CN105693980A - Blocked organosilicone waterborne polyurethane anti-fluffing-and-pilling agent - Google Patents
Blocked organosilicone waterborne polyurethane anti-fluffing-and-pilling agent Download PDFInfo
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- 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
- C08G18/6541—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen the low-molecular compounds being compounds of group C08G18/34
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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- C08G18/0819—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
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- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/6505—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen the low-molecular compounds being compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6511—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen the low-molecular compounds being compounds of group C08G18/32 or polyamines of C08G18/38 compounds of group C08G18/3203
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- 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
- D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/25—Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/35—Abrasion, pilling or fibrillation resistance
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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Abstract
The invention discloses a blocked organosilicone waterborne polyurethane anti-fluffing-and-pilling agent which is composed of, by weight, 20-30 parts of terminated hydroxy modified silicone oil, 7-15 parts of isophorone diisocyanate, 1.5-2.5 parts of dimethylolpropionic acid, 0.2-0.5 part of 1, 4-butanediol, 0.20-0.24 part of dibutyltin dilaurate, 1-2 parts of triethylamine, 10-20 parts of acetone and 90-120 parts of water. The blocked organosilicone water-borne polyurethane anti-fluffing-and-pilling agent prepared is high in film forming strength, compactness and continuity; fabric finished by using the agent is not clammy and free of adhesion with a roller in the process of application, anti-fluffing-and-pilling effect is improved obviously, and the fabric after being finished is good in hand feeling.
Description
Technical field
The present invention relates to a kind of anti-gigging-pilling agent, it is specifically related to a kind of block organosilicon aqueous polyurethane anti-gigging-pilling agent, this block organosilicon aqueous polyurethane anti-gigging-pilling agent is mainly used in Pilus Caprae seu Ovis, fleece fabrics, washs, the anti-pilling finishing of cotton fabrics and blend fabric thereof。
Background technology
Polyurethane (is called for short PU), i.e. polyurethanes, is the macromolecular compound containing-NHCOO-cellular construction。Nineteen thirty-seven, Germanization scholar OttoBayer utilizes the addition of isocyanates and active hydrogen compounds to prepare polyurethane, has thus established the basis of polyurethane chemistry。The 1950's, solvent borne polyurethane coating is first in Europe dyeing and finishing industry application。Along with people's environmental consciousness strengthens, aqueous polyurethane progressively replaces solvent borne polyurethane in recent years, and is rapidly developed at industry-by-industry。In textile industry, aqueous polyurethane can be used for that water-proof moisture-permeation coating agent, wool shrinkproof finishing agent, fabric wash and wear finisher, synthetic fibers are hydrophilic and the aspect such as antistatic additive, anti-gigging-pilling agent and wet friction fastness improving agent。
In recent years, along with the increase of the development of domestic level and import and export, the exterior quality of textile and the requirement of inherent quality are all increased by people day by day。Particularly to knitted fabric, knitted fabric has the good characteristics such as thin, soft, light, warm, extensively by the favor of people。Knitted fabric is soft, fabric abundant plentiful, warmth retention property good, but the easy pilling of knitted fabric, the fiber of fabric face is subject to the impact of the extraneous factor with self, including fibre property and yarn texture, fabric structure, dyeing and finishing technology and mode of washing etc., dissociates at fabric face and out forms longer lint, fluffiness occurs, in follow-up wearing process, fine hair can not come off in time, just mutually tangles the many spherical granules of formation, fluffiness occurs。Causing easily dirty, appearance of fabrics, quality and wearability are had serious impact by the problem ball top such as electrostatic。But through general resin finishing fabric, usually can affect feel, cause aberration even easily to produce xanthochromia。
At present, the research of the anti-fluffing and anti-pilling resin finishing agent of knitted fabric is based on aqueous polyurethane。Such as document " preparation of organic silicon modified polyurethane type aqueous polyurethane finishing agent and application " (printing and dyeing assistant, 2014, Vol.31, No.5), document describes the preparation and application of organic silicon modified aqueous polyurethane, directly softness segment is introduced aqueous polyurethane, eliminates the trouble additionally adding softening agent, but fabric is tacky during consumption height, arrange the easy roll banding of process。And for example document " development of waterborne blocked polyurethane anti-gigging-pilling agent and application " (hosiery industry, 2009, No.12), document describes the preparation and application of waterborne blocked polyurethane, adopt polyether polyol N330 and toluene-1,4-diisocyanate (TDI) is primary raw material, and synthesized waterborne blocked polyurethane using sodium sulfite as end-capping reagent, prepare and have the aqueous polyurethane of good stability and pilling resistance, but the easy yellowing of fabric after arranging and coloured light is had a certain impact。Additionally, the preparation process of such modified aqueous polyurethane is loaded down with trivial details on market, reaction complexity, reaction condition is difficult to control。In sum, a kind of technique of exploitation is simple, and properties of product are safe and reliable, and the block organosilicon aqueous polyurethane anti-gigging-pilling agent of environmental protection has very big realistic meaning。
Summary of the invention
Goal of the invention: the modified polyurethane adaptability limitation that the present invention is prepared to overcome prior art, the problem affecting feel, stability, easy xanthochromia, the present invention provides a kind of block organosilicon aqueous polyurethane anti-gigging-pilling agent。
Technical scheme: a kind of block organosilicon aqueous polyurethane anti-gigging-pilling agent, described block organosilicon aqueous polyurethane anti-gigging-pilling agent is by following component by weight: terminal hydroxy group modified silicon oil: 20～30 parts, isophorone diisocyanate: 7～15 parts, dihydromethyl propionic acid: 1.5～2.5 parts, BDO: 0.2～0.5 part, dibutyl tin dilaurate: 0.20～0.24 part, triethylamine: 1～2 part, acetone: 10～20 parts, water: 90～120 parts。
As optimization: described terminal hydroxy group modified silicon oil by following component by weight: end hydrogen-based silicone oil: 13～20 parts, allyl polyether: 8～12 parts, chloroplatinic acid catalyst: 0.1～0.13 part, wherein, the molecular weight of allyl polyether is 400 or 500。
As optimization: described terminal hydroxy group modified silicon oil is prepared from by following steps: after in the reactor equipped with thermometer, agitator and reflux, addition end hydrogen-based silicone oil is warming up to 110 DEG C～120 DEG C, it is added dropwise over the allyl polyether reaction 3.5～4h containing chloroplatinic acid catalyst, prepares terminal hydroxy group modified silicon oil。
As optimization: described end hydrogen-based silicone oil by following component by weight: hydrogeneous double-seal head agent: 1～2 part, octamethylcy-clotetrasiloxane (D4): 3～12 parts, concentrated sulfuric acid catalyst: 0.1～0.2 part。
As optimization: described end hydrogen-based silicone oil is prepared from as follows: add octamethylcy-clotetrasiloxane (D4), hydrogeneous double-seal head agent and concentrated sulfuric acid catalyst in a kettle., it is to slowly warm up to 35 DEG C～40 DEG C reaction 6.5h～7h, prepares end hydrogen-based silicone oil。
Beneficial effect: when the block organosilicon aqueous polyurethane that the present invention prepares is as anti-gigging-pilling agent, has film strength height, the feature that compactness is good with seriality。The fabric arranged is not tacky, and the viscous roll of application process, good stability, it is obvious that anti-fluffing and anti-pilling promotes effect, and after arrangement, fabric feeling is good, not easily xanthochromia。Preparation technology is simple simultaneously, does not need special equipment, and reaction condition is gentle, and production cost is low。
In the present invention, from molecular structure, existing aqueous polyurethane anti-pilling finishing agent is innovated improvement as follows: on the one hand: introduce block organosilicon, improve intramolecular hydrophobic-hydrophilic balance, improve the resistance to water after molecular film-forming, take into account flexibility simultaneously；On the other hand, synthesis mode is innovated, to synthesize terminal hydroxy group organic silicon polyether and isophorone diisocyanate for primary raw material synthesis block organosilicon aqueous polyurethane anti-pilling finishing agent, simplify synthesis technique, expand the silicone segments ratio in molecule, thus effectively improving its feel and resistance to water simultaneously。
Obtained molecular weight product mensuration and application on the textile thereof measure as follows with performance:
1) technique for applying on the textile: dipping fabric (2%o.w.f., bath raio 1: 20,40 DEG C × 60min.PH6～7), naturally dry。
2) performance measurement standard:
Pilling resistance: by the mensuration part 1 of GB/T4802.3-2008 textile fabric pilling performance: Circular test method " test, grade with standard sample photo comparison。
Feel: adopt 5 people to grade method, carries out finish fabric touching grading。Feel is divided into 5 grades, and unfinished blank sample is 1 grade。
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be described in detail。
In one aspect of the invention, the present invention provides a kind of block organosilicon aqueous polyurethane, and its structure is as follows:
Wherein, m is 7 or 15；N is 16 or 20；M is the abbreviation of aqueous polyurethane hard section。
In another aspect of the present invention, the present invention provides a kind of above-mentioned block organosilicon aqueous polyurethane anti-gigging-pilling agent Preparation Method, and it comprises the steps:
1) add D4, hydrogeneous double-seal head agent and concentrated sulfuric acid catalyst in a kettle., be to slowly warm up to 35 DEG C～40 DEG C reaction 6.5h～7h, prepare end hydrogen-based silicone oil, react as follows:
2), after addition end hydrogen-based silicone oil is warming up to 110 DEG C～120 DEG C in the reactor equipped with thermometer, agitator and reflux, it is added dropwise over the allyl polyether reaction 3.5～4h containing chloroplatinic acid catalyst, prepares terminal hydroxy group modified silicon oil, react as follows:
3) by the step 2 after dehydrated) product, dibutyl tin dilaurate and isophorone diisocyanate add in reactor, reacting by heating 1h, be subsequently adding dihydromethyl propionic acid and BDO, react 1.5h；Adding proper amount of acetone and regulate viscosity, add triethylamine and neutralize, quickly stir 30min after cooling, the high speed that finally adds water emulsifying obtains block organosilicon aqueous polyurethane anti-gigging-pilling agent. generate product structure as follows:
Wherein, m is 7 or 15；N is 16 or 20；M is the abbreviation of aqueous polyurethane hard section。
In another aspect of the present invention, the present invention provides block organosilicon aqueous polyurethane as anti-gigging-pilling agent application in textile industry。
Specific embodiment one:
A kind of block organosilicon aqueous polyurethane anti-gigging-pilling agent, described block organosilicon aqueous polyurethane anti-gigging-pilling agent is by following component by weight: terminal hydroxy group modified silicon oil: 20 parts, isophorone diisocyanate: 7 parts, dihydromethyl propionic acid: 1.5 parts, BDO: 0.2 part, dibutyl tin dilaurate: 0.20 part, triethylamine: 1 part, acetone: 10 parts, water: 90 parts。
A kind of preparation method of the block organosilicon aqueous polyurethane anti-gigging-pilling agent described in basis, terminal hydroxy group modified silicon oil after dehydrated, dibutyl tin dilaurate and isophorone diisocyanate are added in reactor, reacting by heating 1h, it is subsequently adding dihydromethyl propionic acid and 1,4-butanediol, reacts 1.5h；Adding proper amount of acetone and regulate viscosity, add triethylamine and neutralize, quickly stir 30min after cooling, the high speed that finally adds water emulsifying obtains block organosilicon aqueous polyurethane anti-gigging-pilling agent。
Described terminal hydroxy group modified silicon oil is by following component by weight: end hydrogen-based silicone oil: 13 parts, allyl polyether: 8 parts, chloroplatinic acid catalyst: 0.1 part, wherein, the molecular weight of allyl polyether is 400 or 500。
Described terminal hydroxy group modified silicon oil is prepared from by following steps: after in the reactor equipped with thermometer, agitator and reflux, addition end hydrogen-based silicone oil is warming up to 110 DEG C, it is added dropwise over the allyl polyether reaction 3.5h containing chloroplatinic acid catalyst, prepares terminal hydroxy group modified silicon oil。
Described end hydrogen-based silicone oil is by following component by weight: hydrogeneous double-seal head agent: 1 part, octamethylcy-clotetrasiloxane (D4): 3 parts, concentrated sulfuric acid catalyst: 0.1 part。
Described end hydrogen-based silicone oil is prepared from as follows: add octamethylcy-clotetrasiloxane (D4), hydrogeneous double-seal head agent and concentrated sulfuric acid catalyst in a kettle., is to slowly warm up to 35 DEG C of reaction 6.5h, prepares end hydrogen-based silicone oil。
Specific embodiment two:
A kind of block organosilicon aqueous polyurethane anti-gigging-pilling agent, described block organosilicon aqueous polyurethane anti-gigging-pilling agent is by following component by weight: terminal hydroxy group modified silicon oil: 30 parts, isophorone diisocyanate: 15 parts, dihydromethyl propionic acid: 2.5 parts, BDO: 0.5 part, dibutyl tin dilaurate: 0.24 part, triethylamine: 2 parts, acetone: 20 parts, water: 120 parts。
A kind of preparation method of the block organosilicon aqueous polyurethane anti-gigging-pilling agent described in basis, terminal hydroxy group modified silicon oil after dehydrated, dibutyl tin dilaurate and isophorone diisocyanate are added in reactor, reacting by heating 1h, it is subsequently adding dihydromethyl propionic acid and 1,4-butanediol, reacts 1.5h；Adding proper amount of acetone and regulate viscosity, add triethylamine and neutralize, quickly stir 30min after cooling, the high speed that finally adds water emulsifying obtains block organosilicon aqueous polyurethane anti-gigging-pilling agent。
Described terminal hydroxy group modified silicon oil is by following component by weight: end hydrogen-based silicone oil: 20 parts, allyl polyether: 12 parts, chloroplatinic acid catalyst: 0.13 part, wherein, the molecular weight of allyl polyether is 400 or 500。
Described terminal hydroxy group modified silicon oil is prepared from by following steps: after in the reactor equipped with thermometer, agitator and reflux, addition end hydrogen-based silicone oil is warming up to 120 DEG C, it is added dropwise over the allyl polyether reaction 4h containing chloroplatinic acid catalyst, prepares terminal hydroxy group modified silicon oil。
Described end hydrogen-based silicone oil is by following component by weight: hydrogeneous double-seal head agent: 2 parts, octamethylcy-clotetrasiloxane (D4): 12 parts, concentrated sulfuric acid catalyst: 0.2 part。
Described end hydrogen-based silicone oil is prepared from as follows: add octamethylcy-clotetrasiloxane (D4), hydrogeneous double-seal head agent and concentrated sulfuric acid catalyst in a kettle., is to slowly warm up to 40 DEG C of reaction 7h, prepares end hydrogen-based silicone oil。
Specific embodiment three:
A kind of block organosilicon aqueous polyurethane anti-gigging-pilling agent, described block organosilicon aqueous polyurethane anti-gigging-pilling agent is by following component by weight: terminal hydroxy group modified silicon oil: 27 parts, isophorone diisocyanate: 12 parts, dihydromethyl propionic acid: 1.9 parts, BDO: 0.3 part, dibutyl tin dilaurate: 0.22 part, triethylamine: 1.4 parts, acetone: 17 parts, water: 107 parts。
A kind of preparation method of the block organosilicon aqueous polyurethane anti-gigging-pilling agent described in basis, terminal hydroxy group modified silicon oil after dehydrated, dibutyl tin dilaurate and isophorone diisocyanate are added in reactor, reacting by heating 1h, it is subsequently adding dihydromethyl propionic acid and 1,4-butanediol, reacts 1.5h；Adding proper amount of acetone and regulate viscosity, add triethylamine and neutralize, quickly stir 30min after cooling, the high speed that finally adds water emulsifying obtains block organosilicon aqueous polyurethane anti-gigging-pilling agent。
Described terminal hydroxy group modified silicon oil is by following component by weight: end hydrogen-based silicone oil: 18 parts, allyl polyether: 10 parts, chloroplatinic acid catalyst: 0.11 part, wherein, the molecular weight of allyl polyether is 400 or 500。
Described terminal hydroxy group modified silicon oil is prepared from by following steps: after in the reactor equipped with thermometer, agitator and reflux, addition end hydrogen-based silicone oil is warming up to 114 DEG C, it is added dropwise over the allyl polyether reaction 3.6h containing chloroplatinic acid catalyst, prepares terminal hydroxy group modified silicon oil。
Described end hydrogen-based silicone oil is by following component by weight: hydrogeneous double-seal head agent: 1.3 parts, octamethylcy-clotetrasiloxane (D4): 8 parts, concentrated sulfuric acid catalyst: 0.14 part。
Described end hydrogen-based silicone oil is prepared from as follows: add octamethylcy-clotetrasiloxane (D4), hydrogeneous double-seal head agent and concentrated sulfuric acid catalyst in a kettle., is to slowly warm up to 36 DEG C of reaction 6.8h, prepares end hydrogen-based silicone oil。
Specific embodiment four:
The preparation method of a kind of block organosilicon aqueous polyurethane, it comprises the steps:
1, the preparation section of hydrogen-based modified silicon oil is held。
(1) raw material preparing both-end hydrogen-based modified silicon oil includes end hydrogen double-seal head agent, molecule chain extender and acid catalyst, the parts by weight respectively 1 part, 6.41 parts and 0.15 part of this end hydrogen double-seal head agent, molecule chain extender and acid catalyst, wherein, end hydrogen double-seal head agent is 1,1,3,3-tetramethyl disiloxane, molecule chain extender is the famous D4 of octamethylcy-clotetrasiloxane, and acid catalyst is concentrated sulphuric acid。
(2) hold hydrogen-based modified silicon oil preparation method include as follows successively: equipped with thermometer, agitator, condensing unit four mouthfuls of reactors in addition octamethylcy-clotetrasiloxane 64.1 grams, end hydrogen double-seal head agent 10 grams, concentrated sulphuric acid 1.5 grams, 35 DEG C of reaction 6.5h, namely obtain end hydrogen-based modified silicon oil。
2, the preparation section of terminal hydroxy group block silicone oil。
(1) raw material preparing terminal hydroxy group block silicone oil includes end hydrogen-based modified silicon oil, allyl polyether and chloroplatinic acid catalyst, the weight of this end hydrogen-based modified silicon oil, allyl polyether and chloroplatinic acid catalyst respectively 10 parts, 20 parts and 0.16 part, wherein-EO-the number in allyl polyether is 8 or 10。
(2) preparation method of terminal hydroxy group block silicone oil in turn includes the following steps: equipped with thermometer, agitator, condensing unit four mouthfuls of reactors add end hydrogen-based modified silicon oils 10 grams, under low whipping speed 45 revs/min, it is warming up to 110 DEG C, then the mix reagent of 20 grams of allyl polyethers of dropping and 0.16 gram of chloroplatinic acid, it is warming up to 130 DEG C of reaction 3.5h after dropwising, obtains terminal hydroxy group block silicone oil。
3, the preparation section of block organosilicon aqueous polyurethane anti-pilling finishing agent。
(1) raw material preparing block organosilicon aqueous polyurethane anti-pilling finishing include the end hydroxyl silicone oil of 20 grams, 7 grams isophorone diisocyanate, 1.5 grams dihydromethyl propionic acid, 0.2 gram BDO, the dibutyl tin dilaurate catalyst of 0.002g, 1 gram triethylamine, the acetone of 10 grams of parts, the water of 90 grams；
(2) 20 grams of end hydroxyl silicone oils after dehydrated, 0.24 gram of dibutyl tin dilaurate and 7 grams of isophorone diisocyanate are added in reactors, reacting by heating 1h, it is subsequently adding 1.5 grams of dihydromethyl propionic acids and 0.2 gram of BDO, reacts 1.5h；Adding proper amount of acetone and regulate viscosity, add triethylamine and neutralize, quickly stir 30min after cooling, the high speed that finally adds water emulsifying obtains block organosilicon aqueous polyurethane anti-gigging-pilling agent。The finishing agent of solid content 39% is obtained after decompression distillation。
In each embodiment, all raw materials, fabric are commercially available。Obtained molecular weight product mensuration and application on the textile thereof measure as follows with performance:
1) technique for applying on the textile: dipping fabric (2%o.w.f., bath raio 1: 20,40 DEG C × 60min.PH6～7), naturally dry。
2) performance measurement standard:
Pilling resistance: by the mensuration part 1 of GB/T4802.3-2008 textile fabric pilling performance: Circular test method " test, grade with standard sample photo comparison。
Feel: adopt 5 people to grade method, carries out finish fabric touching grading。Feel is divided into 5 grades, and unfinished blank sample is 1 grade。
In the present invention, from molecular structure, existing aqueous polyurethane anti-pilling finishing agent is innovated improvement as follows: on the one hand: introduce block organosilicon, improve intramolecular hydrophobic-hydrophilic balance, improve the resistance to water after molecular film-forming, take into account flexibility simultaneously；On the other hand, synthesis mode is innovated, to synthesize terminal hydroxy group organic silicon polyether and isophorone diisocyanate for primary raw material synthesis block organosilicon aqueous polyurethane anti-pilling finishing agent, simplify synthesis technique, expand the silicone segments ratio in molecule, thus effectively improving its feel and resistance to water simultaneously。
Being modifiied by above-mentioned innovation, inventor finds in surprise, when the block organosilicon aqueous polyurethane that inventive method prepares is as anti-gigging-pilling agent, has film strength height, the feature that compactness is good with seriality。The fabric arranged is not tacky, and the viscous roll of application process, good stability, it is obvious that anti-fluffing and anti-pilling promotes effect, and after arrangement, fabric feeling is good, not easily xanthochromia。Preparation technology is simple simultaneously, does not need special equipment, and reaction condition is gentle, and production cost is low。
The present invention is not limited to above-mentioned preferred forms; anyone can draw other various forms of products under the enlightenment of the present invention; no matter but in its shape or structure, do any change, every have same or like with the application like technical scheme, all fall within protection scope of the present invention。
Claims (5)
1. a block organosilicon aqueous polyurethane anti-gigging-pilling agent, it is characterized in that: described block organosilicon aqueous polyurethane anti-gigging-pilling agent by following component by weight: terminal hydroxy group modified silicon oil: 20～30 parts, isophorone diisocyanate: 7～15 parts, dihydromethyl propionic acid: 1.5～2.5 parts, BDO: 0.2～0.5 part, dibutyl tin dilaurate: 0.20～0.24 part, triethylamine: 1～2 part, acetone: 10～20 parts, water: 90～120 parts。
2. block organosilicon aqueous polyurethane anti-gigging-pilling agent according to claim 1, it is characterized in that: described terminal hydroxy group modified silicon oil by following component by weight: end hydrogen-based silicone oil: 13～20 parts, allyl polyether: 8～12 parts, chloroplatinic acid catalyst: 0.1～0.13 part, wherein, the molecular weight of allyl polyether is 400 or 500。
3. the preparation method of block organosilicon aqueous polyurethane anti-gigging-pilling agent according to claim 2, it is characterized in that: described terminal hydroxy group modified silicon oil is prepared from by following steps: after in the reactor equipped with thermometer, agitator and reflux, addition end hydrogen-based silicone oil is warming up to 110 DEG C～120 DEG C, it is added dropwise over the allyl polyether reaction 3.5～4h containing chloroplatinic acid catalyst, prepares terminal hydroxy group modified silicon oil。
4. the preparation method of the block organosilicon aqueous polyurethane anti-gigging-pilling agent according to any one of claim 2-3, it is characterised in that: described end hydrogen-based silicone oil by following component by weight: hydrogeneous double-seal head agent: 1～2 part, octamethylcy-clotetrasiloxane (D4): 3～12 parts, concentrated sulfuric acid catalyst: 0.1～0.2 part。
5. block organosilicon aqueous polyurethane anti-gigging-pilling agent according to claim 4, it is characterized in that: described end hydrogen-based silicone oil is prepared from as follows: add octamethylcy-clotetrasiloxane (D4), hydrogeneous double-seal head agent and concentrated sulfuric acid catalyst in a kettle., it is to slowly warm up to 35 DEG C～40 DEG C reaction 6.5h～7h, prepares end hydrogen-based silicone oil。
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108707218A (en) * | 2018-06-14 | 2018-10-26 | 南通斯恩特纺织科技有限公司 | A kind of preparation method of the wet elevator that rubs of hyperbranched silicone block aqueous polyurethane |
| CN109134808A (en) * | 2018-08-07 | 2019-01-04 | 苏州思德新材料科技有限公司 | The preparation method of flame retardant polyurethane sponge based on organic foam stabilizer |
| CN109503789A (en) * | 2018-12-02 | 2019-03-22 | 广州市斯洛柯高分子聚合物有限公司 | A kind of polyurethane-modified silicone resin emulsion and its preparation method and application |
| CN109734863A (en) * | 2018-12-29 | 2019-05-10 | 太仓宝霓实业有限公司 | Aqueous polyurethane and preparation method thereof and anti-gigging-pilling agent composition |
| CN113957719A (en) * | 2021-11-12 | 2022-01-21 | 南通大学 | Organic silicon polyurethane waterproof moisture permeable coating agent and preparation method and finishing process thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101381462A (en) * | 2008-09-10 | 2009-03-11 | 中国科学技术大学 | Polysiloxane binary alcohol with polyether block and preparation method thereof |
| CN101434615A (en) * | 2008-12-15 | 2009-05-20 | 蓝星化工新材料股份有限公司江西星火有机硅厂 | Polyether modified silicon oil with ultra-low surface tension and synthesis process thereof |
| CN102031697A (en) * | 2010-11-05 | 2011-04-27 | 辽宁科隆精细化工股份有限公司 | Method for preparing polyester and polyether modified silicone oil ternary copolymer textile finishing agent |
| CN102617863A (en) * | 2012-03-30 | 2012-08-01 | 广东工业大学 | Preparation method of hydrophilic block polyether aminosilicone |
| CN102977315A (en) * | 2012-11-13 | 2013-03-20 | 青岛文创科技有限公司 | Preparation method of polyether polyorganosiloxanediatomic alcoholmodified watersoluble polyurethane |
| CN103951809A (en) * | 2014-04-23 | 2014-07-30 | 西安工程大学 | Preparation method of polyurethane modified organic silicon multipolymer fabric softening agent |
-
2016
- 2016-04-14 CN CN201610232677.7A patent/CN105693980A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101381462A (en) * | 2008-09-10 | 2009-03-11 | 中国科学技术大学 | Polysiloxane binary alcohol with polyether block and preparation method thereof |
| CN101434615A (en) * | 2008-12-15 | 2009-05-20 | 蓝星化工新材料股份有限公司江西星火有机硅厂 | Polyether modified silicon oil with ultra-low surface tension and synthesis process thereof |
| CN102031697A (en) * | 2010-11-05 | 2011-04-27 | 辽宁科隆精细化工股份有限公司 | Method for preparing polyester and polyether modified silicone oil ternary copolymer textile finishing agent |
| CN102617863A (en) * | 2012-03-30 | 2012-08-01 | 广东工业大学 | Preparation method of hydrophilic block polyether aminosilicone |
| CN102977315A (en) * | 2012-11-13 | 2013-03-20 | 青岛文创科技有限公司 | Preparation method of polyether polyorganosiloxanediatomic alcoholmodified watersoluble polyurethane |
| CN103951809A (en) * | 2014-04-23 | 2014-07-30 | 西安工程大学 | Preparation method of polyurethane modified organic silicon multipolymer fabric softening agent |
Non-Patent Citations (1)
| Title |
|---|
| "《轻化工助剂配方》" * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108707218A (en) * | 2018-06-14 | 2018-10-26 | 南通斯恩特纺织科技有限公司 | A kind of preparation method of the wet elevator that rubs of hyperbranched silicone block aqueous polyurethane |
| CN109134808A (en) * | 2018-08-07 | 2019-01-04 | 苏州思德新材料科技有限公司 | The preparation method of flame retardant polyurethane sponge based on organic foam stabilizer |
| CN109503789A (en) * | 2018-12-02 | 2019-03-22 | 广州市斯洛柯高分子聚合物有限公司 | A kind of polyurethane-modified silicone resin emulsion and its preparation method and application |
| CN109734863A (en) * | 2018-12-29 | 2019-05-10 | 太仓宝霓实业有限公司 | Aqueous polyurethane and preparation method thereof and anti-gigging-pilling agent composition |
| CN109734863B (en) * | 2018-12-29 | 2021-01-15 | 太仓宝霓实业有限公司 | Waterborne polyurethane, preparation method thereof and anti-pilling agent composition |
| CN113957719A (en) * | 2021-11-12 | 2022-01-21 | 南通大学 | Organic silicon polyurethane waterproof moisture permeable coating agent and preparation method and finishing process thereof |
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Application publication date: 20160622 |