CN101349010A - Silk broadcloth anti-water anti-oil dressing agent, preparation method and uses thereof - Google Patents
Silk broadcloth anti-water anti-oil dressing agent, preparation method and uses thereof Download PDFInfo
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Abstract
The invention relates to a technique for modifying silk broadcloth functionally and discloses a water repellent and oil repellent finishing agent of the silk broadcloth, a preparation method and an application thereof. The finishing agent consists of an ethylene fluorine monomer, an emulsifying agent and water. The preparation method comprises the following steps that: the emulsifying agent is dissolved into water, the ethylene fluorine monomer is added drop by drop at a rotating speed of 11,000 to 12,000r/min to realize the emulsifying process so that the water repellent and oil repellent finishing agent of the silk broadcloth is obtained. A finishing solution is prepared according to the ratio that the ethylene fluorine monomer is 20 to 120 percent of the textile by weight, the grafting reaction is performed by taking potassium peroxydisulfate as an evocating agent, the soaping, washing by water and drying processes are performed to extract and to remove the autopolymer so that the silk broadcloth with the water repellent and oil repellent functions is obtained. The technique adopts the monomer direct grafting method, ensures that the modified silk fabric not only has perdurable water repellent and oil repellent properties but also has good tactile and strong ventilating property, greatly improves the service performance of the true silk, and widens the application of the real silk fabric to the textile and clothing industry.
Description
Technical field
The present invention relates to a kind of function modified technology of silk broadcloth, particularly a kind of silk broadcloth surface water repellent finishing agent, preparation method and application thereof belong to chemical industry, light textile technical field.
Background technology
In recent years, the idea of silk broadcloth tradition einnehmen function is taking place to change, especially its Application Areas has obtained continuous expansion, real silk fabric is as coat articles for use boundary in off the beaten track season, no longer mainly as frivolous summer clothes lining, the silk fabric that many water and oil repellants are ventilative is used for suit autumn and winter, ski-wear, tippet, high-grade parka, upholstery etc.In addition, people require also more and more high to the real silk clothes, even wish that also not influencing it at misty rain weather wears effect.Therefore, the domestic and international market constantly increases the real silk fabric of water and oil repellant function and the demand of goods thereof, and China is silk big producing country, and real silk is carried out the water and oil repellant functional treatment, improve its added value, the competitiveness that strengthens in the international market is significant especially.
Water repellent finish is to be deposited on fiber surface with hydrophobic compound, does not block the hole that fiber interweaving forms, and air and steam can see through the fabric after the arrangement.In the prior art; paraffin aluminium soap method be the most original also be one of the processing technology of most convenient, its technology is: paraffin soap emulsion and aluminum acetate are mixed, and add protecting colloid in advance avoid breakdown of emulsion in emulsion; adopt single bath process, two soak two rolls fabric is put in order.This method is easy to process, and cost is low, but does not have oil repellent, and it is general to refuse the water effect, and not water-fast washing, and belongs to non-durability water repellent finish, and the real silk fabric feel after the arrangement is coarse, so be not suitable for the arrangement of silk broadcloth.The durable method for sorting of extensive use mainly contains: stearate chromium complex; Pyridine quaternary ammonium salt; The trimethylol melamine derivative; Organic siliconresin; Organofluorine compound etc. though said method can be obtained and necessarily refuse the water effect, has common shortcoming: ABRASION RESISTANCE, feel are not really desirable, and do not have grease proofing, anti-fouling functions (silk broadcloth low temperature is refused water conservancy project skill [J]. silk, 1995,5:15-17.).The fluorine resin finishing agent is most widely used at present, has the fluoropolymer emulsion of refusing water, oil repellent energy concurrently, and it is with the hydrogen atom on the fluorine atom organic hydrocarbon chains of replacement part or whole, generates fluorocarbon chain, the synthetic finishing agent of structure last and other molecule.Produce fluoropolymer emulsion fluorochemical monomer commonly used and mainly contain CTFE, tetrafluoroethylene, PVF, vinylidene, (methyl) acrylic acid fluoroalkyl ester class and fluoroalkyl vinyl ethers etc., utilize emulsifying agent (adopting fluorocarbon surfactant mostly) under the initator effect, make by emulsion copolymerization with acrylic ester monomer.In addition, also useful water-soluble fluoropolymer dispersion stabilizer replaces the report of emulsifying agent.The synthetic used initator great majority of fluoropolymer emulsion are water-soluble ammonium persulfate, sodium peroxydisulfate (potassium), but also useful redox system or oil-soluble initiator come the report of synthesized high-performance fluoropolymer emulsion.It has excellent water and oil repellant, particularly durability and feel be all than the finishing agent excellence of front, and be easy to use, be very suitable for the high grade true silk silk fabric water and oil repellent finish (the water and oil repellant fluorine compounds arrangements [J] of silk broadcloth. Zhejiang Silk Engineering College's journal, 1992,9 (4): 33-38.).At present, fluorochemical mainly is the water and oil repellent finish of fluoropolymer emulsion to the arrangement of fabric.This type of emulsion to the arrangement of fabric many under the effect of cross linking agent by roll-dry by the fire-bake or coating process is put in order on the fabric.
It is a kind of efficient ways of giving the new functional characteristic of silk broadcloth that silk broadcloth is carried out graft modification, the main finishing agent that uses is vinyl monomer, wherein Methacrylamide (MAA) and hydroxyethyl methylacrylate (HEMA) are the vinyl monomers of using always, successfully be used for silk broadcloth crease-resistant [Tsukada, Masuhiro; Freddi, Giuliano; Massafra, Maria Rosaria; Beretta, Silvia.Structure and properties of tussah silk fibers graft-copolymerized withmethacrylamide and 2-hydroxyethyl methacrylate.Journal of AppliedPolymer Science, 1998,67 (8): 1393-1403.], antibiotic [Aoki, Yasukazu.Finishingsilk for lasting antibacterial odor-absorbing properties by grafting silk withmethacrylamide or styrene and treating silk with bactericides.Jpn.KokaiTokkyo Koho, 2002,3.] arrangement.Yet, adopt fluorochemical monomer that silk fabrics is carried out the grafting treatment technology, thereby reach the purpose of silk broadcloth anti-water anti-oil modification, do not see relevant report so far yet.
Summary of the invention
In order to overcome the deficiency that prior art exists, the purpose of this invention is to provide a kind of silk broadcloth that not only makes and have durable water and oil repellant, and good hand touch, gas permeability are strong, finishing agent, preparation method and the application thereof that can effectively improve the wearability of real silk.
For achieving the above object, the technical solution adopted in the present invention is:
A kind of silk broadcloth anti-water anti-oil dressing agent, it is made up of vinyl fluorochemical monomer, emulsifying agent and water, and described vinyl fluorochemical monomer is a kind of in methacrylic acid hexafluoro butyl ester or the methacrylic acid ten difluoro heptyl esters; Described emulsifying agent comprises ethyoxyl non-ion fluorin carbon surface active agent, N-alkyl, N-hydroxyalkyl perfluorinated octyl sulfuryl amine and non-ionic surface active agent, and by weight, they are equivalent to 5～15%, 5～10% and 15～25% of vinyl fluorochemical monomer respectively.
Prepare the method for above-mentioned silk broadcloth anti-water anti-oil dressing agent, step is as follows:
1. with ethyoxyl non-ion fluorin carbon surface active agent, N-alkyl, N-hydroxyalkyl perfluorinated octyl sulfuryl amine and non-ionic surface active agent are dissolved in the water, and by weight, they are equivalent to 5～15%, 5～10% and 15～25% of vinyl fluorochemical monomer respectively;
2. the compound that above-mentioned steps is obtained is handled 1～3min under 8000～9000r/min speed conditions, raise speed again to 11000～12000r/min, under this emulsification treatment condition, dropwise add the vinyl fluorochemical monomer, the dropping time is controlled in 3～5min, the emulsification treatment time is 20～30min, obtains silk broadcloth anti-water anti-oil dressing agent after leaving standstill.
The applying step of above-mentioned silk broadcloth anti-water anti-oil dressing agent is as follows:
1. the pH value with finishing agent is adjusted to 3～4, by the vinyl fluorochemical monomer be fabric heavy 20～120%, bath raio be 1: 40～80 the preparation dressing liquids;
2. silk broadcloth is put in the above-mentioned dressing liquid, being warming up to 70～80 ℃, is initator with the potassium peroxydisulfate of vinyl fluorochemical monomer weight 0.8～4%, and the initator that adds half consumption earlier carries out graft reaction, the initator that adds surplus after 20～40 minutes again continues reaction 60～90 minutes;
3. the silk broadcloth after graft reaction being finished is soaped and is washed, and adopts the soxhlet extraction method to remove autopolymer after the oven dry again, obtains having the silk broadcloth of water and oil repellant function.
Principle of the present invention is: the vinyl fluorochemical monomer that water-refusing oil-refusing finishing agent adopts is methacrylic acid hexafluoro butyl ester or methacrylic acid ten difluoro heptyl esters, and the molecular structural formula of methacrylic acid hexafluoro butyl ester is as follows:
Methacrylic acid ten difluoro heptyl esters are the mixture of following two kinds of molecular structural formulas:
Because it is to carry out at aqueous phase that grafting is handled, and these two kinds of monomers are water insoluble,, make it be dispersed in aqueous phase so need it is utilized suitable emulsifying agent before using.Adopt fluorine-containing series monomers to real silk graft modification be the fluorochemical monomer the mode by phase transfer under the emulsifying agent effect directly and the active group on the silk fiber (as-OH ,-COOH ,-NH
2Deng) in conjunction with or the method for sorting that in dressing liquid, combines with fiber again after the polymerization of part.Many performances such as its durability of silk fabrics after the direct graft modification of monomer, feel, gas permeability are better than with the fabric of fluoropolymer emulsion by the cross linking agent arrangement, can improve the wearability of real silk greatly, not only improved the scope that real silk fabric is used at textile clothing industry, but also widened the application of silk fiber in other field, as medically making the real silk artificial blood vessel.Because fibroin albumen is safe and reliable to human body nonhazardous effect, and good Bc is arranged, the silk artificial blood vessel can not cause irritated or carcinogenic in human body, also can be related by flesh and blood with live body, grow up to the interior adventitia the same with true blood vessel.But if the fiber hole is too little, the cell of human body can't bore the fabric growth and come into, and inwall can't form complete inner membrance; Otherwise if the fiber mesh is too big, blood can infiltrate again.Silk fiber can reduce through fluoride modification rear surface, the water and oil repellant raising, and the mesh scope of the artificial blood vessel of manufacturing can be big slightly, and manufacture difficulty coefficient and cost just can reduce, and the security of the artificial blood vessel of manufacturing and durability can be improved.
Compared with prior art, the present invention has following advantage:
1. the used fluorine-contained finishing agent of the present invention is a vinylic chemical compound, can under initiation conditions, produce monomer free radical and fiber macromolecular radical, Raolical polymerizable takes place in the two, produce chemical bonding between the big molecule of finishing agent and fiber, form stable interaction, so make finishing effect have durability preferably.
2. many performances such as its feel of silk fabrics after the direct graft modification of monomer, gas permeability are better than with the fabric of fluoropolymer emulsion by the cross linking agent arrangement, can improve the wearability of real silk greatly, have widened the application of real silk fabric at textile clothing industry.
The specific embodiment
Below in conjunction with embodiment the present invention is further described:
Embodiment 1:
The preparation of finishing agent:
The vinyl fluorochemical monomer that present embodiment adopts is a methacrylic acid hexafluoro butyl ester, and consumption is respectively 50%, 100%, 200% of Real Silk Habotai weight.
Emulsifying agent is the compound of following three kinds of surfactants:
Ethyoxyl non-ion fluorin carbon surface active agent, addition are to 10% of methacrylic acid hexafluoro butyl ester monomer weight;
N-alkyl perfluorinated octyl sulfuryl amine or N-hydroxyalkyl perfluorinated octyl sulfuryl amine surfactant, addition are to 6% of methacrylic acid hexafluoro butyl ester monomer weight;
Non-ionic surface active agent Tween 80, addition are to 20% of methacrylic acid hexafluoro butyl ester monomer weight.
The preparation of finishing agent:
With emulsifiers dissolve in water, on the high-speed emulsifying machine with rotating speed 9000r/min high-speed stirred 1min after, raise speed to 12000r/min, dropwise splash into by the amount of being prepared at following methacrylic acid hexafluoro butyl ester of emulsify at a high speed condition monomer, the dropping time is controlled in 3～5min, the emulsification treatment time is 20min, leaves standstill stable back stand-by.
Method for sorting:
With silk broadcloth put into that the pH value is 3, bath raio is in 1: 50 the dressing liquid, be warming up to 75 ℃, potassium peroxydisulfate with methacrylic acid hexafluoro butyl ester monomer weight 1% is an initator, the initator that adds half consumption carries out graft reaction earlier, the initator that adds surplus after 30 minutes again continues reaction 90 minutes;
Reaction finishes the back silk fabrics earlier with 5 ‰ the paregal O 30min that soaps under 90 ℃ temperature conditions, be that solvent adopts the method for soxhlet extraction fully to extract to sample with acetone again after washing, the oven dry, remove autopolymer, obtain percent grafting after the oven dry and be respectively 9.36%, 38.78%, 52.45% silk broadcloth with water and oil repellant function.Different percent graftings is determined by methacrylic acid hexafluoro butyl ester monomer weights different in the finishing agent.
Three samples that present embodiment is obtained carry out water repellency test respectively by the difference of percent grafting, method of testing is: the sample to be tested of getting 20cm * 20cm, upward press the test of AATCC-22 (1977) method at YB813 type degree of getting wet analyzer (Wenzhou Daiei textile standard instrument plant), the water spray flux is 250mL.
Three samples that present embodiment obtains are refused the oil test respectively by the difference of percent grafting, method of testing is: sample is fixed, mark by the finish that drips different proportionings, so that the impervious lowest fractional of oil droplet indiffusion is for refusing oil standard behind the 30s, finish proportioning and standards of grading see Table 1.
Three samples that present embodiment provides, its water repellency test result is referring to table 2; Refuse oily test result referring to table 3.
Embodiment 2
The preparation of finishing agent:
The vinyl fluorochemical monomer that present embodiment adopts is methacrylic acid ten difluoro heptyl esters, and consumption is respectively 20%, 40%, 60% of Real Silk Habotai weight.
Emulsifying agent is the compound of following three kinds of surfactants:
Ethyoxyl non-ion fluorin carbon surface active agent uses the FSO of product as du pont company, and addition is to 12% of methacrylic acid ten difluoro heptyl ester monomer weights;
The N-alkyl, N-hydroxyalkyl perfluorinated octyl sulfuryl amine uses the DF-10 of product as Changjiang Chemical Plant, Wuhan City, and addition is to 8% of methacrylic acid ten difluoro heptyl ester monomer weights;
Non-ionic surface active agent Tween 80, addition are to 20% of methacrylic acid ten difluoro heptyl ester monomer weights.
The preparation of finishing agent:
With emulsifiers dissolve in water, on the high-speed emulsifying machine with rotating speed 8000r/min high-speed stirred 2min after, raise speed to 11000r/min, dropwise splash into by the amount of being prepared at a following methacrylic acid ten difluoro heptyl ester monomers of emulsify at a high speed treatment conditions, the dropping time is controlled in 3～5min, the emulsification treatment time is 20min, leaves standstill that to obtain silk broadcloth anti-water anti-oil dressing agent after stable stand-by.
Method for sorting:
With silk broadcloth put into that the pH value is 3, bath raio is in 1: 50 the dressing liquid, be warming up to 80 ℃, potassium peroxydisulfate with methacrylic acid ten difluoro heptyl ester monomer weights 3.5% is an initator, the initator that adds half consumption carries out graft reaction earlier, the initator that adds surplus after 30 minutes again continues reaction 90 minutes;
Reaction finishes the back silk fabrics earlier with 5 ‰ the paregal O 30min that soaps under 90 ℃ temperature conditions, be that solvent adopts the method for soxhlet extraction fully to extract to sample with butanone again after washing, the oven dry, remove autopolymer, obtain percent grafting after the oven dry and be respectively 3.2%, 8.67%, 17.7% silk broadcloth with water and oil repellant function.
Three samples that present embodiment is provided carry out water repellency test respectively, refuse the oil test, and method of testing is with embodiment 1.Its water repellency test result is referring to table 4; Refuse oily test result referring to table 5.
The sample that the foregoing description 1,2 is provided carries out the gas permeability test of grafting front and back silk fabrics, and the gas permeability test result is referring to table 6
Table 1: oil repellent evaluation criteria
Table 2: methacrylic acid hexafluoro butyl ester grafting (embodiment 1 sample) is to the influence of silk fabrics WATER REPELLENCY
Table 3: methacrylic acid hexafluoro butyl ester grafting (embodiment 1 sample) is to the influence of silk fabrics oil repellent
Table 4: methacrylic acid ten difluoro heptyl ester grafting (embodiment 2 samples) are to the influence of silk fabrics WATER REPELLENCY
Table 5: methacrylic acid ten difluoro heptyl ester grafting (embodiment 2 samples) are to the influence of silk fabrics oil repellent
Table 6: grafting is to real silk gas permeability (unit: cc/cm
2/ sec) influence
From table 2, table 3 as can be seen, for the silk fabrics of methacrylic acid hexafluoro butyl ester grafting, percent grafting reaches at 38.78% o'clock to be refused the water effect and can reach 80～90 fens, and refusing oily effect only has 70 fens; Percent grafting reaches at 52.45% o'clock, refuse the water effect and reach 100 fens, refusing the water effect also increases, reach 80 fens, but know from table 6, percent grafting is high more, the gas permeability of fabric is poor more, so when using, can and select the consumption of finishing agent to the influence of fabric breathability in conjunction with the requirement of actual water and oil repellant, but its consumption at least will be at more than 100% of silk fabrics weight.
From table 4, table 5 as can be seen, the silk fabrics of methacrylic acid ten difluoro heptyl ester grafting, just can reach 100 minutes refusing water and refusing oily effect at low percent grafting 3.20%, and gas permeability also is better than the silk fabrics of not grafting as known from Table 6, this method for sorting uses the finishing agent of minute quantity just can reach excellent water and oil repellant effect and does not influence the gas permeability of silk fabrics, is a kind of comparatively economical and practical effective method for sorting.Recommending methacrylic acid ten difluoro heptyl ester consumptions in the practical application is 20～30%.
Claims (3)
1. silk broadcloth anti-water anti-oil dressing agent, it is characterized in that: it is made up of vinyl fluorochemical monomer, emulsifying agent and water, and described vinyl fluorochemical monomer is a kind of in methacrylic acid hexafluoro butyl ester or the methacrylic acid ten difluoro heptyl esters; Described emulsifying agent comprises ethyoxyl non-ion fluorin carbon surface active agent, N-alkyl, N-hydroxyalkyl perfluorinated octyl sulfuryl amine and non-ionic surface active agent, and by weight, they are equivalent to 5～15%, 5～10% and 15～25% of vinyl fluorochemical monomer respectively.
2. method for preparing above-mentioned silk broadcloth anti-water anti-oil dressing agent is characterized in that step is as follows:
1. with ethyoxyl non-ion fluorin carbon surface active agent, N-alkyl, N-hydroxyalkyl perfluorinated octyl sulfuryl amine and non-ionic surface active agent are dissolved in the water, and by weight, they are equivalent to 5～15%, 5～10% and 15～25% of vinyl fluorochemical monomer respectively;
2. the compound that above-mentioned steps is obtained is handled 1～3min under 8000～9000r/min speed conditions, raise speed again to 11000～12000r/min, under this emulsification treatment condition, dropwise add the vinyl fluorochemical monomer, the dropping time is controlled in 3～5min, the emulsification treatment time is 20～30min, obtains silk broadcloth surface water repellent finishing agent emulsifying agent after leaving standstill.
3. the application of an above-mentioned silk broadcloth anti-water anti-oil dressing agent is characterized in that step is as follows:
1. the pH value with finishing agent is adjusted to 3～4, by the vinyl fluorochemical monomer be fabric heavy 20～120%, bath raio be 1: 40～50 the preparation dressing liquids;
2. silk broadcloth is put in the above-mentioned dressing liquid, being warming up to 70～80 ℃, is initator with the potassium peroxydisulfate of vinyl fluorochemical monomer weight 0.8～4%, and the initator that adds half consumption earlier carries out graft reaction, the initator that adds surplus after 20～40 minutes again continues reaction 60～90 minutes;
3. the silk broadcloth after graft reaction being finished is soaped and is washed, and adopts the soxhlet extraction method to remove autopolymer after the oven dry again, obtains having the silk broadcloth of water and oil repellant function.
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| CN102493189A (en) * | 2011-11-15 | 2012-06-13 | 王国栋 | Anti-bloodiness clothing finishing agent and emergency clothes |
| CN103194904A (en) * | 2013-04-27 | 2013-07-10 | 苏州大学 | Water-repellent and oil-repellent fabric finishing agent, as well as preparation method and applications thereof |
| CN103726308A (en) * | 2013-12-17 | 2014-04-16 | 江苏金太阳纺织科技有限公司 | Oil-repellent finishing liquid for woolen sweater and preparation method for oil-repellent finishing liquid |
| CN104153186A (en) * | 2014-07-14 | 2014-11-19 | 桐乡大和纺织服饰有限公司 | High-efficiency, antibacterial and self-cleaning finishing agent, and preparation method and use method thereof |
| CN104844729A (en) * | 2015-05-12 | 2015-08-19 | 苏州棠华纳米科技有限公司 | Composite high molecular surfactant, preparation method thereof and application of composite high molecular surfactant in foam coating process |
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| CN103194904A (en) * | 2013-04-27 | 2013-07-10 | 苏州大学 | Water-repellent and oil-repellent fabric finishing agent, as well as preparation method and applications thereof |
| CN103194904B (en) * | 2013-04-27 | 2015-05-27 | 苏州大学 | Water-repellent and oil-repellent fabric finishing agent, as well as preparation method and applications thereof |
| CN103726308A (en) * | 2013-12-17 | 2014-04-16 | 江苏金太阳纺织科技有限公司 | Oil-repellent finishing liquid for woolen sweater and preparation method for oil-repellent finishing liquid |
| CN104153186A (en) * | 2014-07-14 | 2014-11-19 | 桐乡大和纺织服饰有限公司 | High-efficiency, antibacterial and self-cleaning finishing agent, and preparation method and use method thereof |
| CN104844729A (en) * | 2015-05-12 | 2015-08-19 | 苏州棠华纳米科技有限公司 | Composite high molecular surfactant, preparation method thereof and application of composite high molecular surfactant in foam coating process |
| CN107034671A (en) * | 2017-04-07 | 2017-08-11 | 上海琴馨实业有限公司 | A kind of oil-stain-preventing silk embroidered fabric and preparation method thereof |
| CN107904925A (en) * | 2017-11-27 | 2018-04-13 | 无锡昊瑜节能环保设备有限公司 | A kind of wool fabric oil-repellent finiss technique |
| CN108486884A (en) * | 2018-02-28 | 2018-09-04 | 浙江理工大学 | A kind of preparation method of the soil resistant silk fabrics of water and oil repellant |
| CN109183412A (en) * | 2018-09-13 | 2019-01-11 | 江苏大同宝富纺织科技有限公司 | A kind of dacron water-repellent finishing method based on graft copolymerization |
| CN109183412B (en) * | 2018-09-13 | 2021-04-20 | 江苏大同宝富纺织科技有限公司 | Polyester fabric water repellent finishing method based on graft copolymerization |
| CN111501341A (en) * | 2020-04-10 | 2020-08-07 | 蚌埠学院 | Preparation method of hydrophobic modified silk fiber material |
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