CN100588768C - A kind of sterilizing shape-memory-fabric finishing agent and method for sorting thereof - Google Patents
A kind of sterilizing shape-memory-fabric finishing agent and method for sorting thereof Download PDFInfo
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- CN100588768C CN100588768C CN200710028473A CN200710028473A CN100588768C CN 100588768 C CN100588768 C CN 100588768C CN 200710028473 A CN200710028473 A CN 200710028473A CN 200710028473 A CN200710028473 A CN 200710028473A CN 100588768 C CN100588768 C CN 100588768C
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Abstract
The invention discloses a kind of sterilizing shape-memory-fabric finishing agent and method for sorting thereof, it is made up of following component and percetage by weight: water-based shape memory polyurethane 2～20%, low formaldehyde DP finish resin 3～30%, the Chinese medicine extract 1～10% of energy sterilization, catalyst 1～5%, surplus are water.Each component is composite in proportion to get final product.Sterilization water-based shape-memory-fabric finishing agent content of formaldehyde of the present invention is low, strength loss is little, tool shape-memory properties, high crease resistance, antimicrobial health care function, can replace traditional easy-care finish resin finish fabric, has a extensive future.
Description
Technical field
The present invention relates to the crease-proofing textiles containing technical field, specifically, relate to a kind of sterilizing shape-memory-fabric finishing agent and method for sorting thereof.
Background technology
The crease-proofing textiles containing arrangement is requisite program in the fabric post-treatment, occupies important status in fabric post-treatment processing.The key of crease-proofing textiles containing arrangement is the crease-proofing textiles containing finishing agent, and traditional crease proofing agent mainly comprises and contains formaldehyde and formaldehydeless two big class finishing agents:
1. contain the crease-proofing textiles containing arrangement of formaldehydes finishing agent
Contain the formaldehyde finishing agent wrinkle proofing of fabric is studied early, wherein the most important thing is hydroxymethyl-2 dihydroxy-ethylene urea, be commonly called as the 2D resin.This resin has well durable wrinkle resistant effect to fabric.But it makes the fabric intensity loss serious, the burst size of formaldehyde is also than higher, it uses the restriction that has been subjected to domestic and international environmental protection standard at present, therefore also has some researchers that it has been carried out the etherificate improvement or has added other textile auxiliary (as Chinese invention patent 200610116249.4).
2. the crease-proofing textiles containing arrangement of formaldehydeless class finishing agent
The natural high polymer shitosan: shitosan is the natural high polymer that extracts from chitin, is a kind of and the straight-chain polysaccharide cellulose analog structure, dissolves in the diluted acid.Some researcher thinks that its wrinkle resistance can match in excellence or beauty with the 2D resin, and washability and ABRASION RESISTANCE are better than 2D resin, and intensity reduces littler than 2D resin.But in fact, above-mentioned achievement only is a laboratory level, and its finishing effect is compared with the 2D resin and there is a big difference, does not far reach the requirement (Chinese invention patent 03134276.0) of durable press.
Multi-carboxylic acid's compound: multi-carboxylic acid's compound is the formaldehyde-free crease-proofing finishing agent that research at present has most application prospect, many textile chemistry workers both domestic and external are to BTCA (BTCA), citric acid (CA) and other polybasic carboxylic acid have carried out number of research projects, and have applied for some patents (United States Patent (USP) 4,975,209,4,820,307,5,221,285; China applies for a patent 200610119085.0,200510079829.6), the result shows: polybasic carboxylic acid is compared with traditional 2D resin as the finishing effect of the wrinkle proofing finishing agent of cellulose fibre, and both are in identical level basically.But up to the present, also have many problems to remain further to be solved on the suitability for industrialized production of polybasic carboxylic acid as the wrinkle proofing finishing agent of cellulose fibre.In fact, because the acidity of polybasic carboxylic acid is stronger, needed baking temperature is higher in the arrangement process, causes powerful obviously decline of arrangement back fabric; Simultaneously, for colored fabric, because acid and action of high temperature, many dyestuff generation looks become.More than the existence of two problems, had a strong impact on the industrial applications of this type of finishing agent.
In at present all crease-proofing textiles containing finishing agents, the wrinkle proofing effect is relatively good, domestic and international application is traditional contains formaldehydes fabric finishing agent 2D resin (hydroxymethyl-2 dihydroxy-ethylene urea) and through its modification etherificate 2D resin, but the strength loss of the fabric after the arrangement is big, particularly burst size of methanal is very high, and is very big to human body harm.And the shortcoming of the equal various degrees of other existing crease-proofing textiles containing finishing agent, as it is undesirable to put wrinkle resistant effect in order, and the fabric strength loss is big, and feel is bad, and environmental pollution is big, and performance is single, occurs problems such as yellowing phenomenon easily.
Shape memory polyurethane is as the existing relevant patent documentation report (Chinese invention patent 200410002552.2 of crease proofing agent, 200410047647.6), but the water-based shape memory polyurethane of being invented is an end-sealed type polyurethane, the generation of its shape memory effect must rely on the crosslinked generation of isocyano and cellulose hydroxyl, in actual applications because the end-blocking and the deblocking effect instability of polyurethane isocyano, cause its shape memory finishing effect not ideal, the big defective of it another is in process of production owing to increase technologies such as end-blocking and deblocking, performance is single, cause the shape memory polyurethane cost produced too high, and bring new environmental pollution, be difficult to be accepted by market.
Because the raising of people's living standard, dress has been not only a clothing function for fabric, also require to have fashion, health care, medical treatment, function such as fungi-proofing, also corresponding appearance the on the market such as products such as far infrared underwear, nanometer titanium dioxide fiber derived products, but these products all also exist such as performance can not be lastingly, unsatisfactory curative effect, technology is loaded down with trivial details, nanometer is reunited, itself contain defectives such as chemical attack (Chinese invention patent 95191064.7,03139798.0,03109764.2,200510038593.1).
Summary of the invention
The objective of the invention is to overcome the deficiency that existing crease-proofing textiles containing finishing agent exists, provide that a kind of crease resistance is good, strength loss is little, content of formaldehyde is low, can give the sterilizing shape-memory-fabric finishing agent of fabric form memory function and durable antibiotic health function.
Another object of the present invention provides the method that above-mentioned sterilizing shape-memory-fabric finishing agent carries out textile finishing.
For achieving the above object, the present invention adopts following technical scheme:
A kind of sterilizing shape-memory-fabric finishing agent, form by following component and percetage by weight: water-based shape memory polyurethane 2～20%, low formaldehyde DP finish resin 3～30%, the Chinese medicine extract 1～10% of energy sterilization, catalyst 1～5%, surplus is a water.Each component is composite in proportion to get final product.
Above-mentioned water-based shape memory polyurethane is to be formed by following component and molar ratio prepared in reaction: aliphatic diisocyanate 0.7～1.2, polyether polyol 0.2～0.6, chain extender 0.1～0.5, the end hydroxyl silicone oil 0.2～0.5 of molecular weight 400～10000, catalyst 0～0.05.The water-based shape memory polyurethane in the preparation; usually make emulsion; its method is: add vacuum drying polyether polyol in a four-hole boiling flask of being furnished with the protection of mechanical agitator, drying nitrogen, condenser pipe; end hydroxyl silicone oil; aliphatic diisocyanate; catalyst, a spot of solvent or do not need solubilizer.Under nitrogen protection, be heated to 80 ℃～100 ℃ and reacted with this understanding 1～5 hour, add chain extender then and continue reaction 3～5 hours, being cooled to 30 ℃, to be emulsified into solid content be 20～50% emulsion.
The preferred 2D resin of above-mentioned low formaldehyde modified resin, 2D etherificate resin, BTCA or its mixture.
Above-mentioned Chinese medicine extract is one or more the aqueous extract or the ethanol extract of mixture in folium eucalypti, the tuber of stemona, folium isatidis, honeysuckle, chrysanthemum, Radix Isatidis, tarragon, sweet wormwood, the peppermint.Extracting method is: take by weighing Chinese medicine, added 1～20 times of ethanol or water logging bubble 1 hour～3 days, filter to get filtrate, then ethanol or water are spin-dried for solid extract.
The method of utilizing above-mentioned sterilizing shape-memory-fabric finishing agent to carry out crease-proofing textiles containing arrangement comprises the steps: fabric two is soaked two and rolls liquid carrying rate 70～100% in wrinkle proofing liquid, 85 ℃ of preliminary dryings 3～5 minutes, 150～190 ℃ baked 2 minutes then, washing, oven dry.Utilize sterilizing shape-memory-fabric finishing agent finish fabric provided by the present invention to have transfer of shapes temperature in-30～100 ℃ of scopes, the crimp shape that can recover to cause in the wearing process when this fabric is higher than described shape memory transition temperature, the fabric flatness reaches more than 3.5.
Sterilizing shape-memory-fabric finishing agent provided by the present invention reaches 80～100% to the sterilizing rate of gold-coloured staphylococci, Candida albicans, and formaldehyde discharges content and be lower than 30ppm, powerfully keeps filter more than 70%.
Compared with prior art, the present invention has following beneficial effect: shape-memory-fabric finishing agent of the present invention does not rely on isocyano to participate in reaction, does not therefore need polyurethane is carried out end-blocking and deblocking; And by aqueous polyurethane, contain between the wrinkle resistant auxiliary agent of reactive group, the cellulose fibre three being cross-linked with each other the reaction Chinese medicine active ingredient is coated in the fabric fibre, produce permanent bactericidal effect.Sterilization water-based shape-memory-fabric finishing agent content of formaldehyde of the present invention is low, strength loss is little, tool shape-memory properties, high crease resistance, antimicrobial health care function, can replace traditional easy-care finish resin finish fabric, has a extensive future.
The specific embodiment
Embodiment 1
1. the preparation of water-based shape memory polyurethane
Polypropylene glycol (the molecular weight 2000 that adds 40 grams, dry), 30 gram end hydroxyl silicone oils (molecular weight 1000, dry), stannous octoate (0.5 gram) and 20 gram isofoer diisocyanates in 1000 milliliters, be with mechanical agitation, be connected in the four-hole glass flask of nitrogen port.Feed drying nitrogen, mechanical agitation remains under 80 ℃ of temperature and reacted 4 hours.Add polyethylene glycol 40 grams (molecular weight 1000, dry) then, add 1 again, under the condition of 4-butanediol (0.9 gram) as 90 ℃ of chain extender maintenances, continue reaction 3 hours.Add the 20ml dimethyl formamide in the course of reaction.Then reduce the temperature to 30 ℃ of reactant.Add under the high-speed stirred (2000rp/m) of agitator and contain 500 milliliters of deionized waters, the acquisition solid content is 20% water white water-based shape memory polyurethane.
2. the preparation of the Chinese medicine extract of energy sterilization
Take by weighing 1 kilogram of Radix Isatidis, added 2 kilograms of alcohol immersion 1 day, filter to get filtrate, then ethanol is spin-dried for solid extract.
3. the preparation of sterilizing shape-memory-fabric finishing agent (following weight content is in active ingredient)
Water-based shape memory polyurethane 5%, 2D resin 3%, the Chinese medicine extract of magnesium chloride 1%, 1% energy sterilization, water 90%.Each component is mixed obtains sterilizing shape-memory-fabric finishing agent.
4. sterilizing shape-memory-fabric finishing agent is to the arrangement of fabric
To treat that finish fabric (100% cotton) is immersed in the sterilizing shape-memory polyurethane arrangement liquid of above-mentioned preparation, two soak two rolls, and the pick-up rate weight ratio is 100%, then preliminary drying 3 minutes in 85 ℃ of baking ovens, baked and banked up with earth 2 minutes at 160 ℃ again, be cooled to room temperature and promptly get the sterilizing shape-memory fabric.
5. fabric performance test after putting in order
The result is as follows for the sterilizing shape-memory fabric performance test: arrangement back COTTON FABRIC wrinkle grade is greater than 3.5, the folding line retention rate is greater than 3.5, dry creasing angle is greater than 310 °, ultimate strength retention rate 82%, formaldehyde is released to 18ppm, and the antibiotic rate of gold-coloured staphylococci, Candida albicans is reached 80%.Making fabric form memory transition temperature through present embodiment is 55 ℃.Shape-memory properties test: the wrinkle grade of handling through external force is 1.5 shape memory fabrics, and after 1 minute, wrinkle grade is 3.5 in 55 ℃ water-bath.Annotate: the dry creasing angle of untreated fabric is 170 degree, adopts AATCC 66-1996 canonical measure creasy recovery angle, adopts powerful tensilometer to measure strength retention, adopts the GB aqueous extraction method to measure content of formaldehyde.
Embodiment 2
1. the preparation of water-based shape memory polyurethane
Polyethylene glycol (the molecular weight 3000 that adds 60 grams, dry), 300 gram end hydroxyl silicone oil (molecular weight 6000, dry), dibutyltin dilaurate (2.5 gram) and 20 grams 1, the 6-hexamethylene diisocyanate is in 2000 milliliters, the four-hole glass flask of band mechanical agitation, connection nitrogen port.Feed drying nitrogen, mechanical agitation remains under 80 ℃ of temperature and reacted 3 hours.Add PTMG 40 gram (molecular weight 1000, dry) then, add again under the condition of dihydromethyl propionic acid 4 grams between keeping 90 ℃ as chain extender, continue reaction 4 hours.Then reduce the temperature to 50 ℃ of reactant.Add 570 milliliters of deionized waters that contain 3 gram triethylamines down in the high-speed stirred (2000rp/m) of agitator, obtain solid content and be 43% water white water-based shape memory polyurethane.
2. the preparation of the Chinese medicine extract of energy sterilization
Take by weighing 1 kilogram of folium isatidis, add 20 kilograms of entry, 1 hour heat time heating time of lixiviate, 100 ℃ of reflux temperatures filter to get filtrate, then water is spin-dried for solid extract.
3. the preparation of sterilizing shape-memory-fabric finishing agent (content is in active ingredient)
Water-based shape memory polyurethane 20%, 2D etherificate resin 30%, 5% magnesium sulfate, the Chinese medicine extract of 6% energy sterilization, water 39%.Each component is mixed obtains sterilizing shape-memory-fabric finishing agent.
4. sterilizing shape-memory-fabric finishing agent is to the arrangement of fabric
To treat that finish fabric (100% cotton) is immersed in the sterilizing shape-memory polyurethane arrangement liquid of above-mentioned preparation, two soak two rolls, and the pick-up rate weight ratio is 70%, then preliminary drying 4 minutes in 85 ℃ of baking ovens, baked and banked up with earth 2 minutes at 170 ℃ again, be cooled to room temperature and promptly get the sterilizing shape-memory fabric.
5. fabric performance test after putting in order
The result is as follows for the sterilizing shape-memory fabric performance test: arrangement back COTTON FABRIC wrinkle grade 3.9, folding line retention rate 3.8, dry creasing angle be greater than 325 °, ultimate strength retention rate 76%, formaldehyde is released to 28ppm, and the antibiotic rate of gold-coloured staphylococci, Candida albicans is reached 100%.Making fabric form memory transition temperature through present embodiment is 60 ℃.Shape-memory properties test: the wrinkle grade of handling through external force is 1.5 shape memory fabrics, and after 1 minute, wrinkle grade is 3.8 in 60 ℃ water-bath.
Embodiment 3
1. the preparation of water-based shape memory polyurethane
Polytetrahydrofuran diol (the molecular weight 3000 that adds 60 grams, dry), 300 gram end hydroxyl silicone oil (molecular weight 10000, dry), zinc sulfate (1.0 gram) and 26 grams 4,4 '-dicyclohexyl methyl hydride diisocyanate is in 2000 milliliters, the four-hole glass flask of band mechanical agitation, connection nitrogen port.Feed drying nitrogen, mechanical agitation remains under 80 ℃ of temperature and reacted 5 hours.Add polypropylene glycol 18 gram (molecular weight 600, dry) then, add again under the condition of dihydromethyl propionic acid 2.7 grams between keeping 100 ℃ as chain extender, continue reaction 3 hours.Add the 20ml butanone in the course of reaction.Then reduce the temperature to 50 ℃ of reactant.Add 570 milliliters of deionized waters that contain 0.8 gram NaOH down in the high-speed stirred (2500rp/m) of agitator, obtain solid content and be 41% water white water-based shape memory polyurethane.
2. the preparation of the Chinese medicine extract of energy sterilization
Take by weighing 1 kilogram of honeysuckle, 10 kilograms in water, 80 ℃ of reflux temperatures filter to get filtrate 2 hours heat time heating times of lixiviate, then water is spin-dried for solid extract.
3. the preparation of sterilizing shape-memory-fabric finishing agent
Water-based shape memory polyurethane 10%, BTCA 15%, 3% sodium dihydrogen phosphate, the Chinese medicine extract of 2% energy sterilization, water 70%.Each component is mixed obtains sterilizing shape-memory-fabric finishing agent.
4. sterilizing shape-memory-fabric finishing agent is to the arrangement of fabric
To treat that finish fabric (100% cotton) is immersed in the sterilizing shape-memory polyurethane arrangement liquid of above-mentioned preparation, two soak two rolls, and the pick-up rate weight ratio is 90%, then preliminary drying 5 minutes in 85 ℃ of baking ovens, baked and banked up with earth 2 minutes at 180 ℃ again, be cooled to room temperature and promptly get the sterilizing shape-memory fabric.
5. fabric performance test after putting in order
The result is as follows for the sterilizing shape-memory fabric performance test: arrangement back COTTON FABRIC wrinkle grade 3.7, folding line retention rate 3.5, dry creasing angle be greater than 315 °, ultimate strength retention rate 72%, formaldehyde is released to 0ppm, and the antibiotic rate of gold-coloured staphylococci, Candida albicans is reached 85%.Making fabric form memory transition temperature through present embodiment is 62 ℃.Shape-memory properties test: the wrinkle grade of handling through external force is 1.5 shape memory fabrics, and after 1 minute, wrinkle grade is 3.6 in 62 ℃ water-bath.
Claims (7)
1. sterilizing shape-memory-fabric finishing agent is characterized in that being made up of following component and percetage by weight:
Water-based shape memory polyurethane 2～20%, low formaldehyde DP finish resin 3～30%, the Chinese medicine extract 1～10% of energy sterilization, catalyst 1～5%, surplus is a water;
Described water-based shape memory polyurethane is to be formed by following component and molar ratio prepared in reaction: aliphatic diisocyanate 0.7～1.2, polyether polyol 0.2～0.6, chain extender 0.1～0.5, the neutralizer 0～0.3 that contains basic group, the end hydroxyl silicone oil 0.2～0.5 of molecular weight 400～10000, catalyst 0～0.05.
2. sterilizing shape-memory-fabric finishing agent as claimed in claim 1 is characterized in that:
Described aliphatic diisocyanate is isophorone diisocyanate, 4,4 ' dicyclohexyl methyl hydride diisocyanate or 1, the 6-hexamethylene diisocyanate;
Described polyether polyol is polyethylene glycol, polypropylene glycol, PTMG or its mixture;
Described chain extender is 1,4-butanediol, 1, ammediol, ethylene glycol or dihydromethyl propionic acid;
The described neutralizer that contains basic group is water miscible tertiary amine, alkali metal hydroxide or its mixture;
Described catalyst is pink salt, zinc salt or its mixture.
3. sterilizing shape-memory-fabric finishing agent as claimed in claim 1 is characterized in that described low formaldehyde modified resin is one or more the mixture in 2D resin, 2D etherificate resin, the BTCA.
4. sterilizing shape-memory-fabric finishing agent as claimed in claim 1 is characterized in that described Chinese medicine extract is one or more the aqueous extract or the ethanol extract of mixture in folium eucalypti, the tuber of stemona, folium isatidis, honeysuckle, chrysanthemum, Radix Isatidis, tarragon, sweet wormwood, the peppermint.
5. sterilizing shape-memory-fabric finishing agent as claimed in claim 1 is characterized in that described catalyst is slaine or inorganic acid or its mixture.
6. sterilizing shape-memory-fabric finishing agent as claimed in claim 5 is characterized in that described slaine is magnesium salts, sodium salt or sylvite; Described inorganic acid is hydrochloric acid or phosphoric acid.
7. utilize the described sterilizing shape-memory-fabric finishing agent of claim 1 to carry out the method for crease-proofing textiles containing arrangement, it is characterized in that comprising the steps: fabric two is soaked two and rolls in wrinkle proofing liquid, liquid carrying rate 70～100%, 85 ℃ of preliminary dryings 3～5 minutes, 150～190 ℃ baked 2 minutes then, washing, oven dry.
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| CN200710028473A CN100588768C (en) | 2007-06-07 | 2007-06-07 | A kind of sterilizing shape-memory-fabric finishing agent and method for sorting thereof |
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