization.Many plants
All distributing phytocide, but amount, composition, property and the characteristic of phytocide that different plants distributes are all
Difference, in addition the bacteriocidin having have it is toxic.Korean pine E.O (Phytoncide) comes from pine tree, abies holophylla, the plant of Chinese fir etc.
Bacteriocidin is that just have pharmacological effect since ancient times and be eaten always with health in order to long-lived, to this day known to masses
It is added value and the high natural materials of application value.Korean pine phytocide is mainly with the loose alkene of the antibiotics of high volatility
(terpene) it is that material is constituted, and is made up of the isoprene of volume and is referred to as monoterpene (mono-terpene),
Chinese larch-pine alkene (sequi-terpene), diterpene (di-terpene).
Research shows that Korean pine plant has nontoxicity with respect to plants such as pine tree, Japan cypress, magnificent cypresses, and its Korean pine plant sterilization have
The various bacterias such as anti-Escherichia coli, staphylococcus aureus, Candida albicans, have deodorization to ammonia, yellow water element, methyl mercaptan etc.
Property, there is repelling and killing efficacy to dust mite, fine solid particle, formaldehyde absorbing in air can be removed, with purification air-borne dust degraded
Effect, obtain food additives license, have to human body/poultry concentrated force reinforcing, improve immunity and stress reduction effect.
Chinese patent application (201010576189.0) discloses a kind of containing the phytocide extracted in cones of Pinus koraiensis
Natural antibacterial agent and fruit disease comprising it prevent and kill off raw material, it is disclosed that the phytocide extracted from cones of Pinus koraiensis
It is interior to mix proper amount of thymol or blue lasting, as also describing Korean pine in natural antibacterial agent, and document background technology
The fragrance ingredient and antibacterial activity of phytocide are applied in toothpaste, chewing gum, cosmetic material already.
Chinese patent application (201610125127.5) discloses a kind of environmental protection coating material of phytocide containing Korean pine, wherein
Korean pine phytocide containing 1-3wt%, the coating has formaldehyde, the VOCs effect of removing, and effective percentage also has more than 99%
There is sterilization, kill dust mite, remove ammonia, improve IAQ effect, the rate of avoidance of house dust mite is more than 98%, while energy
Alleviate the pressure of people, strengthen concentrated force, improve learning efficiency.
Korean Patent (10-20110000285A) discloses one kind and plant sterilization is extracted from pine tree using supercritical fluid
The method of element, the method for carrying out plant sterilization extraction from pine using supercritical fluid improves plant sterilization and naphthoic acid
Extraction efficiency, the extracting method is comprised the steps of:Broken pine needle is to powdered;The pine needle powder is poured into container, and added
Mixing extractant comprising supercritical carbon dioxide fluid 60-90%, ethanol 6-34% and water 1-9%.
International monopoly (WO2013/081426A1) discloses a kind of conjunction of the active component containing phytocide for asthma
Into thing, the phytocide is extracted from pine tree, cypress, Japan cypress and rue plant, and its extracting method is selected from hot water extraction method, fat
The extraction of suction method, reflux extraction, solvent extraction method, super critical extraction, the way of distillation, ultrasonic extraction, elution method and compression
Method.
Korean Patent (KR101280315B) is a kind of to prepare the phytocide synthetic for Reduce allergy dermatitis
Method, this method step includes Korean pine and Japan cypress being immersed in water 24-36 hours, dries, is milled to length 8-10mm and 3-
4mm, slow squeezing powdery Korean pine and Japan cypress isolate liquid phase, place the liquid phase 24 hours and collect the liquid on upper strata and are extracted
Liquid, handles 36 hours, finally the green tea extractive liquor hybrid reaction with being obtained by similar steps by the extract solution at 13-15 DEG C
Fermentation filtering.
Chinese patent application (201510680930.0) discloses a kind of preparation of new tea tree essential oil microcapsules finishing agent
Method and its application, its preparation method includes preparing tea tree ethereal oil microcapsules, preparing tea tree ethereal oil microcapsule dressing agent, discloses
Application of the tea tree ethereal oil microcapsules dressing liquid in the postfinishing process of textile, the invention surface of microcapsule is continuous, cyst wall tool
There is semi permeability, tea tree ethereal oil can slowly be discharged by cyst wall, and have very strong affinity to yarn fabric, can firmly adhere to
On yarn fabric, so that yarn fabric has the lasting effect of antibacterial.
Chinese patent application (200910040418.4) discloses a kind of Blumea oil microcapsule textile finishing agent and its application,
By the primary raw material of wall material of natural macromolecular material gelatin or Arabic gum, Blumea oil be core, prepare multi-functional Blumea oil
Microcapsule textile composite finishing agent, carries out microcapsules arrangement to fabric using the method for new cross-linked graft, passes through microcapsules
Chemical bond crosslinking curing is formed between wrinkle resistant crosslinking agent and fabric, fabric durable antibiotic healthcare function is assigned.
Tianjin University of Technology Li Hui celerys etc. are in periodical《Weaving Leader》In the document " natural antibacterial finishing agent " delivered, a text
In talk about fiber various functions arrange in, antibacterial deodourizing processing have developed rapidly, the antiseptic used at present can substantially divide
For inorganic, organic and natural antibacterial agent three major types, category animal class mainly has chitin and chitosan in natural antibacterial agent, and category is planted
Species have juniper, argy wormwood, aloe etc..
By above-mentioned related art, Korean pine phytocide has ecology natural, nontoxic, natural aromatic, suppression
The effects such as bacterium sterilization, anti-mite deodorization, purification air, concentrated force reinforcing, raising immunity and stress reduction, Korean pine bactericide
It has been applied to the field such as agricultural chemicals, coating, cosmetic material, medical, but has had not yet to see applied to textile field as knitting
The relevant report of thing finishing agent, although also disclose that in the prior art and microcapsules are made in the vegetable oil such as tea tree ethereal oil, Blumea oil
Finishing agent is applied in the Final finishing of textile, and its functional effect of the vegetable oil microcapsule dressing agent is single, is only intended to pair
The antibiotic finish of textile fabric, and its antibacterial effect is limited.
The content of the invention
In order to overcome the defect of above-mentioned prior art, and the purposes of Korean pine phytocide can be expanded, the present invention is first
Korean pine phytocide is applied to arrangement to fabric by secondary creative propose, so that it is knitted
Thing can persistently obtain the special work(that the Korean pine phytocides such as fragrance, restraining and sterilizing bacteria, anti-mite, the purification air of deodorization have
Effect.For this following technical scheme provided by the present invention:
A kind of Korean pine phytocide finishing agent, the formula of the finishing agent is as follows:
Preferably, the Korean pine phytocide microcapsules are that core prepared by situ aggregation method is Korean pine phytocide
The mass ratio of urea-formaldehyde resin microcapsule, core Korean pine phytocide and wall material Lauxite is 1:1.5~3.0.
Preferably, this chitosan crosslinked dose be by chitosan solution by after oxidizing in chitosan molecule structure
The modification of chitosan of aldehyde radical is generated, can select to make using periodic acid class oxidant, chloric acid class oxidant or hydrochloric acid plus hydrogen peroxide
For oxidant etc..
The present invention also provides a kind of preparation method of Korean pine phytocide finishing agent as described above, this method include with
Lower step:
(1) extraction of Korean pine phytocide
1.1) branches and leaves for choosing Korean pine plant are rinsed well, are ground after drying;
1.2) by step 1.1) in crush after the branches and leaves of Korean pine plant insert in distiller and distilled, and reclaim distillation
During vapor;
1.3) by step 1.2) in reclaim vapor condensed at 5~20 DEG C, obtain Korean pine phytocide and
The mixing liquid of water;
1.4) by the step 1.3) in mixing liquid filtered, after filtering in the mixing liquid add with should
Mixing liquid volume ratio is 2:1~5:1 60wt%~80wt% ethanol solution progress extracting and developing obtains Korean pine plant and killed
Rhzomorph;
(2) preparation of Korean pine phytocide microcapsules
2.1) prepare microcapsule wall material prepolymer
The mass ratio that urea and formaldehyde are added in a constant volume device is 1:1.1~2.5 urea and the aqueous solution of formaldehyde, lead to
Crossing magnetic stirring apparatus makes urea be dissolved in formalin, and use quality percentage adjusts its pH value for 1%~3% NaOH
For 7.5~9.5, reacted 0.5 hour~1.5 hours at a temperature of 60-75 DEG C, obtain sticky melocol prepolymer A;
2.2) emulsification of Korean pine phytocide core
A certain amount of 13 isomeric alcohol polyethenoxy ether emulsifying agent and prepolymer are added in Korean pine phytocide core
Mixing and deionized water, by mixed liquor with 3000~7500r/min speed 20~30min of emulsifying, the water stablized
Bag fluid B;
2.3) polycondensation reaction:By step 2.1) obtained melocol prepolymer A and step 2.2) obtained oil-in-water liquid B
Mixing, is added dropwise acidic catalyst, regulation ph value of mixture is 1.5~5.0, is heated to 45~65 DEG C, polycondensation reaction is obtained for 1-4 hours
To reactant C;
2.4) solidification and suction filtration are dried, by step 2.3) to add mass fraction be 8~15% by obtained reactant C
NaCl, solidifies 1~3 hour at 60~80 DEG C, and it is neutrality that PH is adjusted after solidification, and suction filtration, deionized water washing are carried out after cooling
And it is dried to obtain the Korean pine phytocide microcapsules of solid;
(3) preparation of Korean pine phytocide finishing agent
By step 2.4) prepared by Korean pine phytocide microcapsules, chitosan crosslinked dose, organosilicon flexible finishing agent
And penetrating agent JFC in proportion in a reservoir carry out mixing preparation after obtain Korean pine phytocide finishing agent;Wherein, Korean pine plant
Bacteriocidin microcapsules consumption 10~40g/L, chitosan crosslinked dose of 10~35g/L of consumption, organosilicon flexible 2~8g/L of finishing agent,
1~3g/L of bleeding agent;
(4) bottle and pack.The Korean pine phytocide finishing agent prepared in step (3) is bottled and packed,
And stored under normal temperature, for being used in textile finishing.
Preferably, the step 1.4) in ethanol be ethanol solution that volumetric concentration is 70-80%, or more preferably second
Alcohol is the ethanol solution that volumetric concentration is 75%.Wherein, using 70-80% ethanol solution as extractant, Korean pine essential oil
Yield is higher, and when the ethanol solution using 75% is as extractant, the yield of Korean pine essential oil is maximum.
It is further preferred that the step 2.2) in the 13 isomeric alcohol polyethenoxy ether emulsifying agent be 13 isomeries
The isomeric alcohol polyethenoxy ether 1305 in mass ratio 1 of alcohol APEO 1307 and 13:1 composite emulsifier.To the urea of preparation
Urea formaldehyde microcapsules average grain diameter is small and distribution is narrower.
It is highly preferred that the step 2.1) in urea and formaldehyde mass ratio be 1:1.8, pH value is 8.5, and reaction temperature is
68 DEG C, the time be 1 hour, the step 2.3) in mixed liquor pH value be 3.5.Prepare urea resin microcapsule wall material pre-polymerization
During thing, when step 2.1) and 2.3) in parameter when further so selecting, prepared microcapsules have good form, point
Scattered property is good, and surface is smooth, compact structure.
In addition, the present invention also provides a kind of application of Korean pine phytocide finishing agent, it is used for the rear whole of bafta
Reason, the especially Final finishing to pure cotton fabric.
In addition, the present invention also provides a kind of Korean pine phytocide finishing agent to the method for sorting of bafta, the arrangement side
Method comprises the following steps:
(1) Korean pine phytocide finishing agent is heated to 55~65 DEG C, it is 3 that bafta is pressed into bath raio:1~6:1 pads
In dressing liquid, two leachings two are rolled, and nip pressure is 0.1~0.25MPa, and it is 100~120% to control liquid carrying rate;
(2) bafta is put into a sealed bored roll device, be pumped in roller storehouse negative pressure value be 0.02~
0.08Mpa, is kept for 3~5 minutes, ventilation to normal pressure;
(3) 0.1~0.3Mpa is forced into arranging storehouse, is kept for 2~5 minutes, removal pressure;
(4) roller is started, 3500~4500r/min of drum rotation speed, centrifugal dewatering 5~8 minutes takes out the fabric;
(5) by bafta at 80~100 DEG C preliminary drying 3~5 minutes, then bake 45~60s at 120~130 DEG C, finally
Through washing, drying and shaping, that is, the bafta after being arranged.
Finally, the present invention also provides the pure cotton fabric after a kind of arrangement using method for sorting as described above, and the pure cotton is knitted
Thing is to staphylococcus aureus bacteriostasis rate>98.2%, to Escherichia coli bacteriostasis rate>92.3%, to Candida albicans bacteriostasis rate>
90.5%, deodorizing rate>97.2%, anti-mite rate>Sterilization, deodorization and anti-mite effect reduced rate are low after 90.6%, and scrubbed 30 times
In 10%.
The advantageous effects that the present invention is obtained:
1) present invention has expanded the purposes of Korean pine phytocide, it is creative propose using Korean pine phytocide as
Textile fabric finishing agent is applied to arrangement to fabric, make it is collated after fabric there are many distinctive effects of Korean pine, tool
There is antibacterial, deodorization, there is repelling and killing efficacy to dust mite, additionally it is possible to which fine solid particle, formaldehyde absorbing in air are removed, it is empty with purification
The effect of gas dust degraded, while specifically there is concentrated force reinforcing to human body, the effect such as immunity and stress reduction is improved;
2) it with the loose alkene (terpene) of the antibiotics of high volatility is material institute structure that Korean pine phytocide main component, which is,
Into its is readily volatilized, and the present invention uses microcapsules technology, is wrapped in its active ingredient as microcapsules core in capsule wall material
Form microcapsule structure of the particle diameter at 0.2-3 μm, using this solve its readily volatilized failure be difficult to sent out as fabric finishing agent
The technical problem of its special efficacy is waved, while Korean pine phytocide can also be made to keep persistently water-fast after arranging to fabric
Washing property.
3) present invention is employed and first taken out when prepared Korean pine phytocide finishing agent is being carried out into Cotton Fabric
Negative pressure supercharging technology means, and pass through the optimum choice of finishing technique parameter again so that Korean pine phytocide can utilize fibre
The absorption affinity produced during dimension surface shrinkage is firmly embedded on fabric, with lasting water-wash resistance, it is ensured that scrubbed
Sterilization, deodorization and anti-mite effect reduced rate are less than 10% after 30 times.
4) Korean pine phytocide finishing agent and preparation method thereof prepared by the present invention and to the method for sorting of fabric, peace
Complete ecological, prepared finishing agent is only with single Korean pine phytocide active ingredient, it is not necessary to multiple with other antimicrobial components
Match somebody with somebody, but the finishing effect to fabric realized by technical solution of the present invention is unexpected, and the finishing agent component is few, prepares
It is simple to operate, knitted wherein adding chitosan crosslinked dose and reaction is crosslinked during fabric post-treatment can adhere to finishing agent
Thing surface, due to the addition of silicone softening agent in finishing agent, the feel of fabric preferably, in addition to yarn dyed fabric washing fastness and is rubbed
Rubbing fastness is almost without influence.
Brief description of the drawings
Below in conjunction with the accompanying drawings and embodiment the invention will be further described:
Fig. 1 is fungistatic effect figure of the bafta after the embodiment of the present invention 1 is arranged to staphylococcus aureus;
Fig. 2 is fungistatic effect figure of the pure cotton fabric after the embodiment of the present invention 2 is arranged to Escherichia coli;
Fig. 3 is fungistatic effect figure of the pure cotton fabric to Candida albicans after the embodiment of the present invention 3 is arranged;
Fig. 4 is fungistatic effect figure of the pure cotton fabric after repeatedly washing to Escherichia coli after the embodiment of the present invention 2 is arranged;
Fungistatic effect figure of the pure cotton fabric after repeatedly washing to Candida albicans after the arrangement of Fig. 5 embodiment of the present invention 2.
Embodiment
Technical scheme is described in detail below by embodiment, it is only the specific of the present invention
Ground embodiment or preferably embodiment, are not thereby limited the scope of the invention.
Embodiment 1
It is whole by extracting Korean pine phytocide, preparation Korean pine phytocide microcapsules, preparation Korean pine phytocide
The process of reason agent and bottling and packaging produces Korean pine phytocide finishing agent to prepare, and then the finishing agent is applied to cotton
In the arrangement of fabric.Preparing Korean pine phytocide finishing agent first includes technique and step in detail below:
(1) extraction of Korean pine phytocide
1.1) branches and leaves for choosing fresh Korean pine plant are used running water to rinse well, are entered after drying by grinder
Row is ground;
1.2) by step 1.1) in crush after the branches and leaves of Korean pine plant insert in distiller and distilled, and reclaim distillation
During vapor;
1.3) by step 1.2) in the vapor that reclaims condensed at 10 DEG C, obtain Korean pine phytocide and water
Mixing liquid;
1.4) by the step 1.3) in mixing liquid filtered, after filtering in the mixing liquid add with should
Mixing liquid volume ratio is 2:1 65wt% ethanol solution carries out extracting and developing and obtains Korean pine phytocide;
(2) preparation of Korean pine phytocide microcapsules
2.1) microcapsule wall material prepolymer is prepared
The mass ratio that urea and formaldehyde are added in a constant volume device is 1:1.1 urea and the aqueous solution of formaldehyde, pass through magnetic
Power agitator makes urea be dissolved in formalin, and it is 7.5 that the NaOH that use quality percentage is 1%, which adjusts its pH value,
Reacted 0.5 hour at a temperature of 60 DEG C, obtain sticky melocol prepolymer A;
2.2) emulsification of Korean pine phytocide core
13 appropriate isomeric alcohol polyethenoxy ether emulsifying agents are added in Korean pine phytocide core to mix with prepolymer
Close and deionized water, by mixed liquor with 3000r/min speed emulsifying 20min, the oil-in-water liquid B stablized;
2.3) polycondensation reaction:By step 2.1) obtained melocol prepolymer A and step 2.2) obtained oil-in-water liquid B
Mixing, is added dropwise acidic catalyst HCl solution, regulation ph value of mixture is 1.5, is heated to 45 DEG C, polycondensation reaction is obtained instead for 2 hours
Answer thing C;
2.4) solidification and suction filtration are dried, by step 2.3) obtained reactant C adds the NaCl that mass fraction is 10%,
Solidify 1 hour at 60 DEG C, it is 7.0 that PH is adjusted after solidification, suction filtration, deionized water washing are carried out after cooling and to be dried to obtain solid-state micro-
The Korean pine phytocide microcapsules of 1~3 μm of grain;
(3) preparation of Korean pine phytocide finishing agent
By step 2.4) prepared by Korean pine phytocide microcapsules, chitosan crosslinked dose, organosilicon flexible finishing agent
And penetrating agent JFC carries out mixing preparation and obtains Korean pine phytocide finishing agent in a reservoir in proportion;Wherein, Korean pine plant kills
Rhzomorph microcapsules consumption 15g/L, chitosan crosslinked dose of consumption 10g/L, organosilicon flexible finishing agent 2g/L, bleeding agent JF 2g/L;
In the embodiment, chitosan crosslinked dose is in chitosan molecule structure after chitosan solution is aoxidized by sodium periodate oxidation agent
The modification shell of middle generation aldehyde radical gathers, and the mol ratio of chitosan glucosides ring and sodium metaperiodate is 1:0.8;
(4) bottle and pack, the Korean pine phytocide finishing agent prepared in step (3) is bottled and packed,
And stored under normal temperature, for being used in textile finishing.
The Korean pine phytocide microcapsules obtained by above-mentioned concrete technology are that core prepared by situ aggregation method is red
The mass ratio of the urea-formaldehyde resin microcapsule of loose phytocide, core Korean pine phytocide quality and wall material Lauxite is 1:
1.5。
Cotton fabrics are arranged using the Korean pine phytocide finishing agent prepared by the present invention, specific finishing technique
Step is as follows:
(1) Korean pine phytocide finishing agent is heated to 55 DEG C, it is 3 that cotton fabrics are pressed into bath raio:1 pads in dressing liquid
In, two leachings two are rolled, and nip pressure is 0.1MPa, and it is 100% to control liquid carrying rate;
(2) cotton fabrics are put into a sealed bored roll device, being pumped to negative pressure value in roller storehouse is
0.02Mpa, is kept for 3 minutes, ventilation to normal pressure;
(3) 0.1Mpa is forced into arranging storehouse, is kept for 2 minutes, removal pressure;
(4) roller is started, drum rotation speed 3500r/mi n, centrifugal dewatering 5 minutes takes out the fabric;
(5) by fabric at 80 DEG C preliminary drying 3 minutes, then bake at 120 DEG C 45s, most afterwards through washing, drying and shaping, i.e.,
Cotton fabrics after being arranged.
Cotton fabrics after being arranged by the present invention, it has Korean pine phytocide natural aromatic, restraining and sterilizing bacteria, deodorization
The effects such as anti-mite, purification air, concentrated force reinforcing, raising immunity and stress reduction, and lasting wash resistant can be kept
Property, go for human body take and household textiles in, the performance test data on its antibiosis anti-acarien is referring to table 1-2.
Embodiment 2
It is whole by extracting Korean pine phytocide, preparation Korean pine phytocide microcapsules, preparation Korean pine phytocide
The process of reason agent and bottling and packaging produces Korean pine phytocide finishing agent to prepare, and then the finishing agent is applied to cotton
In the arrangement of fabric.Preparing Korean pine phytocide finishing agent first includes technique and step in detail below:
(1) extraction of Korean pine phytocide
1.1) branches and leaves for choosing fresh Korean pine plant are used running water to rinse well, are entered after drying by grinder
Row is ground;
1.2) by step 1.1) in crush after the branches and leaves of Korean pine plant insert in distiller and distilled, and reclaim distillation
During vapor;
1.3) by step 1.2) in the vapor that reclaims condensed at 15 DEG C, obtain Korean pine phytocide and water
Mixing liquid;
1.4) by the step 1.3) in mixing liquid filtered, after filtering in the mixing liquid add with should
Mixing liquid volume ratio is 3:1 75wt% ethanol solution carries out extracting and developing and obtains Korean pine phytocide;
(2) preparation of Korean pine phytocide microcapsules
2.1) microcapsule wall material prepolymer is prepared
The mass ratio that urea and formaldehyde are added in a constant volume device is 1:1.8 urea and the aqueous solution of formaldehyde, pass through magnetic
Power agitator makes urea be dissolved in formalin, and it is 8.5 that the NaOH that use quality percentage is 2%, which adjusts its pH value,
Reacted 1 hour at a temperature of 68 DEG C, obtain sticky melocol prepolymer A;
2.2) emulsification of Korean pine phytocide core
Appropriate 13 isomeric alcohol polyethenoxy ethers 1307 and 13 isomery alcohol are added in Korean pine phytocide core
APEO 1305 in mass ratio 1:1 composite emulsifier, is mixed and deionized water with prepolymer, by mixed liquor with 5200r/
Min speed emulsifying 30min, the oil-in-water liquid B stablized;
2.3) polycondensation reaction:By step 2.1) obtained melocol prepolymer A and step 2.2) obtained oil-in-water liquid B
Mixing, is added dropwise acidic catalyst HCl-NH4Cl solution, regulation ph value of mixture is 3.5, is heated to 55 DEG C, polycondensation reaction 3 hours
Obtain reactant C;
2.4) solidification and suction filtration are dried, by step 2.3) obtained reactant C adds the NaCl that mass fraction is 12%,
Solidify 2 hours at 70 DEG C, it is 7.0 that PH is adjusted after solidification, suction filtration, deionized water washing are carried out after cooling and to be dried to obtain solid-state micro-
The Korean pine phytocide microcapsules of 0.6~1 μm of grain;
(3) preparation of Korean pine phytocide finishing agent
By step 2.4) prepared by Korean pine phytocide microcapsules, chitosan crosslinked dose, organosilicon flexible finishing agent
And penetrating agent JFC carries out mixing preparation and obtains Korean pine phytocide finishing agent in a reservoir in proportion;Wherein, Korean pine plant kills
Rhzomorph microcapsules consumption 35g/L, chitosan crosslinked dose of consumption 20g/L, organosilicon flexible finishing agent 6g/L, penetrating agent JFC 2g/
L;In the embodiment, chitosan crosslinked dose be by chitosan solution sodium periodate oxidation agent oxidation after in chitosan molecule structure
The mol ratio of the modification of chitosan of middle generation aldehyde radical, chitosan glucosides ring and sodium metaperiodate is 1:1.2;
(4) bottle and pack, the Korean pine phytocide finishing agent prepared in step (3) is bottled and packed,
And stored under normal temperature, for being used in textile finishing.
The Korean pine phytocide microcapsules obtained by above-mentioned concrete technology are that core prepared by situ aggregation method is red
The mass ratio of the urea-formaldehyde resin microcapsule of loose phytocide, core Korean pine phytocide quality and wall material Lauxite is 1:
2.3。
Because Korean pine phytocide finishing agent its main component prepared by the present invention comes from the branches and leaves of Korean pine plant,
Selection carries out arranging its finishing effect more preferably using pure natural fiber cellulose fiber fabric to it, and the present embodiment is made using the present invention
Standby Korean pine phytocide finishing agent is arranged to pure cotton woven fabric, and specific finishing technique step is as follows:
(1) Korean pine phytocide finishing agent is heated to 60 DEG C, it is 4.5 that pure cotton woven fabric is pressed into bath raio:1 pads whole
Manage in liquid, two leachings two are rolled, and nip pressure is 0.2MPa, it is 110% to control liquid carrying rate;
(2) pure cotton woven fabric is put into a sealed bored roll device, being pumped to negative pressure value in roller storehouse is
0.05Mpa, is kept for 4 minutes, ventilation to normal pressure;
(3) 0.2Mpa is forced into arranging storehouse, is kept for 3 minutes, removal pressure;
(4) roller is started, drum rotation speed 4000r/min, centrifugal dewatering 6 minutes takes out the fabric;
(5) by the fabric at 90 DEG C preliminary drying 4 minutes, then bake at 125 DEG C 55s, most afterwards through washing, drying and shaping,
Pure cotton woven fabric after being arranged.
Cotton fabrics after being arranged by the present invention, it has Korean pine phytocide natural aromatic, restraining and sterilizing bacteria, deodorization
The effects such as anti-mite, purification air, concentrated force reinforcing, raising immunity and stress reduction, and lasting wash resistant can be kept
Property, go for human body take and household textiles in, the performance test data on its antibiosis anti-acarien is referring to table 1-2.
Embodiment 3
It is whole by extracting Korean pine phytocide, preparation Korean pine phytocide microcapsules, preparation Korean pine phytocide
The process of reason agent and bottling and packaging produces Korean pine phytocide finishing agent to prepare, and then the finishing agent is applied to cotton
In the arrangement of fabric.Preparing Korean pine phytocide finishing agent first includes technique and step in detail below:
(1) extraction of Korean pine phytocide
1.1) branches and leaves for choosing fresh Korean pine plant are used running water to rinse well, are entered after drying by grinder
Row is ground;
1.2) by step 1.1) in crush after the branches and leaves of Korean pine plant insert in distiller and distilled, and reclaim distillation
During vapor;
1.3) by step 1.2) in the vapor that reclaims condensed at 20 DEG C, obtain Korean pine phytocide and water
Mixing liquid;
1.4) by the step 1.3) in mixing liquid filtered, after filtering in the mixing liquid add with should
Mixing liquid volume ratio is 5:1 80wt% ethanol solution carries out extracting and developing and obtains Korean pine phytocide;
(2) preparation of Korean pine phytocide microcapsules
2.1) microcapsule wall material prepolymer is prepared
The mass ratio that urea and formaldehyde are added in a constant volume device is 1:2.5 urea and the aqueous solution of formaldehyde, pass through magnetic
Power agitator makes urea be dissolved in formalin, and it is 9.5 that the NaOH that use quality percentage is 2%, which adjusts its pH value,
Reacted 1.5 hours at a temperature of 75 DEG C, obtain sticky melocol prepolymer A;
2.2) emulsification of Korean pine phytocide core
13 appropriate isomeric alcohol polyethenoxy ether emulsifying agents are added in Korean pine phytocide core to mix with prepolymer
Close and deionized water, by mixed liquor with 7500r/min speed emulsifying 25min, the oil-in-water liquid B stablized;
2.3) polycondensation reaction:By step 2.1) obtained melocol prepolymer A and step 2.2) obtained oil-in-water liquid B
Mixing, is added dropwise acidic catalyst HCl-NH4Cl solution, regulation ph value of mixture is 5.0, is heated to 65 DEG C, polycondensation reaction 4 hours
Obtain reactant C;
2.4) solidification and suction filtration are dried, by step 2.3) obtained reactant C adds the NaCl that mass fraction is 15%,
Solidify 3 hours at 80 DEG C, it is 7.0 that PH is adjusted after solidification, suction filtration, deionized water washing are carried out after cooling and to be dried to obtain solid-state micro-
The Korean pine phytocide microcapsules of 0.2~1 μm of grain;
(3) preparation of Korean pine phytocide finishing agent
By step 2.4) prepared by Korean pine phytocide microcapsules, chitosan crosslinked dose, organosilicon flexible finishing agent
Carry out mixing preparation in a reservoir in proportion and obtain Korean pine phytocide finishing agent;Wherein, Korean pine phytocide microcapsules
Consumption 40g/L, chitosan crosslinked dose of consumption 35g/L, organosilicon flexible finishing agent 8g/L, bleeding agent JF 3g/L;The embodiment
In, chitosan crosslinked dose be by chitosan solution by potassium chlorate it is oxidizing after in chitosan molecule structure generate aldehyde radical
Modification of chitosan, the mol ratio of chitosan glucosides ring and potassium chlorate is 1:1;
(4) bottle and pack, the Korean pine phytocide finishing agent prepared in step (3) is bottled and packed,
And stored under normal temperature, for being used in textile finishing.
The Korean pine phytocide microcapsules obtained by above-mentioned concrete technology are that core prepared by situ aggregation method is red
The mass ratio of the urea-formaldehyde resin microcapsule of loose phytocide, core Korean pine phytocide quality and wall material Lauxite is 1:
2.8。
Because Korean pine phytocide finishing agent its main component prepared by the present invention comes from the branches and leaves of Korean pine plant,
Selection carries out arranging its finishing effect more preferably using pure natural fiber cellulose fiber fabric to it, and the present embodiment is made using the present invention
Standby Korean pine phytocide finishing agent is equally arranged to pure cotton woven fabric, and specific finishing technique step is as follows:
(1) Korean pine phytocide finishing agent is heated to 65 DEG C, it is 6 that pure cotton woven fabric is pressed into bath raio:1 pads in arrangement
In liquid, two leachings two are rolled, and nip pressure is 0.25MPa, and it is 120% to control liquid carrying rate;
(2) pure cotton woven fabric is put into a sealed bored roll device, being pumped to negative pressure value in roller storehouse is
0.08Mpa, is kept for 5 minutes, ventilation to normal pressure;
(3) 0.3Mpa is forced into arranging storehouse, is kept for 5 minutes, removal pressure;
(4) roller is started, drum rotation speed 4500r/min, centrifugal dewatering 8 minutes takes out the fabric;
(5) by the fabric at 100 DEG C preliminary drying 5 minutes, then bake at 130 DEG C 60s, most afterwards through washing, drying and shaping,
Pure cotton woven fabric after being arranged.
Cotton fabrics after being arranged by the present invention, it has Korean pine phytocide natural aromatic, restraining and sterilizing bacteria, deodorization
The effects such as anti-mite, purification air, concentrated force reinforcing, raising immunity and stress reduction, and lasting wash resistant can be kept
Property, go for human body take and household textiles in, the performance test data on its antibiosis anti-acarien is referring to table 1-2.
Fabric test after embodiment 1-3 arrangements
The Korean pine phytocide finishing agent prepared using the present invention is carried out after repairing experiment to bafta, according to country's mark
Quasi- GB/T 20944-2007 test to the antibacterial effect of the fabric after present invention arrangement, and its fabric is to golden yellow grape ball
There is excellent restraining and sterilizing bacteria to imitate for bacterium (AATCC6538), Escherichia coli (AATCC8739) and Candida albicans (AATCC10231)
Really, and to ammonia, yellow water is plain, and methyl mercaptan etc. has good deodorizing effect, has preferable anti-mite effect to acarid, specifically
Test experiments data such as following table:
The Korean pine phytocide finishing agent of table 1 bafta is arranged after effect
Using standard GB/T/T20944.3-2008《The evaluation third portion of antibacterial textile performance:Succusion》Carry out
Antibiotic property quantitative test, using color fastness to washing testing machine washing methods, the bafta after being arranged to 1-3 of the embodiment of the present invention
Repeatedly washed, the bafta antibacterial effect (partial test the results are shown in Table 2) tested after washing 30 times carries out Durable antibacterial
Found after experiment, the bafta after being arranged through the present invention is organized in fabric due to Korean pine phytocide in the way of microcapsules
On, sterilization, deodorization and anti-mite and other effects reduced rate are below 10% after it is washed through 30 times, and accompanying drawing 4-5 shows that embodiment 2 is whole
Escherichia coli, the antibacterial effect of Candida albicans respectively when pure cotton fabric after reason wash the 25-30 times.
Effect of the Korean pine phytocide finishing agent of table 2 after being arranged to bafta after multiple washing
Embodiment and experiment institute test result above for technical solution of the present invention, for those skilled in the art
These embodiments are changed, changed, replaced, integrated and work by speech without departing from the principles and spirit of the present invention
Skill parameter modification is each fallen within protection scope of the present invention.
Claims (10)
1. a kind of Korean pine phytocide finishing agent, it is characterised in that the formula of the finishing agent is as follows:
2. Korean pine phytocide finishing agent according to claim 1, it is characterised in that the Korean pine phytocide is micro-
Capsule is prepared by situ aggregation method, the urea-formaldehyde resin microcapsule that core is Korean pine phytocide, core Korean pine plant sterilization
The mass ratio of element and wall material Lauxite is 1:1.5~3.0.
3. Korean pine phytocide finishing agent according to claim 1 or 2, it is characterised in that described chitosan crosslinked dose
It is by generating the modification of chitosan of aldehyde radical after oxidizing in chitosan molecule structure by chitosan solution.
4. the preparation method of the Korean pine phytocide finishing agent according to claim any one of 1-3, it is characterised in that should
Method comprises the following steps:
(1) extraction of Korean pine phytocide
1.1) branches and leaves for choosing Korean pine plant are rinsed well, are ground after drying;
1.2) by step 1.1) in crush after the branches and leaves of Korean pine plant insert in distiller and distilled, and reclaim still-process
In vapor;
1.3) by step 1.2) in the vapor that reclaims condensed at 5~20 DEG C, obtain Korean pine phytocide and water
Mixing liquid;
1.4) by the step 1.3) in mixing liquid filtered, add and mixed with this in the mixing liquid after filtering
Liquid volume ratio is 2:1~5:1 60wt%~80wt% ethanol solution carries out extracting and developing and obtains Korean pine plant sterilization
Element;
(2) preparation of Korean pine phytocide microcapsules
2.1) microcapsule wall material prepolymer is prepared
The mass ratio that urea and formaldehyde are added in a constant volume device is 1:1.1~2.5 urea and the aqueous solution of formaldehyde, pass through magnetic
Power agitator makes urea be dissolved in formalin, and the NaOH that use quality percentage is 1%~3% adjusts its pH value and is
7.5~9.5, reacted 0.5 hour~1.5 hours at a temperature of 60-75 DEG C, obtain sticky melocol prepolymer A;
2.2) emulsification of Korean pine phytocide core
A certain amount of 13 isomeric alcohol polyethenoxy ether emulsifying agent is added in Korean pine phytocide core to mix with prepolymer
And deionized water, by mixed liquor with 3000~7500r/min speed 20~30min of emulsifying, the oil-in-water stablized
Liquid B;
2.3) polycondensation reaction:By step 2.1) obtained melocol prepolymer A and step 2.2) obtained oil-in-water liquid B mixes,
Acidic catalyst is added dropwise, regulation ph value of mixture is 1.5~5.0, is heated to 45~65 DEG C, polycondensation reaction is obtained instead for 1-4 hours
Answer thing C;
2.4) solidification and suction filtration are dried, by step 2.3) obtained reactant C adds the NaCl that mass fraction is 8~15%,
Solidify 1~3 hour at 60~80 DEG C, it is neutrality that PH is adjusted after solidification, suction filtration, deionized water washing and dry are carried out after cooling
To the Korean pine phytocide microcapsules of solid;
(3) preparation of Korean pine phytocide finishing agent
By step 2.4) prepared by Korean pine phytocide microcapsules, chitosan crosslinked dose, organosilicon flexible finishing agent and ooze
Saturating agent JFC carries out mixing preparation in a reservoir in the ratio of the formula, obtains Korean pine phytocide finishing agent;
(4) bottle and pack
The Korean pine phytocide finishing agent prepared in step (3) is bottled and packed, and under normal temperature store, for
Used during textile finishing.
5. the preparation method of Korean pine phytocide finishing agent according to claim 4, it is characterised in that the step
1.4) ethanol in is the ethanol solution that volumetric concentration is 70-80%, and more preferably volumetric concentration is 75% ethanol solution.
6. the preparation method of the Korean pine phytocide finishing agent according to claim 4 or 5, it is characterised in that the step
It is rapid 2.2) in the 13 isomeric alcohol polyethenoxy ether emulsifying agent be 13 isomeric alcohol polyethenoxy ethers 1307 and 13 isomeries
Alcohol APEO 1305 in mass ratio 1:1 composite emulsifier.
7. the preparation method of the Korean pine phytocide finishing agent according to claim 4 or 5, it is characterised in that the step
It is rapid 2.1) in urea and formaldehyde mass ratio be 1:1.8, pH value is 8.5, and reaction temperature is 68 DEG C, and the time is 1 hour, the step
It is rapid 2.3) in mixed liquor pH value be 3.5.
8. the application of the Korean pine phytocide finishing agent according to claim any one of 1-3, it is characterised in that for pair
The Final finishing of bafta.
9. the Korean pine phytocide finishing agent according to claim any one of 1-3 is to the method for sorting of bafta, it is special
Levy and be, the method for sorting comprises the following steps:
(1) Korean pine phytocide finishing agent is heated to 55~65 DEG C, it is 3 that bafta is pressed into bath raio:1~6:1 pads whole
Manage in liquid, two leachings two are rolled, and nip pressure is 0.1~0.25MPa, it is 100~120% to control liquid carrying rate;
(2) bafta is put into a sealed bored roll device, be pumped in roller storehouse negative pressure value be 0.02~
0.08Mpa, is kept for 3~5 minutes, ventilation to normal pressure;
(3) 0.1~0.3Mpa is forced into arranging storehouse, is kept for 2~5 minutes, removal pressure;
(4) roller is started, 3500~4500r/min of drum rotation speed, centrifugal dewatering 5~8 minutes takes out the fabric;
(5) by bafta at 80~100 DEG C preliminary drying 3~5 minutes, then 45~60s is baked at 120~130 DEG C, most afterwards through water
Wash, drying and shaping, that is, the bafta after being arranged.
10. the bafta after method for sorting arrangement according to claim 9, it is characterised in that the bafta is to golden yellow
Staphylococcus bacteriostasis rate>98.2%, to Escherichia coli bacteriostasis rate>92.3%, to Candida albicans bacteriostasis rate>90.5%, deodorization
Rate>97.2%, anti-mite rate>Sterilization, deodorization and anti-mite effect reduced rate are less than 10% after 90.6%, and scrubbed 30 times.
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