CN102167789B - Preparation method of polyurethane aqueous dispersion and device thereof - Google Patents
Preparation method of polyurethane aqueous dispersion and device thereof Download PDFInfo
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- CN102167789B CN102167789B CN2010106248267A CN201010624826A CN102167789B CN 102167789 B CN102167789 B CN 102167789B CN 2010106248267 A CN2010106248267 A CN 2010106248267A CN 201010624826 A CN201010624826 A CN 201010624826A CN 102167789 B CN102167789 B CN 102167789B
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Abstract
The invention discloses a preparation method of polyurethane aqueous dispersion and a device thereof. The preparation method comprises the following steps: polyurethane prepolymer with stabilizer, water and triethylamine solution are respectively sent in a polyurethane emulsifier 4 from the bottom by a metering pump, strong stirring is performed at 50-60 DEG C in 2000-3000rpm, the mixture is sent in a chain-extending kettle from the top of the emulsifier 4, a defined amount of triethylamine solution is added, stirring is performed at the room temperature for 0.5-1h, and the product is placed in a container to be used by the user. The prepared polyurethane aqueous dispersion has the following quality indexes: the particle diameter is 45-75nm, the solid content is 30-42%, the pH value is 7.0-7.5, and the viscosity is 10-30mPa.S at 25 DEG C.
Description
One, technical field
The present invention relates to a kind of preparation method and device thereof of polyurethane aqueous dispersion.
Two, background technology
Polyurethane aqueous dispersion can be used for fields such as coating, tackiness agent, surface treatment agent, building materials.The high density polyurethane aqueous dispersion can be used the coating of various base materials.For example, be used as the paint film of timber, metal, plastics, paper, leather, textiles, felt, glass etc.So that its research and development are in the ascendant.
Polyurethane aqueous dispersion roughly is divided into three types of aqueous dispersions such as forced emulsification type, water-soluble sexual type and self-emulsifying type.
Forced emulsification type polyurethane aqueous dispersions is exactly through adding after emulsifying agent (tensio-active agent) carries out water-dispersion to the urethane resin of solution polymerization; Behind the diamines chain extension; Removing desolvates makes the performed polymer forced emulsification, thereby obtains the polyurethane aqueous dispersion of emulsified state.Its shortcoming is that the polyurethane particles diameter is big in the polyurethane aqueous dispersion, dispersion liquid storage tank poor stability, and cementability reduces.
Water-soluble type polyurethane aqueous dispersions just is to use the water soluble polyether polyvalent alcohol and can prepares the polyurethane aqueous dispersion of aqueous solution state with isocyanate reaction.But, the poor water resistance of this aqueous dispersions goods after crosslinking reaction, can be used for some special occasions.
The self-emulsifying type polyurethane aqueous dispersion imports ionic group exactly and makes urethane resin need not to add emulsifying agent in urethane resin or the base polyurethane prepolymer for use as structure just to form aqueous dispersions.The water-dispersion of self-emulsifying type urethane and other two kinds of aqueous dispersions compare, and its particle dia is little, and storage stability is high, and the molecular designing amplitude is wide, and is better than other two kinds of aqueous dispersions.
The self-emulsifying type polyurethane aqueous dispersion also interosculates with other two kinds of aqueous dispersions, carries out the intermittent type manufacturing with the reaction kettle that is equipped with agitating vane usually.Promptly in reaction kettle by isocyanic ester and polyol reaction; Add the dimethylol propionic acid give hydrophilic group and wetting ability solubility promoter again and react and prepare base polyurethane prepolymer for use as, these solubility promoters are like acetone, butanone, glycol ether and N-Methyl pyrrolidone etc.After water-dispersion and through diamines, come further chain extension then, obtain the urethane of water-dispersion.Sometimes the purposes with goods is different, and lower boiling solubility promoter can be removed with the distillatory method; Sometimes then keep high boiling solubility promoter, omit distillation process.
In the intermittent type ME of self-emulsifying type polyurethane aqueous dispersion, be divided into three main phase such as performed polymer preparation, performed polymer water-dispersion and dispersion liquid chain extension.Performed polymer must add salt forming agents such as triethylamine before getting into water-dispersion.Triethylamine be salt forming agent also be the catalyzer of polyurethane reaction, make to contain-viscosity of NCO group performed polymer sharply rises, must in certain hour (as 60 minutes), use up, otherwise can't emulsification, influence the quality of emulsion; When production contained the performed polymer of TDI, situation can be more serious, even the situation of serious blocking pipe can take place, the production-scale expansion of said circumstances restriction interrupter method, the emulsion that relatively more suitable batch production is 1000 kilograms.
The emulsifying stage of interrupter method production is in the chain extending reaction still of the band stirring of band emulsifier unit, to carry out; The phenomenon that viscosity rises can take place when producing inversion of phases in interrupter method; The water-dispersion processing power is mixed with the performed polymer amount of putting into, reaction kettle; Stirring capacity and different and since stir insufficient and goods particle disperse inhomogeneous, the bad dispersibility of goods; A small amount of performed polymer can stick to reaction kettle inwall and bottom after the polymerization, so each processing finishes all to get the cleaning reaction still once; Carry out a series of processing with a reaction kettle; Big production is restricted, for example, makes 1 ton of goods polyurethane aqueous dispersion and will spend 1～2 day time.
In the dispersion liquid chain extension stage, select for use the mode of dropping above the dispersion liquid liquid level, to add chainextender quadrol (normally 20% the aqueous solution) usually.Based on quadrol and performed polymer terminal-the NCO radical reaction is rapid reaction; Make chain extending reaction evenly must drip two amine aqueous solutions lentamente; If because the stirring shear ability at liquid level place is poor, if adding speed causes the quadrol of local emulsion excessive too soon easily, formed polyurethane molecular amount is low; Degradation forms the terminal polyaminoester emulsion of primary amine; The deficiency that causes other a part of emulsion quadrol amount simultaneously forms the terminal emulsion of NCO, finishes back emulsion of different nature together in reaction, and nature can reduce the stability in storage of dispersion liquid, the usability of goods and the glossiness after the goods film forming.The batch production mode will obtain the emulsion of good chain extension, must fully prolong the dropping time.When industrial scale enlarged, increase consuming time was just obvious especially.
In view of the shortcoming of interrupter method production polyurethane aqueous dispersion length consuming time, develop the method for continuous production polyurethane aqueous dispersion gradually.Prior art US7,345,110B2; Mar, 18,2008 disclose the process of continuous production aqueous polyurethane; At first in proportion with base polyurethane prepolymer for use as and water; Be provided with a spray orifice in by T type nozzle in 80 ℃, this injection diameter 2mm is ejected into performed polymer in the water with 0.2～50 bar pressure difference and produces pre-emulsion through mixing section, then through 6 injection dispersers; Be provided with two apertures in each injector; Nine bore dia 0.8mm become emulsion with pressure difference 17 crust homogenizing milk sap, continue it; Temperature of charge be cooled to 29 ℃ put into Glass Containers with quadrol and Hydrazine Hydrate 80 chain extension, filter and obtain polyurethane aqueous dispersion; Its quality index is: mean ionic diameter 50nm, pH=8.0, solid content 38.6%.This method is with T type nozzle emulsification base polyurethane prepolymer for use as, and the device structure complicacy is difficult to cleaning, and used pressure is bigger.Must add and give improvement.
Prior art JP2009-286892A; 2009.12.10 disclose the method for manufacture and the device thereof of polyurethane aqueous dispersion, these method characteristics be with base polyurethane prepolymer for use as and water in the continuous decollator of CAVTRON CD1010, this decollator starting current is 26A; Rotating speed 11,200min
-1Disperse continuously in 64 ℃, the dispersion liquid that continues gets into storage tank, and according to circumstances dispersion liquid can all or part ofly be circulated among the CAVTRON CD1010 and base polyurethane prepolymer for use as redispersion together; To polyurethane concentration be 40～50 quality %; Just calculate and process polyurethane aqueous dispersion, the polyurethane aqueous dispersion quality index is: solid content 33.2～42.5%, average particle diameter 64～104nm; 63～65mPa.s during 25 ℃ of viscosity; The branch that this method is used spreads that the device power consumption is big, and dispersion liquid circulation dispersion results particle dia is inhomogeneous, and promptly the particle homogenization degree is poor.This method need add give improve perfect.It is thin to be necessary to prepare granularity, and the polyurethane dispersing liquid of assignment stability falls well in the look that is evenly distributed.Be necessary to provide method of manufacture simple, emulsifying device is uncomplicated, and the process of processing ease has been the thing of enjoying popular confidence.
Three, summary of the invention
Prepare the performed polymer poor stability that self-emulsifying waterborne polyurethane dispersion liquid exists based on existing interrupter method, can supply emulsification times limited, enlarge the limited day by day characteristics that obviously prolong with the chainextender time of emulsifying capacity with scale.Present inventors are through concentrating on studies; Taken into full account the characteristics and the mutual relationship of stability, emulsifying capacity and chain extending reaction,, provide method of manufacture simple from the polymerization engineering viewpoint; Emulsifying device is uncomplicated, the preparation facilities of the semi-continuous polyurethane aqueous dispersion liquid of processing ease.Preparation polyurethane aqueous dispersion particle dia is little, is evenly distributed, and is coloury, the polyurethane aqueous dispersion of stable storing.Through particular study complete technical scheme has been proposed.
The preparation process of polyurethane aqueous dispersion comprises base polyurethane prepolymer for use as water-dispersion emulsion preparation and polyurethane aqueous dispersion preparation; Described base polyurethane prepolymer for use as comprises aromatic diisocyanate that uses tolylene diisocyanate (TDI) etc. and/or the prepared performed polymer of aliphatic diisocyanate that comprises isophorone diisocyanate (IPDI).Idiographic flow is: the base polyurethane prepolymer for use as that has carboxyl that 50～60 ℃ 100 weight parts contain stablizer is transported to the emulsor through volume pump from storage tank; Meanwhile 60～95 weight parts waters are also carried the low pressure emulsor from storage tank through volume pump respectively from 90～105 parts of 5～6 weight % salt forming agent triethylamine aqueous solutions of storage tank and performed polymer carboxyl equivalent.Because triethylamine and performed polymer separated before emulsification, also added stablizer in the performed polymer simultaneously, the viscosity of performed polymer is very stable, does not also have the restriction of emulsification times, can guarantee the homogeneity of dispersion liquid particle
Needle-like whisking appliance with 2000～3000 rev/mins of rotating speeds in emulsor is implemented powerful stirring and emulsifying in 50～60 ℃; Constantly flowing into polyurethane aqueous dispersion through low-voltage high speed emulsive performed polymer dispersion liquid prepares in the still; Polyurethane aqueous dispersion prepares still and is equipped with inclined paddle type agitator, and PM stirs 150～170 to be changeed; After the whole emulsifications of performed polymer; Be the basis with 100 weight part base polyurethane prepolymer for use as; The aqueous solution 10～12 weight parts that from storage tank, add 20 weight % chainextender quadrols with semicontinuous form, the reinforced back that finishes continues to stir 0.5～1 hour in room temperature, puts into storage tank then; The device of preparation polyurethane aqueous dispersion comprises: base polyurethane prepolymer for use as storage tank, storage tank are equipped with anchor stirrer, water storage tank, base polyurethane prepolymer for use as emulsor; This still is equipped with pin type whisking appliance, salt forming agent triethylamine solution storage tank, polyurethane aqueous dispersion and prepares still; This still is equipped with liquid pushing tube and polyurethane aqueous dispersion storage tank and performed polymer supply line, water supply line, triethylamine supply line, base polyurethane prepolymer for use as emulsion supply line and the polyurethane aqueous dispersion product line of inclined paddle type agitator and chainextender ethylenediamine solution storage tank, and first volume pump, second volume pump, the 3rd volume pump and chainextender ingress pipe.
The base polyurethane prepolymer for use as that contains stablizer, stablizer are from trichoroacetic acid(TCA), aceticanhydride, Phenylsulfonic acid acyl chlorides, to choose any one kind of them; The add-on of stablizer is 0.5%～0.03% of a base polyurethane prepolymer for use as weight.It is stable for a long time for performed polymer adding stablizer, in production period band dispersive performed polymer viscosity obvious variation does not take place.The liquid pushing tube of chainextender quadrol storage tank extends to the terminal outer rim of agitating vane place; Like this; The ethylenediamine solution that adds can THE ADIABATIC SHEAR IN and disperse; Stir through oblique oar simultaneously and be assigned to the entire reaction still rapidly, when guaranteeing the chain extension quality, shortened the required time of chain extending reaction greatly, improve the efficient of chain extending reaction and the homogeneity of dispersion-s.
According to the polyurethane aqueous dispersion that the present invention implements to prepare, its performance index are: particle dia 50～75nm, and solid content 40～100nm, pH 7.0～7.5, viscosity (25 ℃): 10-30mPa.s.
Four, description of drawings
Fig. 1 is a kind of schematic flow sheet of polyurethane aqueous dispersion preparation
Numeral number is explained as follows:
1, base polyurethane prepolymer for use as basin, 2, the water basin, 3, the triethylamine basin, 4, the base polyurethane prepolymer for use as emulsor; 5 pin type whisking appliances, 6, the quadrol basin, 7, polyurethane aqueous dispersion prepares still, 8, propeller stirrer; 9, polyurethane aqueous dispersion basin, 10, anchor stirrer, 11, the ethylenediamine solution supply line, 12, the base polyurethane prepolymer for use as supply line; 13, water supply line, 14 triethylamine supply lines, 15, base polyurethane prepolymer for use as emulsion supply line, 16, the polyurethane aqueous dispersion product line; 17, first volume pump, 18, second volume pump, the 19, the 3rd volume pump, 20, the chainextender liquid-inlet pipe.
Five, embodiment
For embodiment of the present invention spy better illustrates it, but not limitation of the present invention.
The base polyurethane prepolymer for use as preparation
The preparation of a type polyurethane performed polymer
40g polyneopentyl glycol adipate, 60g PTMG, 383g tolylene diisocyanate and 0.04g dibutyl tin laurate obtained performed polymer in 1 hour in 60～78 ℃ of reactions.Adding 12g dimethylol propionic acid that continues and 15g solubility promoter N-Methyl pyrrolidone, and 0.4g Phenylsulfonic acid acyl chlorides continues reaction 2 hours in 68 ℃, makes to be called a type polyurethane performed polymer.
The preparation of b type polyurethane performed polymer
Except that replacing the 383g tolylene diisocyanate with the 489g isophorone diisocyanate and adding the 1.0g trichoroacetic acid(TCA) replaces outside the 0.4g Phenylsulfonic acid acyl chlorides, other prescriptions are the same with the preparation of a type polyurethane performed polymer with operation steps.
Embodiment 1
A type polyurethane performed polymer is sent into base polyurethane prepolymer for use as emulsor 4 bottoms by first volume pump 17 from basin with 10Kg/min speed; Meanwhile water is sent into base polyurethane prepolymer for use as emulsor 4 emulsification from basin 3 by the 3rd volume pump 19 with 10.2Kg/min speed by the triethylamine aqueous solution of second volume pump 18 and 5 weight % from basin 2 with 9.4Kg/min speed; Stir lasting emulsification 65 minutes with 2000～3000 rev/mins of speed; The emulsification material is constantly sent into polyurethane aqueous dispersion from emulsor 4 tops and is prepared the still 7; Inclined paddle type agitator 8 stirs with 160～170 rev/mins of speed, then, is the basis with the 651.9Kg base polyurethane prepolymer for use as; From storage tank 6, be metered into behind the 20 weight % ethylenediamine solution 180Kg in stirring at room 0.5hr, put into storage tank 9 then and supply users to use.This polyurethane aqueous dispersion particle dia 55nm, solid content 35%, pH7.0,25 ℃ of 10～30mPa.S of viscosity.
Embodiment 2
Remove b type polyurethane performed polymer 13.1Kg/min, water 9.37Kg/min, triethylamine 12.3Kg/min speed adds urethane emulsor 4; 50 ℃ of lasting emulsify at a high speed 60 minutes are the basis with the 787Kg base polyurethane prepolymer for use as, and the performed polymer dispersion liquid carries out chain extending reaction after adding the 81.9Kg ethylenediamine solution; Other operation prescriptions are the same with embodiment 1, particle dia 45nm as a result, solid content 42%; PH7.5,25 ℃ of viscosity, 30mPa.S.
Claims (4)
1. the preparation method of a polyurethane aqueous dispersion is characterised in that the preparation process of polyurethane aqueous dispersion comprises base polyurethane prepolymer for use as water-dispersion emulsion preparation and polyurethane aqueous dispersion preparation; Idiographic flow is: 50～60 ℃ 100 weight parts have the base polyurethane prepolymer for use as that has carboxyl of stablizer to be transported to the emulsor (4) of 10L through first volume pump (17) from base polyurethane prepolymer for use as storage tank (1); 5～6 weight % salt forming agent triethylamine aqueous solutions, 90～105 weight parts of 60～95 weight parts waters and performed polymer carboxyl equivalent meanwhile; Be transported to the emulsor (4) from water storage tank (2) and salt forming agent triethylamine aqueous solution storage tank (3) through second volume pump (18) and the 3rd volume pump (19) respectively; In emulsor (4), have with the needle-like whisking appliance of 2000～3000 rev/mins of rotating speeds and implement powerful stirring and emulsifying in 50～60 ℃; Constantly flowing into polyurethane aqueous dispersion through low-voltage high speed emulsive performed polymer dispersion liquid prepares in the still (7); Polyurethane aqueous dispersion prepares still (7) and is equipped with inclined paddle type agitator, and PM stirs 150～170 to be changeed; After the whole emulsifications of performed polymer; Be the basis with 100 weight part base polyurethane prepolymer for use as; The aqueous solution 10～12 weight parts that from chainextender ethylenediamine solution storage tank (6), add 20 weight % chainextender quadrols with semicontinuous form; The reinforced back that finishes continues to stir 0.5～1 hour in room temperature, puts into polyurethane aqueous dispersion storage tank (9) then.
2. the preparation facilities of a polyurethane aqueous dispersion, comprising: base polyurethane prepolymer for use as storage tank (1), storage tank are equipped with anchor stirrer (10), water storage tank (2), base polyurethane prepolymer for use as emulsor (4); This emulsor has pin type whisking appliance (5), salt forming agent triethylamine aqueous solution storage tank (3), polyurethane aqueous dispersion to prepare still (7), and this still is equipped with liquid pushing tube (11) and polyurethane aqueous dispersion storage tank (9) and performed polymer supply line (12), water supply line (13), triethylamine supply line (14), base polyurethane prepolymer for use as emulsion supply line (15) and polyurethane aqueous dispersion product line (16), first volume pump (17), second volume pump (18) and the 3rd volume pump (19) of paddle stirrer (8) and chainextender ethylenediamine solution storage tank (6).
3. according to the preparation method of a kind of polyurethane aqueous dispersion of claim 1, be characterised in that the described base polyurethane prepolymer for use as that contains stablizer, stablizer is from trichoroacetic acid(TCA), aceticanhydride, Phenylsulfonic acid acyl chlorides, to choose any one kind of them; The add-on of stablizer is 0.5%～0.03% of a base polyurethane prepolymer for use as weight.
4. according to the preparation method of a kind of polyurethane aqueous dispersion of claim 1; The liquid pushing tube (11) that is characterised in that described chainextender quadrol storage tank (6) extends to agitating vane and does not hold the outer rim place; Participate in chain extending reaction in the whole still so that the chainextender quadrol can be distributed at short notice, improve the efficient of reaction and the homogeneity of dispersion-s.
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| US10752727B1 (en) * | 2015-07-10 | 2020-08-25 | Covestro Deutschland Ag | Process and apparatus for continuous production of aqueous polyurethane dispersions |
| CN108236893B (en) * | 2016-12-23 | 2020-03-10 | 中国石油天然气股份有限公司 | System and method for synthesizing dicumyl peroxide |
| CN106582451A (en) * | 2016-12-30 | 2017-04-26 | 哈尔滨天顺化工科技开发有限公司 | Continuous feeding system for polymerization of carbon fiber precursors |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5037864A (en) * | 1989-07-11 | 1991-08-06 | The Dow Chemical Company | Semi-continuous process for the preparation of polyurethane-urea aqueous dispersions |
| CN1502640A (en) * | 2002-11-20 | 2004-06-09 | F.C.I.株式会社 | Thermoplastic polyurethane, method and apparatus for producing same |
| CN201148408Y (en) * | 2007-12-21 | 2008-11-12 | 山东圣光化工集团有限公司 | Multi-kettle continuous production apparatus for waterborne polyurethane polymerization reaction |
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| JP5225901B2 (en) * | 2009-03-17 | 2013-07-03 | 三井化学株式会社 | Method for producing aqueous polyurethane resin, aqueous polyurethane resin and film |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5037864A (en) * | 1989-07-11 | 1991-08-06 | The Dow Chemical Company | Semi-continuous process for the preparation of polyurethane-urea aqueous dispersions |
| CN1502640A (en) * | 2002-11-20 | 2004-06-09 | F.C.I.株式会社 | Thermoplastic polyurethane, method and apparatus for producing same |
| CN201148408Y (en) * | 2007-12-21 | 2008-11-12 | 山东圣光化工集团有限公司 | Multi-kettle continuous production apparatus for waterborne polyurethane polymerization reaction |
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| JP特开2010-215803A 2010.09.30 |
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