CN104130376A - Cationic organosilicon-modified polyurethane emulsion and preparation method thereof - Google Patents
Cationic organosilicon-modified polyurethane emulsion and preparation method thereof Download PDFInfo
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- CN104130376A CN104130376A CN201410311187.7A CN201410311187A CN104130376A CN 104130376 A CN104130376 A CN 104130376A CN 201410311187 A CN201410311187 A CN 201410311187A CN 104130376 A CN104130376 A CN 104130376A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4825—Polyethers containing two hydroxy groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4833—Polyethers containing oxyethylene units
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6681—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38
- C08G18/6688—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3271
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
- C08G77/26—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen nitrogen-containing groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
- C08G77/382—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon
- C08G77/385—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon containing halogens
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
- D06M15/653—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain modified by isocyanate compounds
Abstract
The invention relates to a cationic organosilicon-modified polyurethane emulsion and a preparation method. The method comprises the following steps: 1)synthesizing amino silicone oil, placing octamethylcyclotetrasiloxane, N-beta-(aminoethyl)-gamma- aminopropyl methyl dimethoxyl silane, hexamethyldisiloxane, potassium hydroxide and deionized water in a reaction container under the temperature of 100-110 DEG C to prepare the amino silicone oil; 2)adding haloalkane or epoxy alkyl halide, performing quaternization under 50-90 DEG C, removing micromolecule matter to obtained quaternized modified amino silicone oil; and 3)adding the quaternized modified amino silicone oil in the step 2) drop by drop in high molecular weight polyether polyalcohol, cationic glycol chain extender and isophorone diisocyanate prepolymer and reacting under 60-90 DEG C to obtain cationic organosilicon-modified, then adding deionized water to obtain the cationic organosilicon-modified polyurethane emulsion. The product can be used for textile arrangement, and is especially suitable for acrylic fibers fabric, and has good pilling resistance and hand feel.
Description
Technical field
The present invention relates to a kind of polyaminoester emulsion and preparation method thereof, particularly a kind of cation type organic silicon modified polyaminoester emulsion and preparation method thereof.
Background technology
Fabric, in dress and washing process, through external force continuous actions such as rubbing, rub and scrub, before there is significantly damage, very easily produces pilling phenomenon on fabric.The pilling problem of fabric face generally all can occur on natural fiber and man made fiber fabric, and chemical fibre is comparatively obvious and outstanding, especially acrylic fabric.Fabric pilling had both made appearance of fabrics worsen, and had not only affected the aesthetic property of dress ornament, also affected it and took fastness.
In order to solve the pilling problem of fabric, people at polymeric modification, adjust spinning technique, and arrange modification technology aspect and carried out a large amount of research and exploration work, principle and the method for existing many anti-fluffing and anti-pillings at present, but respectively have its relative merits.As with organic amine or inorganic strong alkali, terylene corroded, reduce fiber strength, though this method is effective wayward; By improving yarn structure and woven fabric structure, although there is certain effect, fabric feeling outward appearance etc. is affected; Also can adopt and manufacture powerful lower terylene or special crosssection silk, although effectively, do not belong to textile dyeing and finishing scope; Also can strengthen singeing and heat setting process, but easily make fabric lose plentiful characteristic, cause that feel plate is firmly coarse, therefore application is restricted; Or in polyster fibre macromole, introduce the 3rd monomer and manufacture anti-pill fibre, as add the 3rd monomer polyoxyethylene glycol, polypropylene glycol, ortho position or a position phthalic acid, aliphatic dibasic acid copolymerization can obtain anti-pill fibre, can be made into good suiting, also can make sweat shirt, housecoat, shirt, bedclothes and adornment etc.; Also can adopt resination method, utilize the finishing compositions such as acrylate copolymer, urethane to carry out arranging after anti-fluffing and anti-pilling.
In these above-mentioned methods, by resination method, can obtain obvious anti-fluffing and play effect, in the method for the current anti-fluffing and anti-pilling at yarn fabric, mainly adopt in this way.Utilize anti-fluffing and anti-pilling agent resin, by being coated the wear-resisting resin molding of one deck at fiber surface, weaken interfibrous slipping property, and utilize resin that fibrous termination is attached on yarn, can effectively improve the pilling resistance of knitted fabrics, but the weak point of these methods be, the anti-fluffing and anti-pilling performance persistence of fabric is poor, after arranging, fabric feeling is stiff, loses original textiles style.
Summary of the invention
One of object of the present invention is to overcome problems of the prior art, and a kind of cation type organic silicon modified polyaminoester emulsion is provided.
Two of object of the present invention is to provide the preparation method of this emulsion.
For achieving the above object, the present invention takes following technical scheme:
A cation type organic silicon modified polyaminoester emulsion, is characterized in that this emulsion is dispersed in and is made in deionized water by cation type organic silicon modified urethane, and solid content is between 40～60%.
A method of preparing above-mentioned cation type organic silicon modified polyaminoester emulsion, is characterized in that the concrete steps of the method are:
A. amido silicon oil is synthetic: the raw material of employing and weight percentage thereof are:
Octamethylcyclotetrasiloxane 80～88%
N-β-(aminoethyl)-γ-aminopropyl methyl dimethoxysilane 15～20%
Hexamethyldisiloxane 0.5～0.9%
Potassium hydroxide 0.2～0.8%
Each composition weight percentage composition sum is 100% above;
Above-mentioned raw materials and deionized water are joined in reaction vessel, at 100～110 ℃ of temperature, react 5～6 hours, the thick liquid obtaining after cooling, is the amido silicon oil of synthesized; Wherein the mol ratio of deionized water and octamethylcyclotetrasiloxane is 1:1;
B. the preparation of quaternised modified amino-silicone oil: haloalkane or epoxy haloalkane are dissolved in ethanol, are heated to after 50～80 ℃, drip while stirring step a gained amido silicon oil, react after 3～5 hours, be warmed up to 80～90 ℃, then react 1～3 hour; Vacuumize, remove after moisture and ethanol, obtain quaternised modified amino-silicone oil; Wherein the mol ratio of haloalkane or epoxy haloalkane and amido silicon oil is 1:(0.7～1.4); The general formula of described haloalkane is:
, wherein, the integer that n is 0～8, * be halogen atom; Described epoxy haloalkane general formula is:
, wherein, the integer that n is 0～3, * be halogen atom.
C. cation type organic silicon modified polyaminoester emulsion is synthetic: polyether glycol, cationic diol chain-extension agent and vulcabond are mixed, react 5～9 hours at 70～90 ℃, obtain positive polyurethane prepolymer; Slowly add again step b gained quaternised modified amino-silicone oil, at 60～90 ℃, react 2～3 hours, regulate pH value to 4～6, slowly add while stirring deionized water, after adding, continue to stir 1 hour, obtain cation type organic silicon modified urethane homogeneous latex emulsion; Deionized water consumption is wherein determined according to the solid content of final product; Wherein the weight ratio of cation type polyurethane prepolymer and quaternised modified amino-silicone oil is 1:0.4～5.0 times; Described chainextender and the mol ratio of polyether glycol are 1～(4: 1), and the mol ratio of the isocyanate group in described vulcabond and the hydroxyl of polyether glycol is 1.0～1.5: 1.
Above-mentioned polyether glycol is molecular weight at 4000～8000 polyoxypropylene glycol and one or both in polyethylene oxide ether glycol.
Above-mentioned described cationic diol chain-extension agent is: 3-dimethylin-1,2-propylene glycol, N, N-bis-(hydroxyethyl)-N ', N '-dimethyl-1,3-propylene diamine or N, N-bis-(2-hydroxypropyl)-N ', N '-dimethyl-1,3-propylene diamine.
Above-mentioned described vulcabond is isophorone diisocyanate.
Cation type organic silicon modified polyaminoester emulsion of the present invention gets up urethane and modified silicon oil, has merged advantage and the feature of these two kinds of conventional finishing compositions.Urethane is the chain segment type block superpolymer being polymerized by polyisocyanates and polyvalent alcohol, because this superpolymer had both had the carbamate strong polarity of section firmly, the kindliness also with polyester soft segment, can make like this polyurethane material there is high strength, resistance to solvent, stronger tack, and the physical and mechanical properties such as good rebound resilience, wear-resisting, anti tear, anti-subduing property.When adopting low-molecular-weight diol containing ionic group as chainextender, can in polyurethane chain, introduce ionogenic group; And organosilicon is to introduce end group or the side group containing amino, epoxy group(ing) or polyethers on polysiloxane macromolecular chain, use it for fabric finishing agent, be adsorbed in fabric fibre surface, give the good film-forming properties of fabric, wrinkle resistance, rebound resilience, flexibility, hydrophobicity, the smooth comfortableness of feel, become the principal item that fabric sofetening arranges.Cation type organic silicon modified urethane of the present invention is in synthetic final stage at urethane, use modified amino silicon oil end-blocking, make urethane and modified amino silicon oil by chemical bond key, thereby avoided the inconsistent problem of blend post-modification silicone oil and urethane, obtained more good finishing effect.
Cation type organic silicon modified polyaminoester emulsion of the present invention is when prepared by product, the urethane of preparation and modified silicon oil are all with positively charged ion charge, thereby this emulsion has stronger positively charged ion charge, utilize the self-emulsifying ability of charged urethane, can prepare easily microemulsified aqueous dispersions, product is expected to obtain special performance.Especially utilize the self-emulsifying feature of finishing composition, can remove low molecule emulsifying agent completely, the size of dispersed particle in reduction system, improves the stability of emulsion dispersion body, and improves and the consistency of other auxiliary agents, realizes the multifunction of fabric finishing agent.Therefore cation type organic silicon modified polyaminoester emulsion has good effect, has more superior finishing effect after the arrangement of fabric.
The cation type organic silicon modified polyaminoester emulsion of preparing by the inventive method, adopt the reactive hydrogen on amino in quaternised modified sealing amido silicon oil segment, thereby change it in processing and take the yellowing degree in process, simultaneously the positively charged ion on finishing composition can with acrylic fibers in the 3rd monomer produce stronger ionization, effectively improve the persistence of anti-pilling finishing effect.By the reactive hydrogen in modified amino silicon oil and urethane-the reacting of NCO functional group, make organosilicon and urethane generation chemical bonding, strengthen resin to the bonding of fabric and treatment effect, made fabric can obtain good feel after arrangement, and significantly improved the pilling resistance of fabric.This cation type organic silicon modified polyaminoester emulsion also can be applicable to the antibacterial finish of fabric simultaneously, further improves the pilling resistance of fabric simultaneously, and keeps other premium properties constant.This cation type organic silicon modified polyaminoester emulsion can be applicable to textile finishing, and especially acrylic fabric, makes it to have splendid anti-fluffing and anti-pilling effect.
Accompanying drawing explanation
Fig. 1 is the performance comparison sheet of fabric after embodiment mono-～five arranges.
Embodiment
Below by embodiment, the invention will be further described, but can not think that the present invention only limits to present embodiment.
Embodiment mono-:
(1) amido silicon oil is synthetic: by 82.0g octamethylcyclotetrasiloxane, 17.7g N-β-(aminoethyl)-γ-aminopropyl methyl dimethoxysilane (commercially available prod of Nanjing Xu Yang Chemical Co., Ltd., trade names are coupling agent KH-602), 0.6g end-capping reagent hexamethyldisiloxane, 0.7g catalyzer potassium hydroxide and 4.1g deionized water join in reaction vessel, be heated to 105 ℃, react 6 hours, the thick liquid obtaining after cooling, is the amido silicon oil of synthesized.
(2) preparation of quaternised modified amino-silicone oil: add 1.1g monobromethane in reaction vessel, be dissolved in ethanol, be heated to after 75 ℃, drip while stirring 100.0g amido silicon oil, continue reaction after 5 hours, be warmed up to 80 ℃, then react 1.5 hours, then vacuumize and remove moisture and ethanol, obtain quaternised modified amino-silicone oil.
(3) cation type organic silicon modified polyaminoester emulsion is synthetic: the polyethers that 30.0g has been dewatered (commercially available prod of Jiangsu Jin Qi urethane company limited, commercial specification is N230) and 10.7g isophorone diisocyanate react 8 hours at 70 ℃.Add 6.5g N, N-bis-(2-hydroxypropyl)-N ', N '-dimethyl-1,3-propylene diamine, continues at 60 ℃, to react 3 hours, slowly adds 50.0g quaternised modified amino-silicone oil, reacts 3 hours, obtains cation type organic silicon modified urethane.The PH value of the cation type organic silicon modified urethane making is adjusted to 5, and 85 ℃ of bath temperatures, slowly add deionized water while stirring, after adding, continue to stir one hour, obtain cation type organic silicon modified urethane homogeneous latex emulsion.
Embodiment bis-:
Monobromethane in the preparation of embodiment mono-(2) quaternised modified amino-silicone oil is replaced with 1.0g epoxy chloropropane, and other raw material consumption and operation steps are identical with embodiment mono-.
Embodiment tri-:
Change the quaternised modified amino-silicone oil consumption in embodiment mono-(3) cation type organic silicon modified polyaminoester emulsion synthetic into 135.0g quaternised modified amino-silicone oil, other raw material consumption and operation steps are identical with embodiment mono-.
Embodiment tetra-:
Change the polyethers in embodiment mono-(3) cation type organic silicon modified polyaminoester emulsion synthetic into polyethers (Jiangsu Jin Qi urethane company limited commercially available prod that 36.0g has dewatered, commercial specification is N240), other raw material consumption and operation steps are identical with embodiment mono-.
Embodiment five:
By the N in embodiment mono-(3) cation type organic silicon modified polyaminoester emulsion synthetic, N-bis-(2-hydroxypropyl)-N ', N '-dimethyl-1,3-propylene diamine changes 6.3g 3-dimethylin-1,2-propylene glycol, N into, N-bis-(hydroxyethyl)-N ', N '-dimethyl-1,3-propylene diamine, other raw material consumption and operation steps are identical with embodiment mono-.
By bath raio, be that 1:20 adds after water, add respectively the cation type organic silicon modified polyaminoester emulsion that makes in embodiment mono-～five (consumption be acrylic fabric weight 3.5%), be warmed up to after 55 ℃ of running 25 min, go out cylinder, dehydration, dries, and at 140 ℃, bakes 3min.Adopt respectively the method for GB/T4802.3-2008 document specifies to detect, the results are shown in Figure 1.
The measurement result of embodiment mono-～five from Fig. 1, utilizes synthetic method provided by the invention, selects suitable, appropriate raw material, can synthesize the pilling resistance finishing composition that feel is smooth, good, than conventional polyurethanes emulsion, exceeds 1 rank.
Claims (5)
1. a cation type organic silicon modified polyaminoester emulsion, is characterized in that this emulsion is directly dispersed in and is made in deionized water by cation type organic silicon modified urethane, and solid content is between 40～60%.
2. a method of preparing cation type organic silicon modified polyaminoester emulsion according to claim 1, is characterized in that the concrete steps of the method are:
A. amido silicon oil is synthetic: the raw material of employing and weight percentage thereof are:
Octamethylcyclotetrasiloxane 80～88%
N-β-(aminoethyl)-γ-aminopropyl methyl dimethoxysilane 15～20%
Hexamethyldisiloxane 0.5～0.9%
Potassium hydroxide 0.2～0.8%
Each composition weight percentage composition sum is 100% above;
Above-mentioned raw materials and deionized water are joined in reaction vessel, at 100～110 ℃ of temperature, react 5～6 hours, the thick liquid obtaining after cooling, is the amido silicon oil of synthesized; Wherein the mol ratio of deionized water and octamethylcyclotetrasiloxane is 1:1;
B. the preparation of quaternised modified amino-silicone oil: haloalkane or epoxy haloalkane are dissolved in ethanol, are heated to after 50～80 ℃, drip while stirring step a gained amido silicon oil, react after 3～5 hours, be warmed up to 80～90 ℃, then react 1～3 hour; Vacuumize, remove after moisture and ethanol, obtain quaternised modified amino-silicone oil; Wherein the mol ratio of haloalkane or epoxy haloalkane and amido silicon oil is 1:(0.7～1.4); The general formula of described haloalkane is:
, wherein, the integer that n is 0～8, * be halogen atom; Described epoxy haloalkane general formula is:
, wherein, the integer that n is 0～3, * be halogen atom;
C. cation type organic silicon modified polyaminoester emulsion is synthetic: polyether glycol, cationic diol chain-extension agent and vulcabond are mixed, react 5～9 hours at 70～90 ℃, obtain positive polyurethane prepolymer; Slowly add again step b gained quaternised modified amino-silicone oil, at 60～90 ℃, react 2～3 hours, regulate pH value to 4～6, slowly add while stirring deionized water, after adding, continue to stir 1 hour, obtain cation type organic silicon modified urethane homogeneous latex emulsion; Deionized water consumption is wherein determined according to the solid content of final product; Wherein the weight ratio of cation type polyurethane prepolymer and quaternised modified amino-silicone oil is 1:0.4～5.0 times; Described chainextender and the mol ratio of polyether glycol are 1～(4: 1), and the mol ratio of the isocyanate group in described vulcabond and the hydroxyl of polyether glycol is 1.0～1.5: 1.
3. method according to claim 3, is characterized in that described polyether glycol is molecular weight at 4000～8000 polyoxypropylene glycol and one or both in polyethylene oxide ether glycol.
4. method according to claim 3, it is characterized in that described cationic diol chain-extension agent is: 3-dimethylin-1,2-propylene glycol, N, N-bis-(hydroxyethyl)-N ', N '-dimethyl-1,3-propylene diamine or N, N-bis-(2-hydroxypropyl)-N ', N '-dimethyl-1,3-propylene diamine.
5. according to the described method of claim 3, it is characterized in that described vulcabond is isophorone diisocyanate.
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Cited By (8)
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| CN107057030A (en) * | 2017-03-27 | 2017-08-18 | 广东银洋环保新材料有限公司 | Cation polyurethane, its preparation method, fabric pretreatment fluid and its application |
| CN108660771A (en) * | 2018-06-13 | 2018-10-16 | 广东传化富联精细化工有限公司 | A kind of preparation method of polyurethane-modified organosilicon moisture control agent microemulsion |
| CN109837760A (en) * | 2019-03-08 | 2019-06-04 | 新昌县高纤纺织有限公司 | Environment-friendly type composite fabric finishing agent and preparation method thereof |
| CN110685161A (en) * | 2019-11-18 | 2020-01-14 | 江南大学 | Preparation method and use method of fabric after-finishing liquid |
| CN111386293A (en) * | 2017-11-28 | 2020-07-07 | 爱克发有限公司 | Aqueous polyurethane resin dispersion |
| CN112680971A (en) * | 2020-12-24 | 2021-04-20 | 创姿服饰(上海)有限公司 | Fabric with excellent performance and application thereof in field of clothes |
| CN114230797A (en) * | 2021-12-30 | 2022-03-25 | 江苏奥斯佳材料科技股份有限公司 | Cationic organosilicon polymer, microemulsion and preparation method thereof |
| CN115094637A (en) * | 2022-07-25 | 2022-09-23 | 博森纺织科技股份有限公司 | Three-proofing finishing process for pure cotton fabric |
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| CN111386293A (en) * | 2017-11-28 | 2020-07-07 | 爱克发有限公司 | Aqueous polyurethane resin dispersion |
| US11708505B2 (en) | 2017-11-28 | 2023-07-25 | Agfa Nv | Aqueous polyurethane resin dispersion |
| CN108660771A (en) * | 2018-06-13 | 2018-10-16 | 广东传化富联精细化工有限公司 | A kind of preparation method of polyurethane-modified organosilicon moisture control agent microemulsion |
| CN109837760A (en) * | 2019-03-08 | 2019-06-04 | 新昌县高纤纺织有限公司 | Environment-friendly type composite fabric finishing agent and preparation method thereof |
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| CN114230797A (en) * | 2021-12-30 | 2022-03-25 | 江苏奥斯佳材料科技股份有限公司 | Cationic organosilicon polymer, microemulsion and preparation method thereof |
| CN114230797B (en) * | 2021-12-30 | 2023-12-01 | 江苏奥斯佳材料科技股份有限公司 | Cationic organosilicon polymer, microemulsion and preparation method thereof |
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