CN102162194A - Textile finishing agent and preparation method thereof - Google Patents
Textile finishing agent and preparation method thereof Download PDFInfo
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- CN102162194A CN102162194A CN2010106199241A CN201010619924A CN102162194A CN 102162194 A CN102162194 A CN 102162194A CN 2010106199241 A CN2010106199241 A CN 2010106199241A CN 201010619924 A CN201010619924 A CN 201010619924A CN 102162194 A CN102162194 A CN 102162194A
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Abstract
The invention discloses an organic silicon modified fluorine-containing acrylate polymer silver-ion-complexed finishing agent for textiles and a preparation method thereof. The finishing agent is characterized by adopting organic silicon and fluorine-containing monomers for co-modification, so that the finishing agent has high self-cleaning and softening properties. Besides, the finishing agent has good anti-bacterial and anti-static functions.
Description
Technical field
The present invention relates to a kind of textile finish and preparation method thereof, be the textiles chemical field.
Background technology
The polyacrylate emulsion has the excellent transparency, film forming, oil resistivity, weatherability, mechanical stability and adhesiveness, and raw material sources are abundant, and cost is lower, is widely used in fields such as coating, weaving, leather, papermaking, adhesive.But its stain resistance, resistance to water are not ideal enough, and cold resistance, heat resistance are relatively poor, and " hot sticky cold crisp " phenomenon easily takes place, and it is further used be restricted.Fluorine is the element of electronegativity maximum; its atom covalence radius (0.064nm) is only big slightly than hydrogen atom; the C-F key is highly stable; and fluorine atom is very tight in the outer field arrangement of carbon skeleton; can form " shielding protection " to main chain and interior molecules; guaranteed the stability of carbon-carbon bond, so fluorocarbon shows remarkable performances such as chemical stability, corrosion resistance and non-oxidizability.Organic fluorine material makes its surface free energy very low owing to contain the stronger fluorine atom of sterically hindered less and close electric energy power on its molecule side group or the side chain, has good performances such as waterproof and oilproof.Argent has the excellent antistatic energy, existing textiles antistatic finishing agent then mainly adopts hydrophilic polymers to reach anlistatig purpose at the surface filming absorption moisture of textiles, the present invention introduces silver in the finishing agent, and be uniformly distributed in the surface of fabric, can derive static rapidly, effectively improve the conduction and the antistatic property of fabric.Therefore, the adding of fluorine and silver has greatly strengthened the automatically cleaning and the antistatic property of textile finish, make textiles be easier to arrange, comfortable.
Summary of the invention
The objective of the invention is to:
(1) provides a kind of textile finish;
(2) provide a kind of preparation method of textile finish.
The present invention is a polymerization single polymerization monomer with acrylate, styrene, acrylic acid, organosilicon cross-linking agent, thiazolinyl amine monomer and fluorochemical monomer, form emulsifying agent with non-ionic surface active agent, anion surfactant, adopt emulsion polymerisation process to prepare the organic-silicon-modified fluorinated acrylate polymer of self-cross linking type, in emulsion, add silver salt again and carry out complex reaction and be prepared into and have textile finish antibiotic, antistatic, self-cleaning function.Be positioned at the polymer micelle superficial layer and have abundant organosilicon and other crosslinking kinetic energy based groups, crosslinked film forming in solidification process, the fastness of increase polyacrylate polymers film; Introduce components such as fluorochemical monomer, improve the water-fast resistance to soiling of polymer.Thereby the finishing agent that makes has preferably resistance to water and characteristics such as low temperature resistant, has functions such as antibiotic, antistatic, automatically cleaning, applicable to the functional treatment of textile surface.
For achieving the above object, product of the present invention is finished by following two steps:
The first step: fluoropolymer emulsion synthetic
Described fluoropolymer emulsion is by comprising that at least acrylate, styrene, acrylic acid, thiazolinyl amine monomer, organosilicon cross-linking agent and fluorochemical monomer, emulsifying agent, initator, deionized water make through emulsion polymerisation process.
In the above-mentioned each component, the acrylic ester monomer consumption is 30～60 parts by umber, 12～19 parts of styrene, 6～14 parts in acrylic acid, the organosilicon cross-linking agent consumption is 3～8 parts by umber, 4～8 parts of thiazolinyl amine monomers, the consumption of emulsifying agent is 5～20 parts by umber, initiator amount is 0.3～0.7 part by umber, and the deionized water consumption is 300～800 parts by umber, and described consumption is weight.
Described acrylic ester monomer comprises one or more the combination in acrylic acid, methacrylic acid, methyl methacrylate, hydroxy methyl methacrylate, hydroxyethyl methylacrylate, hydroxy propyl methacrylate, methyl acrylate, ethyl acrylate, propyl acrylate, butyl acrylate, hydroxy-ethyl acrylate, hydroxypropyl acrylate, acrylic acid hydroxy butyl ester, the own ester of acrylic acid hydroxyl, the 2-EHA.
Described organosilicon cross-linking agent is vinyltriethoxysilane [CH
2=CHSi (OC
2H
5)
3], vinyl three (2-methoxy ethoxy) silane [CH
2=CHSi (OC
2H
4OCH
3)
3], methyl allyl acyloxypropyl trimethoxysilane [CH
2=C (CH
3) COOC
3H
6Si (OCH
3)
3] in one or more.
Described thiazolinyl amine monomer comprises one or more the combination in alkenyl amine, diallylamine, the triallylamine.
Described initator comprises one or more combinations in sodium peroxydisulfate, potassium peroxydisulfate, ammonium persulfate, azodiisobutyronitrile, the benzoyl peroxide.
Described emulsifying agent is made up of non-ionic surface active agent, anion surfactant and low mass molecule alcohol compounds, and wherein anion surfactant is a neopelex; Non-ionic surface active agent is that fatty alcohol-polyoxyethylene ether, the alkyl number of molecular weight 400～1200 is 8～9 AES and in the polyethylene glycol one or more.
In emulsifying agent, the weight of anion surfactant is 3～10 parts by umber, and the weight of non-ionic surface active agent is 3～15 parts by umber.
The concrete steps of preparation fluoropolymer emulsion are as follows:
A, in reactor, add 3～18 parts of emulsifying agents and 300～400 parts of water, heat up, stir, treat emulsifiers dissolve, be cooled to below 50 ℃;
B, 10～20 parts of acrylic ester monomers of adding, 6～8 parts of styrene, 6～14 parts in acrylic acid, emulsification 30min adds 0.15～0.3 part of initator, initator is with 10～30 parts of water-soluble, be warming up to 60～68 ℃ of initiation reactions, along with the carrying out of polymerisation, reaction temperature rises to 70～85 ℃ gradually, reaction time is 1～3h, and emulsion presents light blue;
After c, question response temperature in the kettle fall after rise, emulsion temperature is adjusted into 70 ℃, and insulation 0.5h;
D, under 70～75 ℃ of temperature, drip 20～40 parts of acrylic ester monomers then, 4～13 parts of styrene, 3～8 parts of organosilicon cross-linking agents, 4～8 parts of thiazolinyl amine monomers, and 0.15～0.65 part of initator, initator is with 20～60 parts of water-soluble, the dropping time is 1～1.5h, drips follow-up continuation of insurance temperature 1h, is cooled to below 50 ℃, regulate pH value to 7 with ammoniacal liquor, promptly obtain fluoropolymer emulsion.
Second step: the preparation of textile finish
Under pH neutral, on the nitrogen-atoms in the amido contained lone pair electrons can with Ag
+Ion forms stable complex compound, makes Ag
+Be fixed on the copolymer molecule chain.
In synthetic the containing in the amine copolymer thing emulsion of the first step, add 8～14 parts of silver nitrates, stirred 1～3 hour down at 16～25 ℃, make amido and Ag
+Fully complexing makes and has textile finish antibiotic, antistatic, self-cleaning performance.
This finishing agent has good filming performance, does not need to add adhesive in use again, and silver ion is anchored on the polymer by coordinate bond, has avoided moving during use and weakens its antibiotic, antistatic property, thereby strengthened its endurance quality; In addition, the introducing of fluorochemical monomer has given finishing agent good self-cleaning function, can make finishing agent be widely used in the functional treatment of textiles.
Specific implementation method:
Following embodiment only illustrates, and is not only, so all within the scope of the present invention or making the change similar to the present invention all is contained within the present invention.
Unless stated otherwise, following unit is parts by mass.
The concrete steps of textile finish of the present invention are:
Embodiment 1
(a) with following monomer
Butyl acrylate 6g
Methyl methacrylate 8g
Ethyl acrylate 4g
Acrylic acid 6g
Place in the 500ml reactor, stir, form the polymer monomer mixed liquor A.
(b) with following component
Fatty alcohol-polyoxyethylene ether (10) 2.2g
Emulsifier os 3.4g
Alkylphenol polyoxyethylene (30) 3.2g
Polyethylene glycol (molecular weight 400) 2.2g
Neopelex 2.8g
Glycerine 1.4g
Deionized water 360g
Place the 250ml glass,, form stable emulsifier aqueous solution B in 50 ℃ of stirring and dissolving 40min.Form solution for standby with 55g deionized water dissolving 0.35g ammonium persulfate.
(c) under agitation, the polymer monomer mixed liquor A is joined among the emulsifier aqueous solution B, form the emulsion C of polymer monomer.
(d) in the 1000ml four-hole boiling flask that thermometer, agitator are housed, add above-mentioned emulsion C.Under agitation, temperature in the bottle is risen to 60 ℃, add the ammonium persulfate solution of 1/3 weight with dropping funel, along with the carrying out of polymerisation, reaction temperature rises to 80 ℃ gradually, and emulsion presents light blue, after treating that a bottle interior temperature falls after rise, emulsion temperature is adjusted into 70 ℃, and insulation 0.5h.Then under uniform temp, with the ammonium persulfate solution of 12 parts of 1h dropwise addition of acrylic acid butyl esters, 6 parts, 4 parts vinyltriethoxysilane of styrene, 3 parts of alkenyl amines, 4 parts of diallylamines and 2/3 weight.After dripping, continue insulation 1h.Polymerized emulsion is cooled to below 50 ℃, with ammoniacal liquor adjustment pH value to 7, promptly obtains containing amine copolymer thing emulsion.
(e) in (d) solution for preparing, add 8 parts of silver nitrates, stirred 4 hours down, make amido and Ag at 18 ℃
+Fully complexing makes silver-carrying antibiotic finishing agent.
Embodiment 2
(a) with following monomer
Butyl acrylate 8g
Methyl methacrylate 6g
Isooctyl acrylate monomer 4g
Methacrylic acid 8g
Place in the 250ml reactor, stir, form the polymer monomer mixed liquor A.
(b) with following component
Fatty alcohol-polyoxyethylene ether (10) 2.4g
Emulsifier os 2.5g
Alkylphenol polyoxyethylene (30) 3.4g
Polyethylene glycol (molecular weight 400) 2.6g
Neopelex 2.4g
Glycerine 1.5g
Deionized water 350g
Place the 500ml glass,, form stable emulsifier aqueous solution B in 50 ℃ of stirring and dissolving 40min.Form solution for standby with 85g deionized water dissolving 0.358g sodium peroxydisulfate.
(c) under agitation, the polymer monomer mixed liquor A is joined among the emulsifier aqueous solution B, form the emulsion C of polymer monomer.
(d) in the 1000ml four-hole boiling flask that thermometer, agitator are housed, add above-mentioned emulsion C.Under agitation, temperature in the bottle is risen to 62 ℃, add the sodium peroxydisulfate solution of 1/3 weight with dropping funel, along with the carrying out of polymerisation, reaction temperature rises to 80 ℃ gradually, and emulsion presents light blue, after treating that a bottle interior temperature falls after rise, emulsion temperature is adjusted into 72 ℃, and insulation 0.5h.Then under uniform temp, with the sodium peroxydisulfate solution of 12 parts of 1h dropwise addition of acrylic acid butyl esters, styrene 6 parts, 6 parts gamma-methyl allyl acyloxypropyl three isopropoxy silane, 7 parts of diallylamines and 2/3 weight.After dripping, continue insulation 1h.Polymerized emulsion is cooled to below 50 ℃, with ammoniacal liquor adjustment pH value to 7, promptly obtains containing amine copolymer thing emulsion.
(e) in (d) solution for preparing, add 9 parts of silver nitrates, stirred 4 hours down, make amido and Ag at 20 ℃
+Fully complexing makes silver-carrying antibiotic finishing agent.
Embodiment 3
(a) with following monomer
Butyl acrylate 6g
Ethyl methacrylate 6g
Propyl acrylate 5g
Acrylic acid 5g
Place in the 250ml reactor, stir, form the polymer monomer mixed liquor A.
(b) with following component
Fatty alcohol-polyoxyethylene ether (10) 2.6g
Emulsifier os 4.0g
Alkylphenol polyoxyethylene (30) 3.6g
Polyethylene glycol (molecular weight 400) 1.4g
Neopelex 2.6g
Glycerine 1.6g
Deionized water 450g
Place the 1000ml glass,, form stable emulsifier aqueous solution B in 50 ℃ of stirring and dissolving 40min.Form solution for standby with 75g deionized water dissolving 0.425g potassium peroxydisulfate.
(c) under agitation, the polymer monomer mixed liquor A is joined among the emulsifier aqueous solution B, form the emulsion C of polymer monomer.
(d) in the 1000ml four-hole boiling flask that thermometer, agitator are housed, add above-mentioned emulsion C.Under agitation, temperature in the bottle is risen to 64 ℃, add the potassium persulfate solution of 1/3 weight with dropping funel, along with the carrying out of polymerisation, reaction temperature rises to 80 ℃ gradually, and emulsion presents light blue, after treating that a bottle interior temperature falls after rise, emulsion temperature is adjusted into 75 ℃, and insulation 1h.Then under uniform temp, with the potassium persulfate solution of 14 parts of 2h dropwise addition of acrylic acid butyl esters, styrene 8 parts, 8 parts acryloyl-oxy propyl group three isopropoxy silane, 5 parts of alkenyl amines and 2/3 weight.After dripping, continue insulation 1h.Polymerized emulsion is cooled to below 50 ℃, with ammoniacal liquor adjustment pH value to 7, promptly obtains containing amine copolymer thing emulsion.
(e) in (d) solution for preparing, add 12 parts of silver nitrates, stirred 4 hours down, make amido and Ag at 19 ℃
+Fully complexing makes silver-carrying antibiotic finishing agent.
Embodiment 4
(a) with following monomer
Butyl acrylate 7g
Methyl methacrylate 2g
Ethyl acrylate 4g
Isooctyl acrylate monomer 4g
Acrylic acid 5g
Place in the 250ml reactor, stir, form the polymer monomer mixed liquor A.
(b) with following component
Fatty alcohol-polyoxyethylene ether (10) 3.6g
Emulsifier os 1.6g
Alkylphenol polyoxyethylene (30) 3.7g
Polyethylene glycol (molecular weight 400) 1.8g
Neopelex 2.5g
Glycerine 2.4g
Deionized water 380g
Place the 500ml glass,, form stable emulsifier aqueous solution B in 50 ℃ of stirring and dissolving 40min.Form solution for standby with 75g deionized water dissolving 0.25g azodiisobutyronitrile.
(c) under agitation, the polymer monomer mixed liquor A is joined among the emulsifier aqueous solution B, form the emulsion C of polymer monomer.
(d) in the 1000ml four-hole boiling flask that thermometer, agitator are housed, add above-mentioned emulsion C.Under agitation, temperature in the bottle is risen to 68 ℃, add the azodiisobutyronitrile solution of 1/3 weight with dropping funel, along with the carrying out of polymerisation, reaction temperature rises to 80 ℃ gradually, and emulsion presents light blue, after treating that a bottle interior temperature falls after rise, emulsion temperature is adjusted into 76 ℃, and insulation 0.5h.Then under uniform temp, with the azodiisobutyronitrile solution of 12 parts of 1.5h dropwise addition of acrylic acid butyl esters, 12 parts, 4 parts acryloyl-oxy propyl group three isopropoxy silane of styrene, 4 parts of gamma-methyl allyl acyloxypropyl three isopropoxy silane, 4 parts of alkenyl amines and 2/3 weight.After dripping, continue insulation 1h.Polymerized emulsion is cooled to below 50 ℃, with ammoniacal liquor adjustment pH value to 7, promptly obtains containing amine copolymer thing emulsion.
(e) in (d) solution for preparing, add 11 parts of silver nitrates, stirred 4 hours down, make amido and Ag at 18 ℃
+Fully complexing makes silver-carrying antibiotic finishing agent.
Embodiment 5
(a) with following monomer
Butyl acrylate 6g
Methyl methacrylate 4g
Ethyl acrylate 4g
Methyl acrylate 4g
Acrylic acid 5g
Gamma-methyl allyl acyloxypropyl trimethoxysilane 14g
Place in the 250ml reactor, stir, form the polymer monomer mixed liquor A.
(b) with following component
Fatty alcohol-polyoxyethylene ether (10) 1.6g
Emulsifier os 2.4g
Alkylphenol polyoxyethylene (30) 3.8g
Polyethylene glycol (molecular weight 400) 1.3g
Lauryl sodium sulfate 2.5g
Glycerine 1.7g
Deionized water 420g
Place the 500ml glass,, form stable emulsifier aqueous solution B in 50 ℃ of stirring and dissolving 40min.Form solution for standby with 75g deionized water dissolving 0.48g benzoyl peroxide.
(c) under agitation, the polymer monomer mixed liquor A is joined among the emulsifier aqueous solution B, form the emulsion C of polymer monomer.
(d) in the 1000ml four-hole boiling flask that thermometer, agitator are housed, add above-mentioned emulsion C.Under agitation, temperature in the bottle is risen to 70 ℃, add the benzoyl peroxide solution of 1/3 weight with dropping funel, along with the carrying out of polymerisation, reaction temperature rises to 80 ℃ gradually, and emulsion presents light blue, after treating that a bottle interior temperature falls after rise, emulsion temperature is adjusted into 78 ℃, and insulation 0.5h.Then under uniform temp, with the benzoyl peroxide solution of 14 parts of 2h dropwise addition of acrylic acid butyl esters, 9 parts, 4 parts acryloyl-oxy propyl group three isopropoxy silane of styrene, 4 parts of vinyltriethoxysilane, 7 parts of alkenyl amines and 2/3 weight.After dripping, continue insulation 1h.Polymerized emulsion is cooled to below 50 ℃, with ammoniacal liquor adjustment pH value to 7, promptly obtains containing amine copolymer thing emulsion.
(e) in (d) solution for preparing, add 14 parts of silver nitrates, stirred 4 hours down, make amido and Ag at 22 ℃
+Fully complexing makes silver-carrying antibiotic finishing agent.
Claims (11)
1. textile finish is characterized in that: this finishing agent is mainly made through the complexing reaction by polymer emulsion and silver salt; Described polymer emulsion is formed through emulsion polymerisation by polymer monomer, emulsifying agent, chain-transferring agent, initator and water, and described silver salt is a silver nitrate.
2. a kind of textile finish according to claim 1, it is characterized in that: described polymer monomer is made up of acrylic ester monomer, styrene, acrylic monomer, organosilicon cross-linking agent, thiazolinyl amine monomer and fluorochemical monomer, and described emulsifying agent is made up of non-ionic surface active agent, anion surfactant.
3. a kind of textile finish according to claim 2 is characterized in that: the consumption of silver nitrate is 8～14 parts by part.
4. a kind of textile finish according to claim 2, it is characterized in that: wherein the consumption of emulsifying agent is 5～20 parts by umber, water is deionized water, its consumption is 300～700 parts by umber, the polymer monomer consumption is 20～275 parts by umber, initiator amount is 0.3～1.2 part by umber, and described consumption is weight.
5. a kind of textile finish according to claim 2 is characterized in that: thiazolinyl amine monomer comprises one or more the combination in alkenyl amine, diallylamine, the triallylamine.
6. a kind of textile finish according to claim 2 is characterized in that: described fluorochemical monomer is one or more in hexafluoropropene, hexafluoropropylene dimmer, perfluoro capryl (N-ethyl-N-ethyl acrylate base), N-methyl perfluorooctyl sulfonyl aminoacrylic acid ethyl ester, N-butyl perfluorooctyl sulfonyl aminoacrylic acid second fat, acrylic acid hexafluoro butyl ester, methacrylic acid hexafluoro butyl ester, trifluoroethyl methacrylate, the methacrylic acid ten difluoro heptyl esters.
7. a kind of textile finish according to claim 2, it is characterized in that: acrylic ester monomer is selected from Isooctyl acrylate monomer, butyl acrylate, ethyl acrylate in the described polymer monomer, one or more in methyl methacrylate, the methyl acrylate; Acrylic monomer is selected from one or both in acrylic acid, the methacrylic acid.
8. a kind of textile finish according to claim 2 is characterized in that: in polymer monomer, the weight of acrylic ester monomer is 18～60 parts by umber, and cinnamic weight is 12～19 parts by umber, and acrylic acid weight is pressed 5～14 parts of umbers.
9. a kind of textile finish according to claim 2 is characterized in that: in the described emulsifying agent, anion surfactant is a neopelex; Non-ionic surface active agent is that fatty alcohol-polyoxyethylene ether, the alkyl number of molecular weight 400～1200 is 8～9 AES and in the polyethylene glycol one or more.
10. a kind of textile finish according to claim 1 is characterized in that: in emulsifying agent, the weight of anion surfactant is 5～10 parts by umber, and the weight of non-ionic surface active agent is 6～15 parts by umber.
11. the preparation method of a textile finish is characterized in that, preparation process is:
A, in reactor, add 3～18 parts of emulsifying agents and 300～400 parts of water, be warming up to about 50 ℃, stir, treat emulsifiers dissolve;
B, 20～100 parts of polymer monomers of adding, emulsification 40min adds 0.15～0.3 part of initator, is warming up to 60～75 ℃ of initiation reactions, and along with the carrying out of polymerisation, reaction temperature rises to 70～85 ℃ gradually, and the reaction time is 1～2h;
After c, question response temperature in the kettle fall after rise, emulsion temperature is adjusted into 70～82 ℃, and insulation 0.5h;
D, under 70～85 ℃ of temperature, drip 80～150 parts of polymer monomers then, and 0.55～0.6 part of initator, the dropping time is 2～4h, drip follow-up continuation of insurance temperature 2～6h, be cooled to below 40 ℃,, promptly get organic-silicon-modified fluorinated acrylate polymer emulsion with filtering.
E, in (d) solution for preparing, add 8～14 parts of silver nitrates, stirred 4 hours down, make the abundant complexing of amido and Ag+, make silver-carrying antibiotic finishing agent at 22 ℃.
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|---|---|---|---|
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|---|---|---|---|
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Application publication date: 20110824 |