CN104650363A - Preparation method of hyperbranched ternary polymerization organic silicon - Google Patents
Preparation method of hyperbranched ternary polymerization organic silicon Download PDFInfo
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Abstract
The invention discloses a preparation method of hyperbranched ternary polymerization organic silicon. The preparation method comprises the following steps: preparing allyl polyoxyethylene glycidyl ether; preparing epoxy-terminated polyether block siloxane; preparing polyether/epoxy block silicone oil; preparing hyperbranched ternary polymerization organic silicon. According to the preparation method, a hyperbranched polymer and linear polyether amino block organic silicon are bonded together to research a novel organic silicon softener with a novel modified organic silicon chemical structure, and a synthesized hyperbranched matter is capable of enhancing the cohesive force among fibers and endowing a fabric with soft, plump and washable hand feel, high in molecular mass and low in viscosity and has much hydrophilic groups; the problem that emulsion of traditional amino modified silicon oil is easily broken is solved, the product has self-emulsifying property in water and is good in emulsion stability; the yellowing property is reduced, and the hydrophily is enhanced; a processed fabric is good in hydrophily and low in yellowing property and is bonded with fabric by virtue of chemical bonds, so that the washability is improved, and the fabric has a flexible effect of amino silicon oil.
Description
Technical field
The invention belongs to field of organic silicon, be specifically related to the organosilyl preparation method of a kind of hyperbranched terpolymer.
Background technology
At present, amido silicon oil becomes dyeing application post-finishing agent very widely with its excellent softness, smoothness, and the fabric after it arranges has softness, performance smooth, washable and comfortable and easy to wear.But amido silicon oil makes Hydrophilic Fiber be deteriorated at the arrangement mode of fiber, fabric moisture and snugness of fit decline; White after arranging with it or light coloured fabrics, after high temperature bakes, there will be xanthochromia in various degree and aberration; And its stability of emulsion is poor, in storage and transportation, easily there is " floating oil breakdown of emulsion " phenomenon.
At present, the recent development of weaving organic silicone finishing agent is the silicone based softening agent of the amino terpolymer of linear polyether block, that a class use is widely applicable, in water, there is automatic emulsifying performance, the fabric organic silicone finishing agent of good emulsion stability, through its arrange after fabric have good flexibility, wetting ability, static resistance and not look become performance.Also some performances silicone softening agent relatively is preferably had at present, if publication date is on October 5th, 2011, publication number is in the Chinese patent of CN102206921A, patent discloses a kind of preparation method of polyether block amino silicone soft finishing agent, this preparation method comprises the following steps: A, employing vulcabond, polyether Glycols and hydroxy silicon oil are raw material, prepare the polyether block organic silicon polyurethane with-OH end group; B, with the polyether block organic silicon polyurethane with-OH end group for main raw material, after carrying out chain extending reaction with silane coupling agent, then add acid neutralization, water-dispersion obtains polyether block amino silicone soft finishing agent.And for example publication date is on August 1st, 2012, publication number is in the Chinese patent of CN102617863A, patent discloses a kind of preparation method of hydrophilic block polyether aminosilicone, this preparation method mainly comprises the following steps: A, preparation end containing hydrogen silicone oil intermediate, employing cyclosiloxane is main raw material, carry out block reaction with hydrogeneous double-seal head, generate end containing hydrogen silicone oil intermediate; B, preparation end epoxy silicon oil intermediate, carry out addition reaction by end containing hydrogen silicone oil and allyl group epoxidized polyether, generate end epoxy silicon oil; The preparation of C, finished product, adopts end epoxy silicon oil and polyetheramine to carry out ammonia solution ring-opening reaction, obtained hydrophilic block polyether aminosilicone.The product of above two kinds of preparation methods all belongs to linear polyether block amido silicon oil, by introducing the polyether segment of macromolecule on silicone backbone, improve the wetting ability of fabric after arranging, and improve the state of product in water, improve product emulsion stability, what macromolecular chain was introduced mostly is primary amine groups, relatively stable, be not easy oxidation, the fabric after arrangement produces Yellowing hardly.But as line style terpolymer organosilicon, macromolecular main chain is introduced the polyether segment of macromolecule, cut off by the methyl smooth layer in silicon-oxygen backbone, and molecular weight is large not as good as amido silicon oil, so its soft slipping is not as amido silicon oil; In addition, by amino block in main chain, by sterically hindered and impact that is polarity, in the absorption of fiber surface not as good as amido silicon oil, so its washing fastness is relatively poor.
In sum, the preparation method of the silicone softening agent of the soft slipping of a kind of wetting ability, stability of emulsion and amido silicon oil having tri-block silicone oil concurrently is not also had at present.
Summary of the invention
Goal of the invention: the invention provides the organosilyl preparation method of a kind of hyperbranched terpolymer, the over-expense compound of synthesis has reticulated structure, can not only cohesive force between fortifying fibre, can also strengthen the cohesive force between yarn.
Technical scheme: the organosilyl preparation method of a kind of hyperbranched terpolymer, comprises the steps:
(1) preparation of allyl polyethenoxy glycidyl ether:
Allyl polyethenoxy ether and epoxy chloropropane are mixed, employing sodium hydride is catalyzer, under 55-65 DEG C of condition, react 1.5-2.5h, and then unnecessary epoxy chloropropane is sloughed in decompression; Drip a certain amount of aqueous sodium hydroxide solution to reaction system again, control temperature of reaction and react 1.5-3h under 30-40 DEG C of condition; End capped polyether product is obtained through aftertreatment removing impurity such as underpressure distillation filtrations after reaction terminates;
Concrete reaction formula is as follows:
(2) preparation of epoxy group(ing) end capped polyether block silicone:
Tetramethyl-dihydro base sily oxide and allyl polyethenoxy glycidyl ether are mixed according to the ratio of 1:2.2, stir, add the catalyzer of 1%, consumption is 20mg/kg, be warming up to 80 DEG C ~ 90 DEG C reaction 3 ~ 4h, underpressure distillation removing low-boiling-point substance obtains end ring oxygen closure agent;
Concrete reaction formula is as follows:
(3) preparation of polyether/epoxy resin block silicone oil:
Obtained epoxy group(ing) end capped polyether block silicone, octamethylcyclotetrasiloxane and solvent is even, stir after being warmed up to certain temperature, add a certain amount of alkaline catalysts, continue to be warming up to 100 DEG C ~ 110 DEG C, insulation reaction 4 ~ 5h; Decompression removing low-boiling-point substance again, obtained polyethers/happy looks or appearance block silicone oil;
Concrete reaction formula is as follows:
(4) the organosilyl preparation of the amino block of hyperbranched polyether:
Homemade polyether/epoxy resin block silicone oil, diethylenetriamine are added with nitrogen charging device according to a certain percentage, in three mouthfuls of reactors of reflux condensing tube, add solvent Virahol, consumption is 30% of reaction-ure mixture, 80 DEG C are warmed up to after stirring, after insulation reaction 5h, underpressure distillation, except desolventizing, obtains the amino block polysiloxane of light yellow transparent liquid hyperbranched polyether;
Concrete reaction formula is as follows:
A is
As optimization: described step 1) in the polymerization degree of allyl polyethenoxy ether be 19 ~ 25.
As optimization: described step 1) in the mol ratio of allyl polyethenoxy ether, epoxy chloropropane and sodium hydroxide be 1:1.4:1.3.
As optimization: described step 2) in hydrogeneous double-seal head and the mol ratio of epoxy group(ing) end capped polyether block silicone be 1:2 ~ 2.5.
As optimization: described step 2) in catalyzer be isopropyl alcohol solution of chloroplatinic acid.
As optimization: described step 3) in epoxy group(ing) end capped polyether block silicone, octamethylcyclotetrasiloxane mol ratio be 1:15 ~ 20.
As optimization: described step 3) in catalyzer be Tetramethylammonium hydroxide, catalyst levels is 0.035% ~ 0.055%.
As optimization: described step 3) and 4) in solvent be Virahol, solvent load is the 26%-32% of reaction mass quality.
As optimization: described step 4) in polyether/epoxy resin block silicone oil and the mol ratio of diethylenetriamine be 1.5 ~ 2:1.
Beneficial effect: concrete advantage of the present invention is as follows:
1, amino to hyperbranched polymer and linear polyether block organosilicon combines and is developed into novel organosilicon softening agent by the present invention, it has new modified organic silicon chemical structure, cohesive force between the over-expense compound energy fortifying fibre of synthesis, molecular mass is high, viscosity is low, hydrophilic radical is many, can give the feel that fabric sofetening is plentiful and washable.Diethylenetriamine adds wetting ability and improves weather resistance and effect.Polyethers is added at molecule segment, and EO number n in polyethers is controlled at 25-40, polyether group has extremely strong wetting ability, hydrophobic organosilicon can be made to become hydrophilic organic silicon, solve the problem of emulsion floating oil, simplify emulsifying process, and the fabric after organic silicon modified by polyether arranges also have good soil resistant and static resistance, a series of shortcoming such as " moisture absorption absorption of perspiration is low ", " easily producing frictional static " after overcoming simple polysiloxane finish fabric; Recycling diethylenetriamine carries out hyperbranched, make structure very easily and water form hydrogen bond, emulsification can be carried out without emulsifying agent, overcome the problem of the easy floating oil breakdown of emulsion of conventional organic silicone oil softening agent.Simultaneously, due to the reticulated structure that this product is hyperbranched, the reactive forces such as fiber utilization hydrogen bond in single yarn can not only be coated togather, the reticulated structure of super large can also be utilized to be coated togather by threads simultaneously, considerably increase yarn and interfibrous cohesive force.
2, when silicone oil being made housekeeping liquid, being suitable for Glacial acetic acid, its pH value being regulated between 5 ~ 6, adding of acetic acid, to the formation of dressing liquid and the raising of stability, there is material impact.This mainly because acetic acid can react with amino wherein and generate quaternary ammonium salt, enhances the polarity of silicone oil, makes it be easy to be dispersed in water, and forms O/W type emulsion.The amino block silicone oil of hyperbranched polyether solves the easy breakdown of emulsion problem of traditional amino-modified silicone oil in storage and use procedure, and product has automatic emulsifying performance in water, good emulsion stability; Reduce yellowing, enhance wetting ability, be particularly suitable for the softening of white or light coloured fabrics.
3, the fabric that this Product organization goes out overcomes the shortcoming of common terpolymer silicone oil, and its good hydrophilic property is yellowing little, is combined, adds washing fastness with fabric with chemical bond form, has again the soft effect of amido silicon oil simultaneously.
Accompanying drawing explanation
Fig. 1 is the absorption schematic diagram of silicone softening agent of the present invention.
Embodiment
Below in conjunction with specific embodiment, the present invention will be described in detail.
Specific embodiment 1:
The organosilyl preparation method of a kind of hyperbranched terpolymer, comprises the steps:
(1) preparation of allyl polyethenoxy glycidyl ether:
Allyl polyethenoxy ether and epoxy chloropropane are mixed, employing sodium hydride is catalyzer, under 55 DEG C of conditions, react 1.5h, and then unnecessary epoxy chloropropane is sloughed in decompression; Drip a certain amount of aqueous sodium hydroxide solution to reaction system again, control temperature of reaction and react 1.5h under 30 DEG C of conditions; End capped polyether product is obtained through aftertreatment removing impurity such as underpressure distillation filtrations after reaction terminates.The polymerization degree of described allyl polyethenoxy ether is 19.The mol ratio of described allyl polyethenoxy ether, epoxy chloropropane and sodium hydroxide is 1:1.4:1.3.
(2) preparation of epoxy group(ing) end capped polyether block silicone:
Tetramethyl-dihydro base sily oxide and allyl polyethenoxy glycidyl ether are mixed according to the ratio of 1:2.2, stir, add the catalyzer of 1%, consumption is 20mg/kg, is warming up to 80 DEG C of reaction 3h, and underpressure distillation removing low-boiling-point substance obtains end ring oxygen closure agent.The mol ratio of described hydrogeneous double-seal head and epoxy group(ing) end capped polyether block silicone is 1:2.Described catalyzer is isopropyl alcohol solution of chloroplatinic acid.
(3) preparation of polyether/epoxy resin block silicone oil:
Obtained epoxy group(ing) end capped polyether block silicone, octamethylcyclotetrasiloxane and solvent is even, stir after being warmed up to certain temperature, add a certain amount of alkaline catalysts, continue to be warming up to 100 DEG C, insulation reaction 4h; Decompression removing low-boiling-point substance again, obtained polyethers/happy looks or appearance block silicone oil.The mol ratio of described epoxy group(ing) end capped polyether block silicone, octamethylcyclotetrasiloxane is 1:15.Described catalyzer is Tetramethylammonium hydroxide, and catalyst levels is 0.035%.
(4) the organosilyl preparation of the amino block of hyperbranched polyether:
Homemade polyether/epoxy resin block silicone oil, diethylenetriamine are added with nitrogen charging device according to a certain percentage, in three mouthfuls of reactors of reflux condensing tube, add solvent Virahol, consumption is 30% of reaction-ure mixture, 80 DEG C are warmed up to after stirring, after insulation reaction 5h, underpressure distillation, except desolventizing, obtains the amino block polysiloxane of light yellow transparent liquid hyperbranched polyether.Described solvent is Virahol, and solvent load is 26% of reaction mass quality.The mol ratio of described polyether/epoxy resin block silicone oil and diethylenetriamine is 1.5:1.
Specific embodiment 2:
The organosilyl preparation method of a kind of hyperbranched terpolymer, comprises the steps:
(1) preparation of allyl polyethenoxy glycidyl ether:
Allyl polyethenoxy ether and epoxy chloropropane are mixed, employing sodium hydride is catalyzer, under 65 DEG C of conditions, react 2.5h, and then unnecessary epoxy chloropropane is sloughed in decompression; Drip a certain amount of aqueous sodium hydroxide solution to reaction system again, control temperature of reaction and react 3h under 40 DEG C of conditions; End capped polyether product is obtained through aftertreatment removing impurity such as underpressure distillation filtrations after reaction terminates.The polymerization degree of described allyl polyethenoxy ether is 25.The mol ratio of described allyl polyethenoxy ether, epoxy chloropropane and sodium hydroxide is 1:1.4:1.3.
(2) preparation of epoxy group(ing) end capped polyether block silicone:
Tetramethyl-dihydro base sily oxide and allyl polyethenoxy glycidyl ether are mixed according to the ratio of 1:2.2, stir, add the catalyzer of 1%, consumption is 20mg/kg, is warming up to 90 DEG C of reaction 4h, and underpressure distillation removing low-boiling-point substance obtains end ring oxygen closure agent.The mol ratio of described hydrogeneous double-seal head and epoxy group(ing) end capped polyether block silicone is 1:2.5.Described catalyzer is isopropyl alcohol solution of chloroplatinic acid.
(3) preparation of polyether/epoxy resin block silicone oil:
Obtained epoxy group(ing) end capped polyether block silicone, octamethylcyclotetrasiloxane and solvent is even, stir after being warmed up to certain temperature, add a certain amount of alkaline catalysts, continue to be warming up to 110 DEG C, insulation reaction 5h; Decompression removing low-boiling-point substance again, obtained polyethers/happy looks or appearance block silicone oil.The mol ratio of described epoxy group(ing) end capped polyether block silicone, octamethylcyclotetrasiloxane is 1:20.Described catalyzer is Tetramethylammonium hydroxide, and catalyst levels is 0.055%.
(4) the organosilyl preparation of the amino block of hyperbranched polyether:
Homemade polyether/epoxy resin block silicone oil, diethylenetriamine are added with nitrogen charging device according to a certain percentage, in three mouthfuls of reactors of reflux condensing tube, add solvent Virahol, consumption is 30% of reaction-ure mixture, 80 DEG C are warmed up to after stirring, after insulation reaction 5h, underpressure distillation, except desolventizing, obtains the amino block polysiloxane of light yellow transparent liquid hyperbranched polyether.Described solvent is Virahol, and solvent load is 32% of reaction mass quality.The mol ratio of described polyether/epoxy resin block silicone oil and diethylenetriamine is 2:1.
Specific embodiment 3:
The organosilyl preparation method of a kind of hyperbranched terpolymer, comprises the steps:
(1) preparation of allyl polyethenoxy glycidyl ether:
Allyl polyethenoxy ether and epoxy chloropropane are mixed, employing sodium hydride is catalyzer, under 60 DEG C of conditions, react 2h, and then unnecessary epoxy chloropropane is sloughed in decompression; Drip a certain amount of aqueous sodium hydroxide solution to reaction system again, control temperature of reaction and react 2h under 35 DEG C of conditions; End capped polyether product is obtained through aftertreatment removing impurity such as underpressure distillation filtrations after reaction terminates.The polymerization degree of described allyl polyethenoxy ether is 23.The mol ratio of described allyl polyethenoxy ether, epoxy chloropropane and sodium hydroxide is 1:1.4:1.3.
(2) preparation of epoxy group(ing) end capped polyether block silicone:
Tetramethyl-dihydro base sily oxide and allyl polyethenoxy glycidyl ether are mixed according to the ratio of 1:2.2, stir, add the catalyzer of 1%, consumption is 20mg/kg, be warming up to 85 DEG C of reaction 3.5h, underpressure distillation removing low-boiling-point substance obtains end ring oxygen closure agent.The mol ratio of described hydrogeneous double-seal head and epoxy group(ing) end capped polyether block silicone is 1:2.2.Described catalyzer is isopropyl alcohol solution of chloroplatinic acid.
(3) preparation of polyether/epoxy resin block silicone oil:
Obtained epoxy group(ing) end capped polyether block silicone, octamethylcyclotetrasiloxane and solvent is even, stir after being warmed up to certain temperature, add a certain amount of alkaline catalysts, continue to be warming up to 105 DEG C, insulation reaction 4.5h; Decompression removing low-boiling-point substance again, obtained polyethers/happy looks or appearance block silicone oil.The mol ratio of described epoxy group(ing) end capped polyether block silicone, octamethylcyclotetrasiloxane is 1:18.Described catalyzer is Tetramethylammonium hydroxide, and catalyst levels is 0.045%.
(4) the organosilyl preparation of the amino block of hyperbranched polyether:
Homemade polyether/epoxy resin block silicone oil, diethylenetriamine are added with nitrogen charging device according to a certain percentage, in three mouthfuls of reactors of reflux condensing tube, add solvent Virahol, consumption is 30% of reaction-ure mixture, 80 DEG C are warmed up to after stirring, after insulation reaction 5h, underpressure distillation, except desolventizing, obtains the amino block polysiloxane of light yellow transparent liquid hyperbranched polyether.Described solvent is Virahol, and solvent load is 30% of reaction mass quality.The mol ratio of described polyether/epoxy resin block silicone oil and diethylenetriamine is 1.8:1.
Table 1 is the performance of different polysiloxane emulsion below, as can be seen from table 1 we: product formation self-emulsifying, do not need to add emulsifying agent in addition, then need for the amino-modified silicone oil that existing market consumption is maximum the emulsifying agents such as use 1305,1307 to be made on emulsion ability finish fabric, but there is improper use breakdown of emulsion problem.
The performance of the different polysiloxane emulsion of table 1
The performance of table 2 different amino modified polysiloxane emulsion finish fabric
Table 2 is the performance of different amino modified polysiloxane emulsion finish fabric, and wherein, fabric is: 300D × 300D polyester filament, door width 160cm, grammes per square metre 74g/m2, black fabric.From table, we can find out that product is all significantly improved to wet colour fastness and sublimation fastness, the stronger bonding force of finishing composition and formation of fabrics is described, product softness, elasticity, moisture absorption good heat dispersion performance, after process, the moisture absorption thermal diffusivity of fabric depends on the continuity of product epithelium and the wetting ability of product itself.Wherein, finishing technique flow process is: two leachings two roll → and preliminary drying → bake → sample.
Claims (9)
1. the organosilyl preparation method of hyperbranched terpolymer, is characterized in that: comprise the steps:
(1) preparation of allyl polyethenoxy glycidyl ether:
Allyl polyethenoxy ether and epoxy chloropropane are mixed, employing sodium hydride is catalyzer, under 55-65 DEG C of condition, react 1.5-2.5h, and then unnecessary epoxy chloropropane is sloughed in decompression; Drip a certain amount of aqueous sodium hydroxide solution to reaction system again, control temperature of reaction and react 1.5-3h under 30-40 DEG C of condition; End capped polyether product is obtained through aftertreatment removing impurity such as underpressure distillation filtrations after reaction terminates;
Concrete reaction formula is as follows:
(2) preparation of epoxy group(ing) end capped polyether block silicone:
Tetramethyl-dihydro base sily oxide and allyl polyethenoxy glycidyl ether are mixed according to the ratio of 1:2.2, stir, add the catalyzer of 1%, consumption is 20mg/kg, be warming up to 80 DEG C ~ 90 DEG C reaction 3 ~ 4h, underpressure distillation removing low-boiling-point substance obtains end ring oxygen closure agent;
Concrete reaction formula is as follows:
(3) preparation of polyether/epoxy resin block silicone oil:
Obtained epoxy group(ing) end capped polyether block silicone, octamethylcyclotetrasiloxane and solvent is even, stir after being warmed up to certain temperature, add a certain amount of alkaline catalysts, continue to be warming up to 100 DEG C ~ 110 DEG C, insulation reaction 4 ~ 5h; Decompression removing low-boiling-point substance again, obtained polyethers/happy looks or appearance block silicone oil;
Concrete reaction formula is as follows:
(4) the organosilyl preparation of the amino block of hyperbranched polyether:
Homemade polyether/epoxy resin block silicone oil, diethylenetriamine are added with nitrogen charging device according to a certain percentage, in three mouthfuls of reactors of reflux condensing tube, add solvent Virahol, consumption is 30% of reaction-ure mixture, 80 DEG C are warmed up to after stirring, after insulation reaction 5h, underpressure distillation, except desolventizing, obtains the amino block polysiloxane of light yellow transparent liquid hyperbranched polyether;
Concrete reaction formula is as follows:
A is
2. the organosilyl preparation method of hyperbranched terpolymer according to claim 1, is characterized in that: described step 1) in the polymerization degree of allyl polyethenoxy ether be 19 ~ 25.
3. the organosilyl preparation method of hyperbranched terpolymer according to claim 1, is characterized in that: described step 1) in the mol ratio of allyl polyethenoxy ether, epoxy chloropropane and sodium hydroxide be 1:1.4:1.3.
4. the organosilyl preparation method of hyperbranched terpolymer according to claim 1, is characterized in that: described step 2) in hydrogeneous double-seal head and the mol ratio of epoxy group(ing) end capped polyether block silicone be 1:2 ~ 2.5.
5. the organosilyl preparation method of hyperbranched terpolymer according to claim 1, is characterized in that: described step 2) in catalyzer be isopropyl alcohol solution of chloroplatinic acid.
6. the organosilyl preparation method of hyperbranched terpolymer according to claim 1, is characterized in that: described step 3) in epoxy group(ing) end capped polyether block silicone, octamethylcyclotetrasiloxane mol ratio be 1:15 ~ 20.
7. the organosilyl preparation method of hyperbranched terpolymer according to claim 1, is characterized in that: described step 3) in catalyzer be Tetramethylammonium hydroxide, catalyst levels is 0.035% ~ 0.055%.
8. the organosilyl preparation method of hyperbranched terpolymer according to claim 1, is characterized in that: described step 3) and 4) in solvent be Virahol, solvent load is the 26%-32% of reaction mass quality.
9. the organosilyl preparation method of hyperbranched terpolymer according to claim 1, is characterized in that: described step 4) in polyether/epoxy resin block silicone oil and the mol ratio of diethylenetriamine be 1.5 ~ 2:1.
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