CN108078035A - Protective garment - Google Patents

Protective garment Download PDF

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Publication number
CN108078035A
CN108078035A CN201711325143.XA CN201711325143A CN108078035A CN 108078035 A CN108078035 A CN 108078035A CN 201711325143 A CN201711325143 A CN 201711325143A CN 108078035 A CN108078035 A CN 108078035A
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CN
China
Prior art keywords
small
solid
aloe
woven fabric
revs
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CN201711325143.XA
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Chinese (zh)
Inventor
袁强
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Xiantao Tripod Labour Protection Products Co Ltd
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Xiantao Tripod Labour Protection Products Co Ltd
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Priority to CN201711325143.XA priority Critical patent/CN108078035A/en
Publication of CN108078035A publication Critical patent/CN108078035A/en
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    • AHUMAN NECESSITIES
    • A41WEARING APPAREL
    • A41DOUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
    • A41D13/00Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches
    • AHUMAN NECESSITIES
    • A41WEARING APPAREL
    • A41DOUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
    • A41D31/00Materials specially adapted for outerwear
    • A41D31/04Materials specially adapted for outerwear characterised by special function or use
    • A41D31/30Antimicrobial, e.g. antibacterial
    • A41D31/305Antimicrobial, e.g. antibacterial using layered materials
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C231/00Preparation of carboxylic acid amides
    • C07C231/02Preparation of carboxylic acid amides from carboxylic acids or from esters, anhydrides, or halides thereof by reaction with ammonia or amines
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C231/00Preparation of carboxylic acid amides
    • C07C231/12Preparation of carboxylic acid amides by reactions not involving the formation of carboxamide groups
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C46/00Preparation of quinones
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/08Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/28Preparation of carboxylic acid esters by modifying the hydroxylic moiety of the ester, such modification not being an introduction of an ester group
    • C07C67/29Preparation of carboxylic acid esters by modifying the hydroxylic moiety of the ester, such modification not being an introduction of an ester group by introduction of oxygen-containing functional groups
    • 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
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/12Aldehydes; Ketones
    • D06M13/123Polyaldehydes; Polyketones
    • 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
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/152Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen having a hydroxy group bound to a carbon atom of a six-membered aromatic ring
    • 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
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/61Polyamines polyimines
    • 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
    • D06M16/00Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
    • 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
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/18Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/20Polyalkenes, polymers or copolymers of compounds with alkenyl groups bonded to aromatic groups

Abstract

The invention discloses a kind of protective garment, the protective garment includes inner layer and outer layer, and the inner layer is non-woven fabrics, and the outer layer is coating or coating prepared by nonwoven surface.Protective garment of the present invention have the characteristics that ventilative, anti-asbestos penetrate, waterproof, antibacterial it is wear-resisting, be mainly used in the environment such as hospital, farm, Center for Disease Control, oil drilling, toilet workshop.

Description

Protective garment
Technical field
The invention belongs to protection technology fields, and in particular to a kind of protective garment.
Background technology
Hospital, farm, Center for Disease Control, oil drilling, toilet workshop etc. in environment, operating personnel need Protective garment is dressed, the purpose is to isolate human body with external environment.
The patent of invention of Application No. 201611254768.7 discloses a kind of PTFE protective garments, is used to prepare FTIE protection Clothes are formed by three kinds of Material claddings, including PTFE fabric surface layer, intermediate PTFE film layer and terylene/nylon fabric inner layer;Institute It is compound through hot pressing using hot melt adhesive to state compound.The present invention is using the surface layer of composite material is made in PTFE fabric, PTFE film is made The inner layer of composite material is made in the middle level of composite material, terylene/nylon fabric;This trilaminate material is compound by hot melt adhesive hot pressing A kind of new material is made afterwards;The protective garment of this material preparation alternatively full protection rubber suit of the prior art, and with light Just, breathe freely, bury, etch-proof feature.
The application for a patent for invention of Application No. CN200710094115.1 discloses a kind of industrial fire retardant protective clothing fabric And its manufacturing method and protective garment, the industrial fire retardant protective clothing fabric yarn are fine by anti-flaming viscose, wool fiber and nylon Tie up it is blended form, the blending rate (weight) for stating anti-flaming viscose, wool fiber and nylon fiber is respectively 45-55%, 35- 45%, 5-15%.Fire retardant protective clothing fabric before the electric welding and metallurgical smelting furnace has permanent fire-retardant, high temperature resistant, resists The invention of the functions such as advection heat, fusion proof metal liquid splash is not only suitable in fire-entry suit, flight fighting uniform etc., is reached if desired for forever Long property is fire-retardant, it is heat safe simultaneously, be also applied for needing electric welding and the metallurgy of the functions such as anti-advection heat, fusion proof metal liquid splash Fire retardant protective clothing fabric requirement before smelting furnace.
The content of the invention
For above-mentioned deficiency in the prior art, the first technical problem to be solved by the present invention is to provide a kind of anti- Shield clothes.
The present invention seeks to what is be achieved through the following technical solutions:
The invention discloses a kind of protective garment, the protective garment includes inner layer and outer layer, and the inner layer is non-woven fabrics, described Outer layer is the coating or coating prepared in the nonwoven surface.
In some embodiments of the invention, the non-woven fabrics is polypropylene non-woven fabric.
Polypropylene non-woven fabric with stronger mechanical strength and larger specific surface area due to being widely used in protective garment Base fabric.But polypropylene non-woven fabric does not have the performance of antibacterial in itself, and it is sterile in hospital, farm etc. can not to meet protective garment The application in place.Aloe-emodin is the active material with antibacterial and antivirus action being widely present in a kind of nature. Inventor attempts aloe-emodin or Aloe emodin derivative being grafted on by covalently bonded mode poly- in the present invention The surface of propylene non-woven fabrics.Inventor utilizes glutaraldehyde and polyethyleneimine absorption-covalent manner, is given birth to by Maillard reaction Into schiff base structure, effectively by aloe-emodin or Aloe emodin derivative scion grafting on polypropylene non-woven fabric, formed There is the non-woven fabrics of antibacterial functions.
In some embodiments of the invention, the non-woven fabrics is grafting aloe-emodin or Aloe emodin derivative Polypropylene non-woven fabric.
The preparation process of polypropylene non-woven fabric of the grafting aloe-emodin or Aloe emodin derivative is:
(1) when immersion 12-24 is small in the hydrochloric acid for being 4-6mol/L in molar concentration by polypropylene non-woven fabric, polypropylene non-woven The solid-to-liquid ratio of cloth and hydrochloric acid is 1:(10-20) (g/mL) takes out polypropylene non-woven fabric, with 50-200 times of polypropylene non-woven fabric weight Deionized water cleaning, when 50-60 DEG C of dry 8-12 is small;
(2) it is 0.01-0.03mg/ aloe-emodin or Aloe emodin derivative to be configured to concentration with absolute ethyl alcohol The solution of mL;
(3) polypropylene non-woven fabric and mass fraction obtained step (1) is the glutaraldehyde water solution of 20-25% with solid-liquid Than 1:(0.02-0.05) (g/mL) is mixed, and is stirred 60-120 minutes, taken out with 120-150 revs/min of rotating speed in 80-90 DEG C Polypropylene non-woven fabric is cleaned with 50-200 times of deionized water of polypropylene non-woven fabric weight, when 50-60 DEG C of dry 8-12 is small;
(4) polypropylene non-woven fabric for obtaining step (3) and mass fraction are the aq. polyethyleneimine of 5-6% with solid Liquor ratio 1:(0.02-0.05) (g/mL) is mixed, and is stirred 60-120 minutes, taken with 120-150 revs/min of rotating speed in 30-40 DEG C Go out polypropylene non-woven fabric, cleaned with 50-200 times of deionized water of polypropylene non-woven fabric weight, it is small in 50-60 DEG C of dry 8-12 When;
(5) the aloe-emodin solution or aloe obtained the polypropylene non-woven fabric that step (4) obtains and step (2) is big Flavin derivatives solution is with solid-to-liquid ratio 1:(0.02-0.05) (g/mL) is mixed, in 30-40 DEG C with 120-150 revs/min of rotating speed When stirring 10-12 is small, polypropylene non-woven fabric is taken out;
(6) it is the polypropylene non-woven fabric that step (5) obtains is clear with the absolute ethyl alcohol of 50-80 times of polypropylene non-woven fabric weight It washes, is then cleaned with the deionized water of 50-200 times of polypropylene non-woven fabric weight, when 50-60 DEG C of dry 8-12 is small, obtain institute State grafting aloe-emodin or the polypropylene non-woven fabric of Aloe emodin derivative.
The Aloe emodin derivative for Aloe emodin derivative I, one kind in Aloe emodin derivative II or Composition.
The preparation process of the Aloe emodin derivative I is:By aloe-emodin and Anhydrous potassium carbonate with mass ratio 1: (10-11) is mixed;The solid-to-liquid ratio of addition anhydrous propanone and dimethyl suflfate, Anhydrous potassium carbonate and anhydrous propanone is 1:(80-90) (g/mL), the molar ratio of Anhydrous potassium carbonate and dimethyl suflfate is 1:(1-1.2) is warming up to 50-60 DEG C, in 50-60 after mixing DEG C reaction 12-15 it is small when;After reaction, reaction solution is removed into acetone, obtains residue;Residue weight is added in into residue The water of 0.6-0.8 times of amount is stirred 20-30 minutes with 230-280 revs/min of rotating speed;Using 80-100 mesh filter-cloth filterings, collect Filter cake;After filter cake is washed with deionized, the solid-to-liquid ratio of filter cake and deionized water is 1:(80-120) (g/mL), in 50-60 DEG C, when dry 6-10 is small under conditions of vacuum degree 0.07-0.09MPa, obtain the Aloe emodin derivative I.
The preparation process of the Aloe emodin derivative II is:
(1) by aloe-emodin and pyridine with solid-to-liquid ratio 1:(30-50) (g/mL) mix, add in acetic anhydride, acetic anhydride and The volume ratio of pyridine is 1:(2-3), in 40-50 DEG C with 260-320 revs/min of rotating speed be stirred to react 15-24 it is small when;It has reacted Cheng Hou pours into reaction solution in ice water, and solid is precipitated, and using 80-100 mesh filter-cloth filterings, collects filter cake;By filter cake deionization The solid-to-liquid ratio of water washing, filter cake and deionized water is 1:(50-80) (g/mL), in 50-60 DEG C, vacuum degree 0.07-0.09MPa Under the conditions of dry 6-10 it is small when, obtain solid A;
(2) by solid A, acetic anhydride and glacial acetic acid with ratio 1:5:(40-50) (g/mL/mL) mix, 260-320 turn/ The chromium trioxide of 1-1.5 times of solid A mass and the deionization of 0.4-0.5 times of acetic anhydride volume are added under the stirring condition of minute Water, in 90-100 DEG C with 260-320 revs/min be stirred to react 5-7 it is small when;After reaction, reaction solution is poured into ice water, analysed Go out solid, using 80-100 mesh filter-cloth filterings, collect filter cake;After filter cake is washed with deionized, filter cake and deionized water Solid-to-liquid ratio is 1:(50-80) (g/mL) when dry 6-10 is small under conditions of 50-60 DEG C, vacuum degree 0.07-0.09MPa, is obtained Solid B;
(3) by 1,8- diacetyls -3- carboxyls anthraquinone and anhydrous dimethyl formamide with solid-to-liquid ratio 1:(8-10)(g/mL) Mixing adds in the Glucosamine hydrochlorate of 1-1.2 times of 1,8- diacetyl -3- carboxyl anthraquinones quality and 1,8- diacetyl -3- The dicyclohexylcarbodiimide of 0.5-0.6 times of carboxyl anthraquinone quality is stirred to react in 23-25 DEG C with 200-300 revs/min When 20-24 is small;After reaction, reaction solution is collected into filtrate using 80-100 mesh filter-cloth filterings;Anhydrous two are added in into filtrate The glacial acetic acid of 0.05-0.06 times of methylformamide volume mixes and stands 30-40 minutes after 0-2 DEG C, using 80-100 mesh filter clothes Filtrate is collected in filtering;The water of 0.5-0.8 times of filtrate volume is added in into filtrate, when 20-25 DEG C of standing 5-10 is small, using 80- 100 mesh filter-cloth filterings collect filter cake;Filter cake is chromatographed using silicagel column, mobile phase is by ethyl acetate and hexamethylene with body Product is than (0.7-0.8):1 mixes, and collects eluent;By eluent in 50-60 DEG C, the condition of vacuum degree 0.07-0.09MPa When lower dry 6-10 is small, the Aloe emodin derivative II is obtained.
Inventor has found in practice process, is grafted the anti-microbial property of the polypropylene non-woven fabric of Aloe emodin derivative II Better than grafting aloe-emodin or the polypropylene non-woven fabric of Aloe emodin derivative I.This may be due to aloe-emodin Hydroxyl on derivative II on Han You Onion Huan , Onion rings has certain contribution function for antibacterial effect.
Among the prior art, usually the mechanical property of coating and wear-resisting property etc. are improved by adding inorganic particulate.But Be inorganic particulate additive amount it is more, be more unfavorable for the adhesiving effect of coating.This invention address that it provides a kind of with good viscous The coating of attached effect and very good mechanical properties.
In the present invention, it is in the process of nonwoven surface prepares coating:
(1) formulation for coating material:Functional particles 17-20%, organic bond 20-30wt%, mass fraction are 5% six inclined phosphorus Acid sodium aqueous solution 1-2wt%, surplus are dimethylformamide;
(2) dimethylformamide of dimethylformamide total amount 60-70% is weighed, functional particles are added in, with 400-500 Rev/min rotating speed stir 20-30 minute, add in mass fraction be 5% sodium hexametaphosphate solution, continue with 400-500 Rev/min rotating speed stir 30-40 minutes, obtain mixed liquor I;
(3) organic bond with remaining dimethylformamide is mixed, 10- is stirred with 400-500 revs/min of rotating speed After twenty minutes, 30-40 minutes are stood in 20-25 DEG C, obtains mixed liquor II;
(4) mixed liquor I that step (2) obtains is added in the mixed liquor II that step (3) obtains, with 400-500 revs/min The rotating speed of clock stirs 20-30 minutes, obtains coating;
(5) by coating by way of padding coated in nonwoven surface, the solid-to-liquid ratio of non-woven fabrics and coating is 1:(20- 30) (g/mL) is dried 3-5 minutes in 90-100 DEG C;Non-woven fabrics is subjected to secondary coating, non-woven fabrics and painting by way of padding The solid-to-liquid ratio of material is 1:(20-30) (g/mL) is dried 3-5 minutes in 90-100 DEG C;By non-woven fabrics non-woven weight 50-200 Times deionized water washing, when dry 8-12 is small under conditions of 50-60 DEG C, vacuum degree 0.07-0.08MPa to get.
The polyethers that the functional particles are montmorillonite-dimethyl silicone polymer functional particles, silica-DOPA is amine-modified One kind or its composition in sulfone functional particles.Preferably, the functional particles are montmorillonite-dimethyl silicone polymer function grain The mixture of son and the amine-modified polyether sulfone functional particles of silica-DOPA, wherein montmorillonite-dimethyl silicone polymer function The mass ratio of particle and the amine-modified polyether sulfone functional particles of silica-DOPA is 1:(2-3).
The preparation process of the montmorillonite-dimethyl silicone polymer functional particles is:By absolute ethyl alcohol, deionized water, 3- Aminopropyltriethoxywerene werene is with weight ratio (15-20):1:1 is uniformly mixed, and obtains mixed liquor;By mixeding liquid volume 0.01- 0.02 times of dimethyl silicone polymer is added in mixed liquor, is handled under conditions of 45-50 DEG C, ultrasonic power 300-400W 30-50 minutes, obtain sonification fluid;The illiteracy that 0.5-0.7 times of dimethyl silicone polymer weight is added in into sonification fluid takes off Soil, in the rotating speed of 45-50 DEG C, 210-300 revs/min be stirred to react 12-15 it is small when;After the completion of reaction, reaction solution is used into 80- 100 mesh filter-cloth filterings collect filter cake;After filter cake is washed with the deionized water of 50-100 times of filter cake weight, in 50-60 DEG C, it is true When drying 6-10 is small under conditions of reciprocal of duty cycle 0.07-0.09MPa, the montmorillonite-dimethyl silicone polymer functional particles are obtained.
For dopamine after polyether sulfone surface aggregate, the poly-dopamine of generation can freely be coated on the table of arbitrary solid matter Face, and non-covalent bond effect power is generated, enhance the combination power between dopamine and substance, while substantial amounts of reactivity is provided Position.Under the catalytic action of ammonium hydroxide, the silanol for being dehydrated generation can occur to take off tetraethyl orthosilicate with the hydroxyl on dopamine surface Water reacts, so as to achieve the purpose that growth in situ nano silicon dioxide.This not only contributes to adherency of the functional particles in base fabric, Being cross-linked with each other between particle is also beneficial to, enhances the interface cohesion effect between polymer.
The preparation process of the amine-modified polyether sulfone functional particles of the silica-DOPA is:Using trihydroxy methyl amino The PH of deionized water is adjusted to 8.5 by methane;By dopamine and the deionized water of pH is mixed up with solid-to-liquid ratio 1:(400-500)(g/ ML) it is uniformly mixed, adds in the polyether sulfone of 50-60 times of dopamine weight, 20-24 is stirred to react with 200-300 revs/min of rotating speed Hour;By reaction solution using 80-100 mesh filter-cloth filterings, filter cake is collected;By filter cake in 70-80 DEG C, vacuum degree 0.06-0.08MPa Under conditions of dry 8-10 it is small when, obtain the amine-modified polyether sulfone of DOPA;By the amine-modified polyether sulfone of DOPA and absolute ethyl alcohol with Solid-to-liquid ratio 1:(8-12) (g/mL) is uniformly mixed, and is ultrasonically treated 20-30 minutes under conditions of ultrasonic power 300-400W, by nothing The ammonium hydroxide that the concentration of 0.01-0.02 times of water-ethanol volume is 25-28% adds in, and is uniformly mixed and obtains mixed liquor A;By ammonium hydroxide volume 0.9-1 times of tetraethyl orthosilicate and the absolute ethyl alcohol of 20-30 times of ammonium hydroxide volume are uniformly mixed, and obtain mixed liquid B;By mixed liquor B is added in mixed liquor A, with 200-300 revs/min of rotating speed be stirred to react 20-25 it is small when;By reaction solution in 50-55 DEG C, it is true When drying 10-16 is small under conditions of reciprocal of duty cycle 0.06-0.08MPa, the amine-modified polyether sulfone function of the silica-DOPA is obtained Particle.
Protective garment of the present invention have the characteristics that ventilative, anti-asbestos penetrate, waterproof, antibacterial it is wear-resisting, be mainly used in doctor The environment such as institute, farm, Center for Disease Control, oil drilling, toilet workshop.
Specific embodiment
Each raw material introduction in embodiment:
Polypropylene non-woven fabric, purchased from the southern seven star non-woven fabrics Co., Ltd in Guangzhou, ingredient is polypropylene, article No. NQX, gram Weight is 75g/cm2
Aloe-emodin, No. CAS:481-72-1 is provided by Shaanxi Pa Nier bio tech ltd.
Anhydrous potassium carbonate, No. CAS:584-08-7 is provided by scientific and technological (Jiangsu) Co., Ltd of China's chemistry forever.
Pyridine, No. CAS:110-86-1 is provided by Anhui gracefulness Chemical Co., Ltd..
Acetic anhydride, No. CAS:108-24-7 is provided by Nantong Dong Hua Chemical Co., Ltd.s.
Chromium trioxide, No. CAS:1333-82-0, the chemicals Co., Ltd offer that shines together of being shone by Wuhan peak.
1,8- diacetyl -3- carboxyl anthraquinones, No. CAS:13739-02-1 is provided by Xi'an Kang Nuo Chemical Co., Ltd.s.
The preparation process of aminoglucose hydrochloride is:By hydrochloric acid that chitosan and mass fraction are 37% with solid-to-liquid ratio 1: 15 (g/mL) mix, in the rotating speed of 100 DEG C, 260 revs/min be stirred to react 3 it is small when, obtain reaction solution;It is added in into reaction solution The deionized water that 1 times of hydrochloric acid volume with 260 revs/min of rotating speed stirring after twenty minutes, using 80 mesh filter-cloth filterings, collects filter Liquid;By filtrate when drying 8 is small under conditions of 50 DEG C, vacuum degree 0.07MPa, aminoglucose hydrochloride is obtained.
Chitosan, No. CAS:9012-76-4, is provided by Shanghai Industry Co., Ltd in future, and deacetylated degree is 95%.
Anhydrous dimethyl formamide is provided by the graceful bio tech ltd of upper Hypon.
Dicyclohexylcarbodiimide, No. CAS:538-75-0 is provided by Suzhou Highfine Biotech Co., Ltd..
Glacial acetic acid, No. CAS:64-19-7 is provided by Henan Wei Yuan bio tech ltd.
Organic bond, specific polyurethane binder provided using Heng Ye trade Co., Ltds of Foshan City.
Montmorillonite is provided, smectite content 65%, apparent viscosity 600mPa by Lingshou County Dong Bang mineral powders factory s。
Dimethyl silicone polymer, No. CAS:9016-00-6 is provided, product by AlfaAesar (China) Chemical Co., Ltd. Number is 042501, MW 6000.
3-aminopropyltriethoxysilane, No. CAS:919-30-2 is provided by Chemical Industry Co., Ltd. of earth of Hangzhou.
Trishydroxymethylaminomethane, No. CAS:77-86-1 is provided by Suzhou subfamily Science and Technology Co., Ltd..
Polyether sulfone, No. CAS:9002-88-4 is provided, product identification by Shanghai Aladdin biochemical technology limited company For P119576, melt flow rate (MFR) 6.98g/10min.
Dopamine, No. CAS:51-61-6 is provided by Shanghai Lan Ke medical sci-teches Development Co., Ltd.
Tetraethyl orthosilicate, No. CAS:562-90-3 is provided by Shanghai Ji Laide new materials Science and Technology Ltd..
Embodiment 1
The protective garment includes inner layer and outer layer, and the inner layer is polypropylene non-woven fabric, and the outer layer is polypropylene non-woven Coating prepared by cloth surface.
It is in the process of nonwoven surface prepares coating:
(1) formulation for coating material:Montmorillonite-dimethyl silicone polymer functional particles 17wt%, organic bond 20wt%, quality Fraction is 5% sodium hexametaphosphate solution 2wt%, and surplus is dimethylformamide;
(2) dimethylformamide of dimethylformamide total amount 60% is weighed, functional particles are added in, with 400 revs/min Rotating speed stirs 20 minutes, adds in the sodium hexametaphosphate solution that mass fraction is 5%, continues the rotating speed stirring with 400 revs/min 30 minutes, obtain mixed liquor I;
(3) organic bond with remaining dimethylformamide is mixed, is stirred 10 minutes with 400 revs/min of rotating speed Afterwards, 30 minutes are stood in 25 DEG C, obtains mixed liquor II;
(4) mixed liquor I that step (2) obtains is added in the mixed liquor II that step (3) obtains, with 400 revs/min Rotating speed stirs 20 minutes, obtains coating;
(5) by coating by way of padding coated in nonwoven surface, the solid-to-liquid ratio of non-woven fabrics and coating is 1:20(g/ ML), dried 5 minutes in 90 DEG C;Non-woven fabrics is subjected to secondary coating by way of padding, the solid-to-liquid ratio of non-woven fabrics and coating is 1:20 (g/mL) are dried 5 minutes in 90 DEG C;Non-woven fabrics is washed with the deionized water of 200 times of non-woven weight, in 60 DEG C, it is true Under conditions of reciprocal of duty cycle 0.07MPa it is dry 8 it is small when to get.
The preparation process of the montmorillonite-dimethyl silicone polymer functional particles is:By absolute ethyl alcohol, deionized water, 3- Aminopropyltriethoxywerene werene is with weight ratio 16:1:1 is uniformly mixed, and obtains mixed liquor;By 0.02 times gather of mixeding liquid volume Dimethyl siloxane is added in mixed liquor, is handled 40 minutes, is ultrasonically treated under conditions of 45 DEG C, ultrasonic power 300W Liquid;The montmorillonite of 0.5 times of dimethyl silicone polymer weight is added in into sonification fluid, in 45 DEG C, 210 revs/min of rotating speed Be stirred to react 14 it is small when;After the completion of reaction, by reaction solution using 80 mesh filter-cloth filterings, filter cake is collected;By filter cake filter cake weight After 70 times of deionized water washing, under conditions of 55 DEG C, vacuum degree 0.07MPa it is dry 8 it is small when, obtain the montmorillonite-poly- Dimethyl siloxane functional particles.
Embodiment 2
The protective garment includes inner layer and outer layer, and the inner layer is described to be grafted the polypropylene non-woven fabric of aloe-emodin The coating that outer layer is prepared for the polypropylene non-woven fabric surface of grafting aloe-emodin.
The preparation process of polypropylene non-woven fabric of the grafting aloe-emodin is:
(1) by polypropylene non-woven fabric molar concentration be 6mol/L hydrochloric acid in impregnate 24 it is small when, polypropylene non-woven fabric and The solid-to-liquid ratio of hydrochloric acid is 1:10 (g/mL) take out polypropylene non-woven fabric, clear with 200 times of deionized water of polypropylene non-woven fabric weight It washes, when 50 DEG C of dryings 8 are small, the impurity on removal polypropylene non-woven fabric surface;
(2) aloe-emodin is configured to the solution that concentration is 0.01mg/mL with absolute ethyl alcohol;
(3) glutaraldehyde water solution that the polypropylene non-woven fabric and mass fraction obtained step (1) is 20% is with solid-to-liquid ratio 1:0.03 (g/mL) is mixed, and is stirred 120 minutes with 150 revs/min of rotating speed in 90 DEG C, polypropylene non-woven fabric is taken out, with poly- third The deionized water cleaning that 200 times of alkene non-woven weight, when 50 DEG C of dryings 8 are small;
(4) aq. polyethyleneimine that the polypropylene non-woven fabric for obtaining step (3) and mass fraction are 6% is with solid-liquid Than 1:0.03 (g/mL) is mixed, it is stirred 60 minutes with 150 revs/min of rotating speed in 40 DEG C, takes out polypropylene non-woven fabric, with poly- The deionized water cleaning that 200 times of propylene non-woven weight, when 50 DEG C of dryings 8 are small;
(5) the aloe-emodin solution that the polypropylene non-woven fabric for obtaining step (4) is obtained with step (2) is with solid-to-liquid ratio 1: 0.02 (g/mL) is mixed, when 30 DEG C small with 150 revs/min of rotating speed stirring 12, make aloe-emodin be fixed on polypropylene without In woven fabric, polypropylene non-woven fabric is taken out;
(6) by the polypropylene non-woven fabric that step (5) the obtains washes of absolute alcohol of 80 times of polypropylene non-woven fabric weight, so Cleaned afterwards with the deionized water of 200 times of polypropylene non-woven fabric weight, in 50 DEG C it is dry 8 it is small when, obtain the grafting aloe rheum officinale The polypropylene non-woven fabric of element.
It is in the process of nonwoven surface prepares coating:
(1) formulation for coating material:Montmorillonite-dimethyl silicone polymer functional particles 17wt%, organic bond 20wt%, quality Fraction is 5% sodium hexametaphosphate solution 2wt%, and surplus is dimethylformamide;
(2) dimethylformamide of dimethylformamide total amount 60% is weighed, functional particles are added in, with 400 revs/min Rotating speed stirs 20 minutes, adds in the sodium hexametaphosphate solution that mass fraction is 5%, continues the rotating speed stirring with 400 revs/min 30 minutes, obtain mixed liquor I;
(3) organic bond with remaining dimethylformamide is mixed, is stirred 10 minutes with 400 revs/min of rotating speed Afterwards, 30 minutes are stood in 25 DEG C, obtains mixed liquor II;
(4) mixed liquor I that step (2) obtains is added in the mixed liquor II that step (3) obtains, with 400 revs/min Rotating speed stirs 20 minutes, obtains coating;
(5) by coating by way of padding coated in nonwoven surface, the solid-to-liquid ratio of non-woven fabrics and coating is 1:20(g/ ML), dried 5 minutes in 90 DEG C;Non-woven fabrics is subjected to secondary coating by way of padding, the solid-to-liquid ratio of non-woven fabrics and coating is 1:20 (g/mL) are dried 5 minutes in 90 DEG C;Non-woven fabrics is washed with the deionized water of 200 times of non-woven weight, in 60 DEG C, it is true Under conditions of reciprocal of duty cycle 0.07MPa it is dry 8 it is small when to get.
The preparation process of the montmorillonite-dimethyl silicone polymer functional particles is:By absolute ethyl alcohol, deionized water, 3- Aminopropyltriethoxywerene werene is with weight ratio 16:1:1 is uniformly mixed, and obtains mixed liquor;By 0.02 times gather of mixeding liquid volume Dimethyl siloxane is added in mixed liquor, is handled 40 minutes, is ultrasonically treated under conditions of 45 DEG C, ultrasonic power 300W Liquid;The montmorillonite of 0.5 times of dimethyl silicone polymer weight is added in into sonification fluid, in 45 DEG C, 210 revs/min of rotating speed Be stirred to react 14 it is small when;After the completion of reaction, by reaction solution using 80 mesh filter-cloth filterings, filter cake is collected;By filter cake filter cake weight After 70 times of deionized water washing, under conditions of 55 DEG C, vacuum degree 0.07MPa it is dry 8 it is small when, obtain the montmorillonite-poly- Dimethyl siloxane functional particles.
Embodiment 3
The protective garment includes inner layer and outer layer, and the inner layer is the polypropylene non-woven of grafting Aloe emodin derivative I Cloth, the coating that the outer layer is prepared for the polypropylene non-woven fabric surface of grafting Aloe emodin derivative I.
The preparation process of polypropylene non-woven fabric of the grafting Aloe emodin derivative I is:
(1) by polypropylene non-woven fabric molar concentration be 6mol/L hydrochloric acid in impregnate 24 it is small when, polypropylene non-woven fabric and The solid-to-liquid ratio of hydrochloric acid is 1:10 (g/mL) take out polypropylene non-woven fabric, clear with 200 times of deionized water of polypropylene non-woven fabric weight It washes, when 50 DEG C of dryings 8 are small, the impurity on removal polypropylene non-woven fabric surface;
(2) Aloe emodin derivative I is configured to the solution that concentration is 0.01mg/mL with absolute ethyl alcohol;
(3) glutaraldehyde water solution that the polypropylene non-woven fabric and mass fraction obtained step (1) is 20% is with solid-to-liquid ratio 1:0.03 (g/mL) is mixed, and is stirred 120 minutes with 150 revs/min of rotating speed in 90 DEG C, polypropylene non-woven fabric is taken out, with poly- third The deionized water cleaning that 200 times of alkene non-woven weight, when 50 DEG C of dryings 8 are small;
(4) aq. polyethyleneimine that the polypropylene non-woven fabric for obtaining step (3) and mass fraction are 6% is with solid-liquid Than 1:0.03 (g/mL) is mixed, it is stirred 60 minutes with 150 revs/min of rotating speed in 40 DEG C, takes out polypropylene non-woven fabric, with poly- The deionized water cleaning that 200 times of propylene non-woven weight, when 50 DEG C of dryings 8 are small;
(5) I solution of Aloe emodin derivative that the polypropylene non-woven fabric for obtaining step (4) and step (2) obtain with Solid-to-liquid ratio 1:0.02 (g/mL) is mixed, and when 30 DEG C small with 150 revs/min of rotating speed stirring 12, makes Aloe emodin derivative I It is fixed on polypropylene non-woven fabric, takes out polypropylene non-woven fabric;
(6) by the polypropylene non-woven fabric that step (5) the obtains washes of absolute alcohol of 80 times of polypropylene non-woven fabric weight, so Cleaned afterwards with the deionized water of 200 times of polypropylene non-woven fabric weight, in 50 DEG C it is dry 8 it is small when, obtain the grafting aloe rheum officinale The polypropylene non-woven fabric of plain derivatives I.
The preparation process of the Aloe emodin derivative I is:By aloe-emodin and Anhydrous potassium carbonate with mass ratio 1: 10 mixing;The solid-to-liquid ratio of addition anhydrous propanone and dimethyl suflfate, Anhydrous potassium carbonate and anhydrous propanone is 1:90 (g/mL), it is anhydrous The molar ratio of potassium carbonate and dimethyl suflfate is 1:1,60 DEG C are warming up to after mixing, when 60 DEG C of reactions 15 are small;After reaction, Reaction solution is removed into acetone, obtains residue;The water of 0.8 times of residue weight is added in into residue, with 230 revs/min Rotating speed stirs 20 minutes;Using 100 mesh filter-cloth filterings, filter cake is collected;After filter cake is washed with deionized, filter cake and deionization The solid-to-liquid ratio of water is 1:90 (g/mL) when drying 8 is small under conditions of 50 DEG C, vacuum degree 0.07MPa, obtain the aloe rheum officinale Plain derivatives I.
It is in the process of nonwoven surface prepares coating:
(1) formulation for coating material:Montmorillonite-dimethyl silicone polymer functional particles 17wt%, organic bond 20wt%, quality Fraction is 5% sodium hexametaphosphate solution 2wt%, and surplus is dimethylformamide;
(2) dimethylformamide of dimethylformamide total amount 60% is weighed, functional particles are added in, with 400 revs/min Rotating speed stirs 20 minutes, adds in the sodium hexametaphosphate solution that mass fraction is 5%, continues the rotating speed stirring with 400 revs/min 30 minutes, obtain mixed liquor I;
(3) organic bond with remaining dimethylformamide is mixed, is stirred 10 minutes with 400 revs/min of rotating speed Afterwards, 30 minutes are stood in 25 DEG C, obtains mixed liquor II;
(4) mixed liquor I that step (2) obtains is added in the mixed liquor II that step (3) obtains, with 400 revs/min Rotating speed stirs 20 minutes, obtains coating;
(5) by coating by way of padding coated in nonwoven surface, the solid-to-liquid ratio of non-woven fabrics and coating is 1:20(g/ ML), dried 5 minutes in 90 DEG C;Non-woven fabrics is subjected to secondary coating by way of padding, the solid-to-liquid ratio of non-woven fabrics and coating is 1:20 (g/mL) are dried 5 minutes in 90 DEG C;Non-woven fabrics is washed with the deionized water of 200 times of non-woven weight, in 60 DEG C, it is true Under conditions of reciprocal of duty cycle 0.07MPa it is dry 8 it is small when to get.
The preparation process of the montmorillonite-dimethyl silicone polymer functional particles is:By absolute ethyl alcohol, deionized water, 3- Aminopropyltriethoxywerene werene is with weight ratio 16:1:1 is uniformly mixed, and obtains mixed liquor;By 0.02 times gather of mixeding liquid volume Dimethyl siloxane is added in mixed liquor, is handled 40 minutes, is ultrasonically treated under conditions of 45 DEG C, ultrasonic power 300W Liquid;The montmorillonite of 0.5 times of dimethyl silicone polymer weight is added in into sonification fluid, in 45 DEG C, 210 revs/min of rotating speed Be stirred to react 14 it is small when;After the completion of reaction, by reaction solution using 80 mesh filter-cloth filterings, filter cake is collected;By filter cake filter cake weight After 70 times of deionized water washing, under conditions of 55 DEG C, vacuum degree 0.07MPa it is dry 8 it is small when, obtain the montmorillonite-poly- Dimethyl siloxane functional particles.
Embodiment 4
The protective garment includes inner layer and outer layer, and the inner layer is the polypropylene non-woven of grafting Aloe emodin derivative II Cloth, the coating that the outer layer is prepared for the polypropylene non-woven fabric surface of grafting Aloe emodin derivative II.
The preparation process of polypropylene non-woven fabric of the grafting Aloe emodin derivative II is:
(1) by polypropylene non-woven fabric molar concentration be 6mol/L hydrochloric acid in impregnate 24 it is small when, polypropylene non-woven fabric and The solid-to-liquid ratio of hydrochloric acid is 1:10 (g/mL) take out polypropylene non-woven fabric, clear with 200 times of deionized water of polypropylene non-woven fabric weight It washes, when 50 DEG C of dryings 8 are small, the impurity on removal polypropylene non-woven fabric surface;
(2) Aloe emodin derivative II is configured to the solution that concentration is 0.01mg/mL with absolute ethyl alcohol;
(3) glutaraldehyde water solution that the polypropylene non-woven fabric and mass fraction obtained step (1) is 20% is with solid-to-liquid ratio 1:0.03 (g/mL) is mixed, and is stirred 120 minutes with 150 revs/min of rotating speed in 90 DEG C, polypropylene non-woven fabric is taken out, with poly- third The deionized water cleaning that 200 times of alkene non-woven weight, when 50 DEG C of dryings 8 are small;
(4) aq. polyethyleneimine that the polypropylene non-woven fabric for obtaining step (3) and mass fraction are 6% is with solid-liquid Than 1:0.03 (g/mL) is mixed, and is stirred 60 minutes with 150 revs/min of rotating speed in 40 DEG C, polypropylene non-woven fabric is taken out, with poly- third The deionized water cleaning that 200 times of alkene non-woven weight, when 50 DEG C of dryings 8 are small;
(5) II solution of Aloe emodin derivative that the polypropylene non-woven fabric for obtaining step (4) and step (2) obtain with Solid-to-liquid ratio 1:0.02 (g/mL) is mixed, and when 30 DEG C small with 150 revs/min of rotating speed stirring 12, makes Aloe emodin derivative II is fixed on polypropylene non-woven fabric, takes out polypropylene non-woven fabric;
(6) by the polypropylene non-woven fabric that step (5) the obtains washes of absolute alcohol of 80 times of polypropylene non-woven fabric weight, so Cleaned afterwards with the deionized water of 200 times of polypropylene non-woven fabric weight, in 50 DEG C it is dry 8 it is small when, obtain the grafting aloe rheum officinale The polypropylene non-woven fabric of plain derivative II.
The preparation process of the Aloe emodin derivative II is:
(1) by aloe-emodin and pyridine with solid-to-liquid ratio 1:30 (g/mL) mixing, addition acetic anhydride, acetic anhydride and pyridine Volume ratio is 1:2, in 45 DEG C with 260 revs/min of rotating speed be stirred to react 20 it is small when;After the completion of reaction, reaction solution is poured into ice In water, solid is precipitated, using 100 mesh filter-cloth filterings, collects filter cake;Filter cake is washed with deionized, filter cake and deionized water Solid-to-liquid ratio be 1:80 (g/mL) when drying 10 is small under conditions of 50 DEG C, vacuum degree 0.07MPa, obtain solid A;
(2) by solid A, acetic anhydride and glacial acetic acid with ratio 1:5:40 (g/mL/mL) are mixed, in 260 revs/min of stirring Under the conditions of add in the chromium trioxide of 1.3 times of solid A mass and the deionized water of 0.4 times of acetic anhydride volume, in 90 DEG C with 260 turns/ When minute reaction 5 is small;After reaction, reaction solution is poured into ice water, solid is precipitated, using 100 mesh filter-cloth filterings, collect filter Cake;After filter cake is washed with deionized, the solid-to-liquid ratio of filter cake and deionized water is 1:80 (g/mL), in 50 DEG C, vacuum degree When drying 10 is small under conditions of 0.07MPa, solid B is obtained;
(3) by 1,8- diacetyls -3- carboxyls anthraquinone and anhydrous dimethyl formamide with solid-to-liquid ratio 1:8 (g/mL) are mixed, Add in the Glucosamine hydrochlorate of 1.2 times of 1,8- diacetyl -3- carboxyl anthraquinones quality and 1,8- diacetyl -3- carboxyl anthraquinones The dicyclohexylcarbodiimide that 0.5 times of quality, in 25 DEG C with 300 revs/min of rotating speed be stirred to react 24 it is small when;Reaction terminates Afterwards, reaction solution is collected into filtrate using 80 mesh filter-cloth filterings;0.05 times of anhydrous dimethyl formamide volume is added in into filtrate Glacial acetic acid mixes and stands 30 minutes after 0 DEG C, using 80 mesh filter-cloth filterings, collects filtrate;Filtrate volume is added in into filtrate 0.7 times of water when 25 DEG C of standings 10 are small, using 80 mesh filter-cloth filterings, collects filter cake;Filter cake is subjected to layer using silicagel column Analysis, mobile phase is by ethyl acetate and hexamethylene with volume ratio 0.8:1 mixes, and collects eluent;By eluent in 50 DEG C, it is true When drying 10 is small under conditions of reciprocal of duty cycle 0.07MPa, the Aloe emodin derivative II is obtained.
It is in the process of nonwoven surface prepares coating:
(1) formulation for coating material:Montmorillonite-dimethyl silicone polymer functional particles 17wt%, organic bond 20wt%, quality Fraction is 5% sodium hexametaphosphate solution 2wt%, and surplus is dimethylformamide;
(2) dimethylformamide of dimethylformamide total amount 60% is weighed, functional particles are added in, with 400 revs/min Rotating speed stirs 20 minutes, adds in the sodium hexametaphosphate solution that mass fraction is 5%, continues the rotating speed stirring with 400 revs/min 30 minutes, obtain mixed liquor I;
(3) organic bond with remaining dimethylformamide is mixed, is stirred 10 minutes with 400 revs/min of rotating speed Afterwards, 30 minutes are stood in 25 DEG C, obtains mixed liquor II;
(4) mixed liquor I that step (2) obtains is added in the mixed liquor II that step (3) obtains, with 400 revs/min Rotating speed stirs 20 minutes, obtains coating;
(5) by coating by way of padding coated in nonwoven surface, the solid-to-liquid ratio of non-woven fabrics and coating is 1:20(g/ ML), dried 5 minutes in 90 DEG C;Non-woven fabrics is subjected to secondary coating by way of padding, the solid-to-liquid ratio of non-woven fabrics and coating is 1:20 (g/mL) are dried 5 minutes in 90 DEG C;Non-woven fabrics is washed with the deionized water of 200 times of non-woven weight, in 60 DEG C, it is true Under conditions of reciprocal of duty cycle 0.07MPa it is dry 8 it is small when to get.
The preparation process of the montmorillonite-dimethyl silicone polymer functional particles is:By absolute ethyl alcohol, deionized water, 3- Aminopropyltriethoxywerene werene is with weight ratio 16:1:1 is uniformly mixed, and obtains mixed liquor;By 0.02 times gather of mixeding liquid volume Dimethyl siloxane is added in mixed liquor, is handled 40 minutes, is ultrasonically treated under conditions of 45 DEG C, ultrasonic power 300W Liquid;The montmorillonite of 0.5 times of dimethyl silicone polymer weight is added in into sonification fluid, in 45 DEG C, 210 revs/min of rotating speed Be stirred to react 14 it is small when;After the completion of reaction, by reaction solution using 80 mesh filter-cloth filterings, filter cake is collected;By filter cake filter cake weight After 70 times of deionized water washing, under conditions of 55 DEG C, vacuum degree 0.07MPa it is dry 8 it is small when, obtain the montmorillonite-poly- Dimethyl siloxane functional particles.
Embodiment 5
The protective garment includes inner layer and outer layer, and the inner layer is the polypropylene non-woven of grafting Aloe emodin derivative II Cloth, the coating that the outer layer is prepared for the polypropylene non-woven fabric surface of grafting Aloe emodin derivative II.
The preparation process and embodiment 4 of the polypropylene non-woven fabric of the grafting Aloe emodin derivative II are identical, herein It repeats no more.
It is in the process of nonwoven surface prepares coating:
(1) formulation for coating material:The amine-modified polyether sulfone functional particles 17wt% of silica-DOPA, organic bond 20wt%, mass fraction are 5% sodium hexametaphosphate solution 2wt%, and surplus is dimethylformamide;
(2) dimethylformamide of dimethylformamide total amount 60% is weighed, functional particles are added in, with 400 revs/min Rotating speed stirs 20 minutes, adds in the sodium hexametaphosphate solution that mass fraction is 5%, continues the rotating speed stirring with 400 revs/min 30 minutes, obtain mixed liquor I;
(3) organic bond with remaining dimethylformamide is mixed, is stirred 10 minutes with 400 revs/min of rotating speed Afterwards, 30 minutes are stood in 25 DEG C, obtains mixed liquor II;
(4) mixed liquor I that step (2) obtains is added in the mixed liquor II that step (3) obtains, with 400 revs/min Rotating speed stirs 20 minutes, obtains coating;
(5) by coating by way of padding coated in nonwoven surface, the solid-to-liquid ratio of non-woven fabrics and coating is 1:20(g/ ML), dried 5 minutes in 90 DEG C;Non-woven fabrics is subjected to secondary coating by way of padding, the solid-to-liquid ratio of non-woven fabrics and coating is 1:20 (g/mL) are dried 5 minutes in 90 DEG C;Non-woven fabrics is washed with the deionized water of 200 times of non-woven weight, in 60 DEG C, it is true Under conditions of reciprocal of duty cycle 0.07MPa it is dry 8 it is small when to get.
The preparation method of the amine-modified polyether sulfone functional particles of the silica-DOPA is:Using trihydroxy methyl amino The PH of deionized water is adjusted to 8.5 by methane;By dopamine and the deionized water of pH is mixed up with solid-to-liquid ratio 1:400 (g/mL) are mixed Uniformly, add in the polyether sulfone of 50 times of dopamine weight, with 300 revs/min of rotating speed be stirred to react 22 it is small when;Reaction solution is used 80 mesh filter-cloth filterings collect filter cake;By filter cake when drying 10 is small under conditions of 70 DEG C, vacuum degree 0.06MPa, dopamine is obtained The polyether sulfone of modification;By the amine-modified polyether sulfone of DOPA and absolute ethyl alcohol with solid-to-liquid ratio 1:8 (g/mL) are uniformly mixed, in ultrasonic work( It is ultrasonically treated 20 minutes, the ammonium hydroxide that 0.01 times of concentration of absolute ethyl alcohol volume is 25% is added in, mixing under conditions of rate 300W Uniformly obtain mixed liquor A;The absolute ethyl alcohol of 20 times of the tetraethyl orthosilicate of 1 times of ammonium hydroxide volume and ammonium hydroxide volume is uniformly mixed, Obtain mixed liquid B;Mixed liquid B is added in mixed liquor A, with 300 revs/min of rotating speed be stirred to react 24 it is small when;It will reaction Liquid obtains the amine-modified polyether sulfone of the silica-DOPA when drying 12 is small under conditions of 50 DEG C, vacuum degree 0.08MPa Functional particles.
Embodiment 6
The protective garment includes inner layer and outer layer, and the inner layer is the polypropylene non-woven of grafting Aloe emodin derivative II Cloth, the coating that the outer layer is prepared for the polypropylene non-woven fabric surface of grafting Aloe emodin derivative II.
The preparation process and embodiment 4 of the polypropylene non-woven fabric of the grafting Aloe emodin derivative II are identical, herein It repeats no more.
It is in the process of nonwoven surface prepares coating:
(1) formulation for coating material:Montmorillonite-dimethyl silicone polymer functional particles 5wt%, silica-DOPA are amine-modified Polyether sulfone functional particles 12wt%, organic bond 20wt%, mass fraction is 5% sodium hexametaphosphate solution 2wt%, remaining It measures as dimethylformamide;
(2) dimethylformamide of dimethylformamide total amount 60% is weighed, functional particles are added in, with 400 revs/min Rotating speed stirs 20 minutes, adds in the sodium hexametaphosphate solution that mass fraction is 5%, continues the rotating speed stirring with 400 revs/min 30 minutes, obtain mixed liquor I;
(3) organic bond with remaining dimethylformamide is mixed, is stirred 10 minutes with 400 revs/min of rotating speed Afterwards, 30 minutes are stood in 25 DEG C, obtains mixed liquor II;
(4) mixed liquor I that step (2) obtains is added in the mixed liquor II that step (3) obtains, with 400 revs/min Rotating speed stirs 20 minutes, obtains coating;
(5) by coating by way of padding coated in nonwoven surface, the solid-to-liquid ratio of non-woven fabrics and coating is 1:20(g/ ML), dried 5 minutes in 90 DEG C;Non-woven fabrics is subjected to secondary coating by way of padding, the solid-to-liquid ratio of non-woven fabrics and coating is 1:20 (g/mL) are dried 5 minutes in 90 DEG C;Non-woven fabrics is washed with the deionized water of 200 times of non-woven weight, in 60 DEG C, it is true Under conditions of reciprocal of duty cycle 0.07MPa it is dry 8 it is small when to get.
The preparation process of the montmorillonite-dimethyl silicone polymer functional particles is:By absolute ethyl alcohol, deionized water, 3- Aminopropyltriethoxywerene werene is with weight ratio 16:1:1 is uniformly mixed, and obtains mixed liquor;By 0.02 times gather of mixeding liquid volume Dimethyl siloxane is added in mixed liquor, is handled 40 minutes, is ultrasonically treated under conditions of 45 DEG C, ultrasonic power 300W Liquid;The montmorillonite of 0.5 times of dimethyl silicone polymer weight is added in into sonification fluid, in 45 DEG C, 210 revs/min of rotating speed Be stirred to react 14 it is small when;After the completion of reaction, by reaction solution using 80 mesh filter-cloth filterings, filter cake is collected;By filter cake filter cake weight After 70 times of deionized water washing, under conditions of 55 DEG C, vacuum degree 0.07MPa it is dry 8 it is small when, obtain the montmorillonite-poly- Dimethyl siloxane functional particles.
The preparation method of the amine-modified polyether sulfone functional particles of the silica-DOPA is:Using trihydroxy methyl amino The PH of deionized water is adjusted to 8.5 by methane;By dopamine and the deionized water of pH is mixed up with solid-to-liquid ratio 1:400 (g/mL) are mixed Uniformly, add in the polyether sulfone of 50 times of dopamine weight, with 300 revs/min of rotating speed be stirred to react 22 it is small when;Reaction solution is used 80 mesh filter-cloth filterings collect filter cake;By filter cake when drying 10 is small under conditions of 70 DEG C, vacuum degree 0.06MPa, dopamine is obtained The polyether sulfone of modification;By the amine-modified polyether sulfone of DOPA and absolute ethyl alcohol with solid-to-liquid ratio 1:8 (g/mL) are uniformly mixed, in ultrasonic work( It is ultrasonically treated 20 minutes, the ammonium hydroxide that 0.01 times of concentration of absolute ethyl alcohol volume is 25% is added in, mixing under conditions of rate 300W Uniformly obtain mixed liquor A;The absolute ethyl alcohol of 20 times of the tetraethyl orthosilicate of 1 times of ammonium hydroxide volume and ammonium hydroxide volume is uniformly mixed, Obtain mixed liquid B;Mixed liquid B is added in mixed liquor A, with 300 revs/min of rotating speed be stirred to react 24 it is small when;It will reaction Liquid obtains the amine-modified polyether sulfone of the silica-DOPA when drying 12 is small under conditions of 50 DEG C, vacuum degree 0.08MPa Functional particles.
Test case 1
The antibiotic rate of non-woven fabrics to being used in embodiment 2-4 is tested:
Nutrient agar:0.5% peptone, 0.3% beef extract and 0.5% sodium chloride and 1.5% agar, with distillation The boil-off solution of boiling, pH 7.
Nutrient broth medium:0.5% peptone, 0.3% beef extract and 0.5% sodium chloride boil dissolving with distilled water, PH is 7.
Bacteria suspension:Strain (ATCC) is weighed in nutrient agar culture with oese, is dissolved in nutrient broth medium, It is 1-9 × 10 to prepare strain concentration6The bacteria suspension of cfu/mL.
The non-woven fabrics of embodiment 2-4 and the non-woven fabrics of embodiment 1 that area is 1cmx1cm are respectively placed in containing 2mL's In the sterilizing test tubes of nutrient broth medium, 10mL bacteria suspensions are added in, in 37 DEG C with 150 revs/min of speed oscillation culture 24 Hour;By cultivate 24 it is small when after nonwoven sample take out, take out the nutrient broth medium that 0.1mL culture solutions add in 0.9mL Do gradient dilution.Then the culture solution of 0.1mL is taken to be placed on nutrient agar surface, it is hooked coated on nutrient agar Culture medium.After when 37 DEG C of cultures 24 are small, the strain number on nutrient agar is calculated.It is anti-that it is calculated by following formula Bacterium rate:R (%)=(logA-logB)/logA.
In formula:A is the cfu//mL after the non-woven fabrics culture of embodiment 2-4;After B is the non-woven fabrics culture of embodiment 1 Strain concentration c fu//mL.
Specific test result is shown in Table 1.
Table 1:Bacteriostasis property test result table
Test case 2
The cutting resistance of the protective garment of embodiment 1-6 is tested, with reference to JIS T 8051:2005 carry out, sample A diameter of 55mm is needled into speed as 100mm/min.Each embodiment takes four samples, takes its average value as test result.
Specific test result is shown in Table 2.
Table 2:Cutting resistance test result table
Test case 3
The gas permeability of the protective garment of embodiment 1-6 is tested, according to 8.26 gas permeability A method (the not thunders of JIS-L1096 Damp type Frazir methods) it is measured.
Specific test result is shown in Table 3.
Table 3:Permeability test result table
From table 3 it can be seen that the air permeability of protective garment of the present invention is all in 10cm3/cm2During more than sec, have good Good gas permeability.

Claims (9)

1. protective garment, which is characterized in that the protective garment includes inner layer and outer layer, and the inner layer is non-woven fabrics, and the outer layer is In coating or coating prepared by the nonwoven surface.
2. protective garment according to claim 1, which is characterized in that the non-woven fabrics is polypropylene non-woven fabric.
3. protective garment according to claim 1, which is characterized in that the non-woven fabrics is grafting aloe-emodin or aloe The polypropylene non-woven of the polypropylene non-woven fabric of emodin derivates, the grafting aloe-emodin or Aloe emodin derivative The preparation process of cloth is:
(1) by polypropylene non-woven fabric molar concentration be 4-6mol/L hydrochloric acid in impregnate 12-24 it is small when, polypropylene non-woven fabric and The solid-to-liquid ratio of hydrochloric acid is 1:(10-20) (g/mL) takes out polypropylene non-woven fabric, with 50-200 times go of polypropylene non-woven fabric weight Ionized water cleans, when 50-60 DEG C of dry 8-12 is small;
(2) it is 0.01-0.03mg/mL's aloe-emodin or Aloe emodin derivative to be configured to concentration with absolute ethyl alcohol Solution;
(3) polypropylene non-woven fabric and mass fraction obtained step (1) is the glutaraldehyde water solution of 20-25% with solid-to-liquid ratio 1: (0.02-0.05) (g/mL) is mixed, and is stirred 60-120 minutes with 120-150 revs/min of rotating speed in 80-90 DEG C, is taken out poly- third Alkene non-woven fabrics is cleaned with 50-200 times of deionized water of polypropylene non-woven fabric weight, when 50-60 DEG C of dry 8-12 is small;
(4) polypropylene non-woven fabric for obtaining step (3) and mass fraction are the aq. polyethyleneimine of 5-6% with solid-to-liquid ratio 1:(0.02-0.05) (g/mL) is mixed, and is stirred 60-120 minutes with 120-150 revs/min of rotating speed in 30-40 DEG C, is taken out poly- Propylene non-woven fabrics is cleaned with 50-200 times of deionized water of polypropylene non-woven fabric weight, when 50-60 DEG C of dry 8-12 is small;
(5) the aloe-emodin solution or aloe-emodin that the polypropylene non-woven fabric for obtaining step (4) is obtained with step (2) Derivative solution is with solid-to-liquid ratio 1:(0.02-0.05) (g/mL) is mixed, and is stirred in 30-40 DEG C with 120-150 revs/min of rotating speed When 10-12 is small, polypropylene non-woven fabric is taken out;
(6) by the polypropylene non-woven fabric that step (5) the obtains washes of absolute alcohol of 50-80 times of polypropylene non-woven fabric weight, so It is cleaned afterwards with the deionized water of 50-200 times of polypropylene non-woven fabric weight, when 50-60 DEG C of dry 8-12 is small, obtains the grafting The polypropylene non-woven fabric of aloe-emodin or Aloe emodin derivative.
4. protective garment according to claim 3, which is characterized in that the Aloe emodin derivative is spread out for aloe-emodin Biology I, one kind in Aloe emodin derivative II or composition.
5. protective garment according to claim 4, which is characterized in that the preparation process of the Aloe emodin derivative I is: By aloe-emodin and Anhydrous potassium carbonate with mass ratio 1:(10-11) is mixed;Add in anhydrous propanone and dimethyl suflfate, anhydrous carbon The solid-to-liquid ratio of sour potassium and anhydrous propanone is 1:The molar ratio of (80-90) (g/mL), Anhydrous potassium carbonate and dimethyl suflfate is 1:(1- 1.2) 50-60 DEG C, is warming up to after mixing, when 50-60 DEG C of reaction 12-15 is small;After reaction, reaction solution is removed into acetone, Obtain residue;The water of 0.6-0.8 times of residue weight is added in into residue, is stirred with 230-280 revs/min of rotating speed 20-30 minutes;Using 80-100 mesh filter-cloth filterings, filter cake is collected;After filter cake is washed with deionized, filter cake and deionized water Solid-to-liquid ratio be 1:(80-120) (g/mL), when dry 6-10 is small under conditions of 50-60 DEG C, vacuum degree 0.07-0.09MPa, Obtain the Aloe emodin derivative I.
6. protective garment according to claim 4, which is characterized in that the preparation process of the Aloe emodin derivative II For:
(1) by aloe-emodin and pyridine with solid-to-liquid ratio 1:(30-50) (g/mL) is mixed, and adds in acetic anhydride, acetic anhydride and pyridine Volume ratio be 1:(2-3), in 40-50 DEG C with 260-320 revs/min of rotating speed be stirred to react 15-24 it is small when;Reaction is completed Afterwards, reaction solution is poured into ice water, solid is precipitated, using 80-100 mesh filter-cloth filterings, collect filter cake;By filter cake deionized water The solid-to-liquid ratio of washing, filter cake and deionized water is 1:(50-80) (g/mL), in 50-60 DEG C, the item of vacuum degree 0.07-0.09MPa When drying 6-10 is small under part, solid A is obtained;
(2) by solid A, acetic anhydride and glacial acetic acid with ratio 1:5:(40-50) (g/mL/mL) is mixed, at 260-320 revs/min Stirring condition under add in the chromium trioxide of 1-1.5 times of solid A mass and the deionized water of 0.4-0.5 times of acetic anhydride volume, in 90-100 DEG C with 260-320 revs/min be stirred to react 5-7 it is small when;After reaction, reaction solution is poured into ice water, be precipitated solid Body using 80-100 mesh filter-cloth filterings, collects filter cake;After filter cake is washed with deionized, the solid-liquid of filter cake and deionized water Than for 1:(50-80) (g/mL) when dry 6-10 is small under conditions of 50-60 DEG C, vacuum degree 0.07-0.09MPa, obtains solid B;
(3) by 1,8- diacetyls -3- carboxyls anthraquinone and anhydrous dimethyl formamide with solid-to-liquid ratio 1:(8-10) (g/mL) is mixed, Add in the Glucosamine hydrochlorate of 1-1.2 times of 1,8- diacetyl -3- carboxyl anthraquinones quality and 1,8- diacetyl -3- carboxyl anthracenes The dicyclohexylcarbodiimide of 0.5-0.6 times of quinone quality, in 23-25 DEG C with 200-300 revs/min to be stirred to react 20-24 small When;After reaction, reaction solution is collected into filtrate using 80-100 mesh filter-cloth filterings;Anhydrous dimethyl Ji Jia is added in into filtrate The glacial acetic acid of 0.05-0.06 times of amide volume mixes and stands 30-40 minutes after 0-2 DEG C, using 80-100 mesh filter-cloth filterings, Collect filtrate;The water of 0.5-0.8 times of filtrate volume is added in into filtrate, when 20-25 DEG C of standing 5-10 is small, using 80-100 mesh Filter-cloth filtering collects filter cake;Filter cake is chromatographed using silicagel column, mobile phase is by ethyl acetate and hexamethylene with volume ratio (0.7-0.8):1 mixes, and collects eluent;Eluent is done under conditions of 50-60 DEG C, vacuum degree 0.07-0.09MPa When dry 6-10 is small, the Aloe emodin derivative II is obtained.
7. protective garment according to claim 1, which is characterized in that be in the process of the nonwoven surface prepares coating:
(1) formulation for coating material:Functional particles 17-20%, organic bond 20-30wt%, mass fraction are 5% calgon Aqueous solution 1-2wt%, surplus are dimethylformamide;
(2) dimethylformamide of dimethylformamide total amount 60-70% is weighed, functional particles are added in, with 400-500 revs/min The rotating speed of clock stirs 20-30 minutes, adds in the sodium hexametaphosphate solution that mass fraction is 5%, continues with 400-500 revs/min The rotating speed of clock stirs 30-40 minutes, obtains mixed liquor I;
(3) organic bond is mixed with remaining dimethylformamide, with 400-500 revs/min of 10-20 points of rotating speed stirring Zhong Hou stands 30-40 minutes in 20-25 DEG C, obtains mixed liquor II;
(4) mixed liquor I that step (2) obtains is added in the mixed liquor II that step (3) obtains, with 400-500 revs/min Rotating speed stirs 20-30 minutes, obtains coating;
(5) by coating by way of padding coated in nonwoven surface, the solid-to-liquid ratio of non-woven fabrics and coating is 1:(20-30) (g/mL), dried 3-5 minutes in 90-100 DEG C;Non-woven fabrics is subjected to secondary coating, non-woven fabrics and coating by way of padding Solid-to-liquid ratio be 1:(20-30) (g/mL) is dried 3-5 minutes in 90-100 DEG C;By 50-200 times of non-woven weight of non-woven fabrics Deionized water washing, when dry 8-12 is small under conditions of 50-60 DEG C, vacuum degree 0.07-0.08MPa to get.
8. protective garment according to claim 7, which is characterized in that the functional particles are montmorillonite-polydimethylsiloxanes Alkoxyl functional particle, the preparation process of the montmorillonite-dimethyl silicone polymer functional particles are:By absolute ethyl alcohol, deionized water, 3-aminopropyltriethoxysilane is with weight ratio (15-20):1:1 is uniformly mixed, and obtains mixed liquor;By mixeding liquid volume 0.01-0.02 times of dimethyl silicone polymer is added in mixed liquor, under conditions of 45-50 DEG C, ultrasonic power 300-400W Processing 30-50 minutes, obtains sonification fluid;0.5-0.7 times of dimethyl silicone polymer weight is added in into sonification fluid Montmorillonite, in the rotating speed of 45-50 DEG C, 210-300 revs/min be stirred to react 12-15 it is small when;After the completion of reaction, reaction solution is adopted With 80-100 mesh filter-cloth filterings, filter cake is collected;After filter cake is washed with the deionized water of 50-100 times of filter cake weight, in 50-60 DEG C, when dry 6-10 is small under conditions of vacuum degree 0.07-0.09MPa, obtain the montmorillonite-dimethyl silicone polymer function grain Son.
9. protective garment according to claim 7, which is characterized in that the functional particles are amine-modified for silica-DOPA Polyether sulfone functional particles, the preparation process of the amine-modified polyether sulfone functional particles of the silica-DOPA is:Using three hydroxyls The PH of deionized water is adjusted to 8.5 by aminomethane;By dopamine and the deionized water of pH is mixed up with solid-to-liquid ratio 1:(400- 500) (g/mL) is uniformly mixed, and adds in the polyether sulfone of 50-60 times of dopamine weight, anti-with 200-300 revs/min of rotating speed stirring When answering 20-24 small;By reaction solution using 80-100 mesh filter-cloth filterings, filter cake is collected;By filter cake in 70-80 DEG C, vacuum degree 0.06- When drying 8-10 is small under conditions of 0.08MPa, the amine-modified polyether sulfone of DOPA is obtained;By the amine-modified polyether sulfone of DOPA and anhydrous Ethyl alcohol is with solid-to-liquid ratio 1:(8-12) (g/mL) is uniformly mixed, and 20-30 points are ultrasonically treated under conditions of ultrasonic power 300-400W The ammonium hydroxide that 0.01-0.02 times of concentration of absolute ethyl alcohol volume is 25-28% is added in, is uniformly mixed and obtains mixed liquor A by clock;It will The tetraethyl orthosilicate of 0.9-1 times of ammonium hydroxide volume and the absolute ethyl alcohol of 20-30 times of ammonium hydroxide volume are uniformly mixed, and obtain mixed liquid B; Mixed liquid B is added in mixed liquor A, with 200-300 revs/min of rotating speed be stirred to react 20-25 it is small when;By reaction solution in 50-55 DEG C, when dry 10-16 is small under conditions of vacuum degree 0.06-0.08MPa, it is amine-modified to obtain the silica-DOPA Polyether sulfone functional particles.
CN201711325143.XA 2017-12-13 2017-12-13 Protective garment Pending CN108078035A (en)

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Application publication date: 20180529