CN104650363B - 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, and in particular to a kind of preparation method of hyperbranched ternary polymerization organosilicon.
Background technology
At present, amido silicon oil becomes the quite varied post-finishing agent of dyeing application with its excellent softness, flatness,
Fabric Jing after its arrangement has soft, smooth, washable and comfortable and easy to wear performance.But amido silicon oil is in the arrangement mode of fiber
Hydrophilic Fiber is made to be deteriorated, fabric moisture and snugness of fit decline；White or light coloured fabrics after being arranged with it, in high temperature
After baking, it may appear that different degrees of xanthochromia and aberration；And its stability of emulsion is poor, easily occur in storage and transportation
" floating oil breakdown of emulsion " phenomenon.
At present, the latest development of weaving organic silicone finishing agent is that linear polyether block amino ternary polymerization silicone is soft
Agent, be a class use it is widely applicable, in water have automatic emulsifying performance, the fabric organic silicone finishing agent of good emulsion stability, Jing
Its fabric after arranging has good flexibility, hydrophilic, antistatic behaviour and the not performance of complexion changed.Also there are some performances at present
Relatively good silicone softening agent, such as publication date be on October 5th, 2011, the Chinese patent of Publication No. CN102206921A
In, patent discloses a kind of preparation method of polyether block amino silicone soft finishing agent, and the preparation method is comprised the following steps：
A, diisocyanate, polyether Glycols and hydroxy silicon oil are adopted for raw material, prepare the polyether block organosilicon with-OH end groups and gather
Urethane；B, with-OH end groups polyether block organic silicon polyurethane as primary raw material, carry out chain extending reaction with silane coupler
Afterwards, add acid neutralization, moisture dissipate obtain polyether block amino silicone soft finishing agent.And for example publication date is August 1 in 2012
Day, in the Chinese patent of Publication No. CN102617863A, patent discloses a kind of system of hydrophilic block polyether aminosilicone
Preparation Method, the preparation method are mainly included the following steps that：A, preparation end containing hydrogen silicone oil intermediate, adopt cyclosiloxane for main former
Material, carries out block reaction with hydrogeneous double-seal head, generates end containing hydrogen silicone oil intermediate；B, preparation end epoxy silicon oil intermediate, by end
Containing hydrogen silicone oil carries out additive reaction with pi-allyl epoxidized polyether, generates end epoxy silicon oil；The preparation of C, finished product, using end ring oxygen silicon
Oil carries out ammonolysis ring-opening reaction with polyetheramine, and hydrophilic block polyether aminosilicone is obtained.The product of both the above preparation method
Linear polyether block amido silicon oil is belonged to, and by the polyether segment for macromolecule being introduced on silicone backbone, is improve whole
The hydrophilic of fabric after reason, and improve state of the product in water, product emulsion stability is improve, is introduced on macromolecular chain
Mostly be primary amine groups, relatively stable, it is not easy to aoxidize, the fabric after arrangement is nearly free from Yellowing.But as line
Type ternary polymerization organosilicon, introduces the polyether segment of macromolecule on macromolecular main chain, the methyl in silicon-oxygen backbone is smoothed
Layer cut-out, and molecular weight is big not as good as amido silicon oil, so its soft slipping is not so good as amido silicon oil；Additionally, amino block is existed
In main chain, affected by sterically hindered and polarity, fiber surface absorption not as good as amido silicon oil, so its washability is relatively
Difference.
In sum, a kind of hydrophilic for having tri-block silicone oil concurrently, stability of emulsion and amido silicon oil be there is presently no
The preparation method of the silicone softening agent of soft slipping.
The content of the invention
Goal of the invention：The present invention provides a kind of preparation method of hyperbranched ternary polymerization organosilicon, the over-expense compound of synthesis
With network structure, cohesive force that can not only be between reinforcing fiber, moreover it is possible to strengthen the cohesive force between yarn.
Technical scheme：A kind of preparation method of hyperbranched ternary polymerization organosilicon, comprises the steps：
(1) preparation of allyl polyethenoxy glycidyl ether：
By allyl polyethenoxy ether and epoxychloropropane mix homogeneously, sodium hydride is adopted for catalyst, in 55-65 DEG C of bar
1.5-2.5h is reacted under part, unnecessary epoxychloropropane is sloughed in then decompression；Again to a certain amount of hydroxide of reaction system Deca
Sodium water solution, controlling reaction temperature react 1.5-3h under the conditions of 30-40 DEG C；Reaction terminate after after the distillating filtering etc. of reducing pressure
Process removing impurity and obtain end capped polyether product；
Concrete reaction equation is as follows：
(2) preparation of epoxy radicals end-blocking polyether block siloxanes：
By two hydrogen-based disiloxane of tetramethyl and allyl polyethenoxy glycidyl ether according to 1:2.2 ratio mixing,
Stir, add 1% catalyst, consumption is 20mg/kg, be warming up to 80 DEG C～90 DEG C 3～4h of reaction, vacuum distillation is removed
Low-boiling-point substance obtains end ring oxygen closure agent；
Concrete reaction equation is as follows：
(3) preparation of polyether/epoxy resin block silicone oil：
By obtained epoxy radicals end-blocking polyether block siloxanes, octamethylcy-clotetrasiloxane and solvent mix homogeneously, stir
After being warmed up to uniform temperature, a certain amount of base catalyst is added, 100 DEG C～110 DEG C is continuously heating to, 4～5h of insulation reaction；Subtract again
Pressure removes low-boiling-point substance, and polyethers/happy looks or appearance block silicone oil is obtained；
Concrete reaction equation is as follows：
(4) preparation of hyperbranched polyether amino block organosilicon：
Homemade polyether/epoxy resin block silicone oil, diethylenetriamine are added according to a certain percentage with nitrogen charging device,
In three mouthfuls of reactors of reflux condensing tube, solvent isopropanol, consumption for reaction-ure mixture 30% is added to heat up after stirring
To 80 DEG C, after insulation reaction 5h, vacuum distillation removes solvent, obtains the poly- silicon of light yellow transparent liquid hyperbranched polyether amino block
Oxygen alkane；
Concrete reaction equation is as follows：
A is
As optimization：The step 1) in allyl polyethenoxy ether the degree of polymerization be 19～25.
As optimization：The step 1) in allyl polyethenoxy ether, epoxychloropropane and sodium hydroxide mol ratio
For 1:1.4:1.3.
As optimization：The step 2) in hydrogeneous double-seal head and the mol ratio of epoxy radicals end-blocking polyether block siloxanes be
1:2～2.5.
As optimization：The step 2) in catalyst be isopropyl alcohol solution of chloroplatinic acid.
As optimization：The step 3) in epoxy radicals end-blocking polyether block siloxanes, octamethylcy-clotetrasiloxane rubs
You are than being 1:15～20.
As optimization：The step 3) in catalyst be Tetramethylammonium hydroxide, catalyst amount be 0.035%～
0.055%.
As optimization：The step 3) and 4) in solvent be isopropanol, solvent load is reaction mass quality
26%-32%.
As optimization：The step 4) in polyether/epoxy resin block silicone oil and diethylenetriamine mol ratio be 1.5～2:
1。
Beneficial effect：The concrete advantage of the present invention is as follows：
1st, the present invention dissaving polymer and linear polyether amino block organosilicon are combined be developed into it is new organic
Silicone softener, it possesses new modified organic silicon chemical constitution, and the cohesive force between the over-expense compound energy reinforcing fiber of synthesis is divided
Protonatomic mass is high, and viscosity is low, and hydrophilic radical is more, can give fabric sofetening plentiful and washable feel.Diethylenetriamine increases
Hydrophilic and improve durability and effect.Polyethers be increased in molecule segment, and EO numbers n in polyethers is controlled in 25-
40, polyether group has extremely strong hydrophilic, and hydrophobic organosilicon can be made to be changed into hydrophilic organic silicon, emulsion floating oil is solved
Problem, simplify emulsifying process, and the fabric Jing after organic silicon modified by polyether is arranged also have good soil resistant and anti-quiet
Electrically, after overcoming simple polysiloxanes finish fabric, " moisture absorption absorption of perspiration is low ", " being also easy to produce frictional static " etc. are a series of lacks
Point；Diethylenetriamine is recycled to carry out hyperbranched so that structure easily forms hydrogen bond with water very, can carry out emulsifying without emulsifying agent,
Overcome the problem of the easy floating oil breakdown of emulsion of conventional organic silicone oil softening agent.Simultaneously as the product is hyperbranched network structure, no
It is only capable of the active force such as fiber utilization hydrogen bond in single yarn is coated togather, while the network structure that can also utilize super large will be many
One thread is coated togather, and considerably increases yarn and interfibrous cohesive force.
2nd, when silicone oil is made housekeeping liquid, suitably its pH value is adjusted between 5～6 with glacial acetic acid, acetic acid
Add, the raising of formation and stability to dressing liquid has material impact.This is primarily due to acetic acid can be with amino therein
Reaction generates quaternary ammonium salt, enhances the polarity of silicone oil so as to be readily dispersed in water, forms O/W type emulsions.Hyperbranched polyether ammonia
Base block silicone oil solves the problems, such as the easy breakdown of emulsion of traditional amino-modified silicone oil during storage and use, and product has certainly in water
Emulsifiability, good emulsion stability；Reduce yellowing, enhance hydrophilic, be particularly suitable for the softness of white or light coloured fabrics
Arrange.
3rd, the fabric that this product is sorted out overcomes the shortcoming of common ternary polymerization silicone oil, and its good hydrophilic property is yellowing little,
Combined with chemical bond form with fabric, increased washability, while and the soft effect with amido silicon oil.
Description of the drawings
Fig. 1 is the absorption schematic diagram of the silicone softening agent of the present invention.
Specific embodiment
With reference to specific embodiment, the present invention will be described in detail.
Specific embodiment 1：
A kind of preparation method of hyperbranched ternary polymerization organosilicon, comprises the steps：
(1) preparation of allyl polyethenoxy glycidyl ether：
By allyl polyethenoxy ether and epoxychloropropane mix homogeneously, sodium hydride is adopted for catalyst, in 55 DEG C of conditions
Lower reaction 1.5h, then decompression slough unnecessary epoxychloropropane；It is water-soluble to a certain amount of sodium hydroxide of reaction system Deca again
Liquid, controlling reaction temperature react 1.5h under the conditions of 30 DEG C；Reaction removes roguing through the post processings such as distillating filtering of reducing pressure after terminating
Matter obtains end capped polyether product.The degree of polymerization of the allyl polyethenoxy ether is 19.The allyl polyethenoxy ether, epoxy
The mol ratio of chloropropane and sodium hydroxide is 1:1.4:1.3.
(2) preparation of epoxy radicals end-blocking polyether block siloxanes：
By two hydrogen-based disiloxane of tetramethyl and allyl polyethenoxy glycidyl ether according to 1:2.2 ratio mixing,
Stir, add 1% catalyst, consumption is 20mg/kg, be warming up to 80 DEG C of reaction 3h, vacuum distillation removes low-boiling-point substance and obtains
End ring oxygen closure agent.The mol ratio of the hydrogeneous double-seal head and epoxy radicals end-blocking polyether block siloxanes is 1:2.The catalyst
For isopropyl alcohol solution of chloroplatinic acid.
(3) preparation of polyether/epoxy resin block silicone oil：
By obtained epoxy radicals end-blocking polyether block siloxanes, octamethylcy-clotetrasiloxane and solvent mix homogeneously, stir
After being warmed up to uniform temperature, a certain amount of base catalyst is added, 100 DEG C is continuously heating to, insulation reaction 4h；Low boiling is removed under reduced pressure again
Thing, is obtained polyethers/happy looks or appearance block silicone oil.The epoxy radicals end-blocking polyether block siloxanes, octamethylcy-clotetrasiloxane mole
Than for 1:15.The catalyst is Tetramethylammonium hydroxide, and catalyst amount is 0.035%.
(4) preparation of hyperbranched polyether amino block organosilicon：
Homemade polyether/epoxy resin block silicone oil, diethylenetriamine are added according to a certain percentage with nitrogen charging device,
In three mouthfuls of reactors of reflux condensing tube, solvent isopropanol, consumption for reaction-ure mixture 30% is added to heat up after stirring
To 80 DEG C, after insulation reaction 5h, vacuum distillation removes solvent, obtains the poly- silicon of light yellow transparent liquid hyperbranched polyether amino block
Oxygen alkane.The solvent is isopropanol, solvent load for reaction mass quality 26%.The polyether/epoxy resin block silicone oil and
The mol ratio of diethylenetriamine is 1.5:1.
Specific embodiment 2：
A kind of preparation method of hyperbranched ternary polymerization organosilicon, comprises the steps：
(1) preparation of allyl polyethenoxy glycidyl ether：
By allyl polyethenoxy ether and epoxychloropropane mix homogeneously, sodium hydride is adopted for catalyst, in 65 DEG C of conditions
Lower reaction 2.5h, then decompression slough unnecessary epoxychloropropane；It is water-soluble to a certain amount of sodium hydroxide of reaction system Deca again
Liquid, controlling reaction temperature react 3h under the conditions of 40 DEG C；Reaction removes impurity through the post processings such as distillating filtering of reducing pressure after terminating
Obtain end capped polyether product.The degree of polymerization of the allyl polyethenoxy ether is 25.The allyl polyethenoxy ether, epoxy chlorine
The mol ratio of propane and sodium hydroxide is 1:1.4:1.3.
(2) preparation of epoxy radicals end-blocking polyether block siloxanes：
By two hydrogen-based disiloxane of tetramethyl and allyl polyethenoxy glycidyl ether according to 1:2.2 ratio mixing,
Stir, add 1% catalyst, consumption is 20mg/kg, be warming up to 90 DEG C of reaction 4h, vacuum distillation removes low-boiling-point substance and obtains
End ring oxygen closure agent.The mol ratio of the hydrogeneous double-seal head and epoxy radicals end-blocking polyether block siloxanes is 1:2.5.The catalysis
Agent is isopropyl alcohol solution of chloroplatinic acid.
(3) preparation of polyether/epoxy resin block silicone oil：
By obtained epoxy radicals end-blocking polyether block siloxanes, octamethylcy-clotetrasiloxane and solvent mix homogeneously, stir
After being warmed up to uniform temperature, a certain amount of base catalyst is added, 110 DEG C is continuously heating to, insulation reaction 5h；Low boiling is removed under reduced pressure again
Thing, is obtained polyethers/happy looks or appearance block silicone oil.The epoxy radicals end-blocking polyether block siloxanes, octamethylcy-clotetrasiloxane mole
Than for 1:20.The catalyst is Tetramethylammonium hydroxide, and catalyst amount is 0.055%.
(4) preparation of hyperbranched polyether amino block organosilicon：
Homemade polyether/epoxy resin block silicone oil, diethylenetriamine are added according to a certain percentage with nitrogen charging device,
In three mouthfuls of reactors of reflux condensing tube, solvent isopropanol, consumption for reaction-ure mixture 30% is added to heat up after stirring
To 80 DEG C, after insulation reaction 5h, vacuum distillation removes solvent, obtains the poly- silicon of light yellow transparent liquid hyperbranched polyether amino block
Oxygen alkane.The solvent is isopropanol, solvent load for reaction mass quality 32%.The polyether/epoxy resin block silicone oil and
The mol ratio of diethylenetriamine is 2:1.
Specific embodiment 3：
A kind of preparation method of hyperbranched ternary polymerization organosilicon, comprises the steps：
(1) preparation of allyl polyethenoxy glycidyl ether：
By allyl polyethenoxy ether and epoxychloropropane mix homogeneously, sodium hydride is adopted for catalyst, in 60 DEG C of conditions
Lower reaction 2h, then decompression slough unnecessary epoxychloropropane；Again to a certain amount of sodium hydrate aqueous solution of reaction system Deca,
Controlling reaction temperature reacts 2h under the conditions of 35 DEG C；Reaction removes impurity through the post processings such as distillating filtering of reducing pressure after terminating and obtains
End capped polyether product.The degree of polymerization of the allyl polyethenoxy ether is 23.The allyl polyethenoxy ether, epoxychloropropane
Mol ratio with sodium hydroxide is 1:1.4:1.3.
(2) preparation of epoxy radicals end-blocking polyether block siloxanes：
By two hydrogen-based disiloxane of tetramethyl and allyl polyethenoxy glycidyl ether according to 1:2.2 ratio mixing,
Stir, add 1% catalyst, consumption is 20mg/kg, be warming up to 85 DEG C of reaction 3.5h, vacuum distillation removes low-boiling-point substance
Obtain end ring oxygen closure agent.The mol ratio of the hydrogeneous double-seal head and epoxy radicals end-blocking polyether block siloxanes is 1:2.2.It is described to urge
Agent is isopropyl alcohol solution of chloroplatinic acid.
(3) preparation of polyether/epoxy resin block silicone oil：
By obtained epoxy radicals end-blocking polyether block siloxanes, octamethylcy-clotetrasiloxane and solvent mix homogeneously, stir
After being warmed up to uniform temperature, a certain amount of base catalyst is added, 105 DEG C is continuously heating to, insulation reaction 4.5h；It is removed under reduced pressure again low
Boiling thing, is obtained polyethers/happy looks or appearance block silicone oil.The epoxy radicals end-blocking polyether block siloxanes, octamethylcy-clotetrasiloxane rub
You are than being 1:18.The catalyst is Tetramethylammonium hydroxide, and catalyst amount is 0.045%.
(4) preparation of hyperbranched polyether amino block organosilicon：
Homemade polyether/epoxy resin block silicone oil, diethylenetriamine are added according to a certain percentage with nitrogen charging device,
In three mouthfuls of reactors of reflux condensing tube, solvent isopropanol, consumption for reaction-ure mixture 30% is added to heat up after stirring
To 80 DEG C, after insulation reaction 5h, vacuum distillation removes solvent, obtains the poly- silicon of light yellow transparent liquid hyperbranched polyether amino block
Oxygen alkane.The solvent is isopropanol, solvent load for reaction mass quality 30%.The polyether/epoxy resin block silicone oil and
The mol ratio of diethylenetriamine is 1.8:1.
Table 1 below is the performance of different polysiloxane emulsions, be we can see that from table 1：Product formation self emulsifying, no
Emulsifying agent need to be added in addition, and the amino-modified silicone oil maximum for existing market consumption is then needed using the emulsifyings such as 1305,1307
Agent is made on emulsion ability finish fabric, but there is improper use breakdown of emulsion.
The performance of 1 different polysiloxane emulsions of table
The performance of 2 different amino modified polysiloxane emulsion finish fabrics of table
Performance of the table 2 for different amino modified polysiloxane emulsion finish fabrics, wherein, fabric is：300D × 300D is washed
Synthetic fibre long filament, door width 160cm, grammes per square metre 74g/m2, black fabric.From table, we can see that product to wet colour fastness and distillation
Fastness is significantly improved, and illustrates that finishing agent defines stronger adhesion with fabric, and product is soft, elasticity, moisture absorption thermal diffusivity
Can preferably, after process, the moisture absorption thermal diffusivity of fabric depends on the hydrophilic of the seriality and product itself of product epithelium.Wherein, it is whole
Managing technological process is：Two leachings two roll → and preliminary drying → bake → sample.
Claims (6)
1. a kind of preparation method of hyperbranched ternary polymerization organosilicon, it is characterised in that：Comprise the steps：
(1) preparation of allyl polyethenoxy glycidyl ether：
By allyl polyethenoxy ether and epoxychloropropane mix homogeneously, sodium hydride is adopted for catalyst, under the conditions of 55-65 DEG C
Reaction 1.5-2.5h, then decompression slough unnecessary epoxychloropropane；Again to a certain amount of sodium hydroxide water of reaction system Deca
Solution, controlling reaction temperature react 1.5-3h under the conditions of 30-40 DEG C；Reaction is removed through distillating filtering post processing of reducing pressure after terminating
Decontamination obtains end capped polyether product；
Concrete reaction equation is as follows：
(2) preparation of epoxy radicals end-blocking polyether block siloxanes：
By two hydrogen-based disiloxane of tetramethyl and allyl polyethenoxy glycidyl ether according to 1:2.2 ratio mixing, stirring
Uniformly, 1% catalyst is added, consumption is 20mg/kg, is warming up to 80 DEG C～90 DEG C 3～4h of reaction, vacuum distillation removes low boiling
Thing obtains end ring oxygen closure agent；
Concrete reaction equation is as follows：
(3) preparation of polyether/epoxy resin block silicone oil：
Obtained epoxy radicals end-blocking polyether block siloxanes, octamethylcy-clotetrasiloxane and solvent mix homogeneously, stirring are heated up
To after uniform temperature, a certain amount of base catalyst is added, 100 DEG C～110 DEG C is continuously heating to, 4～5h of insulation reaction；Reduce pressure again and remove
Low-boiling-point substance is removed, polyether/epoxy resin block silicone oil is obtained；
Concrete reaction equation is as follows：
(4) preparation of hyperbranched polyether amino block organosilicon：
Homemade polyether/epoxy resin block silicone oil, diethylenetriamine are added according to a certain percentage with nitrogen charging device, backflow
In three mouthfuls of reactors of condensing tube, solvent isopropanol, consumption is added to be the 30% of reaction-ure mixture, after stirring, be warmed up to 80
DEG C, after insulation reaction 5h, vacuum distillation removes solvent, obtains the poly- silica of light yellow transparent liquid hyperbranched polyether amino block
Alkane；
Concrete reaction equation is as follows：
A is
The step 1) in allyl polyethenoxy ether the degree of polymerization be 19～25；
The step 1) in allyl polyethenoxy ether, epoxychloropropane and sodium hydroxide mol ratio be 1:1.4:1.3；
The step 2) in hydrogeneous double-seal head and epoxy radicals end-blocking polyether block siloxanes mol ratio be 1:2～2.5.
2. the preparation method of hyperbranched ternary polymerization organosilicon according to claim 1, it is characterised in that：The step 2)
In catalyst be isopropyl alcohol solution of chloroplatinic acid.
3. the preparation method of hyperbranched ternary polymerization organosilicon according to claim 1, it is characterised in that：The step 3)
In epoxy radicals end-blocking polyether block siloxanes, octamethylcy-clotetrasiloxane mol ratio be 1:15～20.
4. the preparation method of hyperbranched ternary polymerization organosilicon according to claim 1, it is characterised in that：The step 3)
In catalyst be Tetramethylammonium hydroxide, catalyst amount be 0.035%～0.055%.
5. the preparation method of hyperbranched ternary polymerization organosilicon according to claim 1, it is characterised in that：The step 3)
Isopropanol, 26%-32% of the solvent load for reaction mass quality are with the solvent in 4).
6. the preparation method of hyperbranched ternary polymerization organosilicon according to claim 1, it is characterised in that：The step 4)
In polyether/epoxy resin block silicone oil and diethylenetriamine mol ratio be 1.5～2:1.
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| CN104195836A (en) * | 2014-08-19 | 2014-12-10 | 西安工程大学 | Preparation method of ternary block organic-silicon softening agent |
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