CN103923455A - Micro-porous polyurethane film and preparation method thereof - Google Patents
Micro-porous polyurethane film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a micro-porous polyurethane film and a preparation method thereof. The polyurethane film comprises waterborne polyurethane resin, and 9-15 percent of a bridging agent, 1-2 percent of extinction powder, 0.4-0.6 percent of a flatting agent, 0.4-0.6 percent of a peeling aid, 1-5 percent of a surfactant and 30-50 percent of an organic solvent based on the mass of the waterborne polyurethane resin, and the balance of water. According to the polyurethane film disclosed by the invention, large volatilization difference is caused due to polarity difference of the organic solvent and the water in drying and film formation processes, so that micro-pores are formed during the volatilization from a polyurethane phase; by regulating the ratio of the organic solvent to the water, the ratio of the organic solvent/water to polyurethane and the ratio of the extinction powder to the flatting agent, the sizes of the micro-pores can be controlled, so the polyurethane film has relatively good waterproofness and air permeability.
Description
Technical field
The technical field that the present invention relates to polyurethane film, relates in particular to polyurethane film of a kind of waterproof and breathable and preparation method thereof.
Background technology
Polyurethane film is applied to the preparation of ready-made clothes and fashionable dress more and more in recent years, and the clothes that adopt ventilative thin polyurethane mould material to prepare not only have respiratory function, can also be antistatic; Polyurethane film in sportwear and goods with making the fabrics such as submarine armor, swim suit, rhythm clothing and air Landing clothes, Aerated water bed, ball inner bag, boat, safety buoy and material inside.Shape memory polyurethane film newly developed, there is good crystallinity, block is gathered into microcell and plays physical crosslinking point, controlling the shape of shape memory polyurethane fixes and recovers, the shape memory temperature of these shape memory polyurethanes is decided to be to room temperature, for the production of compound fabric, as home wear facework, below room temperature, can play thermal effect, more than room temperature, can there is good water vapour permeability.It is good that thermoplasticity polyurethane film has soft feel, and intensity is high, windproof ventilative, outstanding features such as environmental protection and be widely used in textile composite fabric, and for Sport & Casual, the fields such as special type protection.The polyurethane film of prior art mostly is the film of hydrophilic, and its water-repellancy is poor, shows as water-swellable, and its ventilation property is also poor in addition.
Summary of the invention
In view of this, one aspect of the present invention provides a kind of microporous polyurethane film, and this polyurethane film has good water-repellancy and ventilation property.
A kind of microporous polyurethane film, comprise waterborne polyurethane resin, in the bridging agent of the quality 9～15% of waterborne polyurethane resin, 1～2% flatting silica, 0.4～0.6% flow agent, 0.4～0.6% help stripping agent, 1～5% tensio-active agent, 30～50% organic solvent, and the water of surplus.
Wherein, comprise waterborne polyurethane resin, in the bridging agent of the quality 13% of waterborne polyurethane resin, 1.5% flatting silica, 0.5% flow agent, 0.5% help stripping agent, 3% tensio-active agent, 40% organic solvent, and the water of surplus.
Wherein, described tensio-active agent is (3/2～2) by quality: 1 anion surfactant and nonionogenic tenside form.
Wherein, described anion surfactant is SDS and/or SDBS; Described nonionogenic tenside is a kind of in OP-10, OP-9, NP-9 and NP-10 or at least separately plants.
Wherein, described bridging agent is aliphatic polymeric isocyanate.
Wherein, described flatting silica is OK-412 flatting silica, and described flow agent is C
1～10alkyl-modified organopolysiloxane, described in help stripping agent be polyether-modified polydimethylsiloxane.
Wherein, described organic solvent organic solvent is comprised of quality 15～25% butanone and 15～25% toluene in waterborne polyurethane resin.
In the feed composition of above polyurethane film, using the mixed solution of organic solvent and water as the good distribution medium of disperse aqueous urethane resin, bridging agent and auxiliary agent.After one in organic solvent and water is scattered in another one, because both are mutual exclusive two-phase, can form the dispersion liquid of water-in-oil or oil-in-water two kinds of different states.In the molecular structure of tensio-active agent, contain hydrophilic radical and lipophilicity group, hydrophilic radical can be inserted in the molecular grouping aggressiveness of organic solvent, hydrophilic radical inserts in water clusters aggressiveness, so just can make oil be scattered in preferably in water or water-dispersion in oil.The add-on of water and organic solvent can take water more than organic solvent or organic solvent more than in water.The present invention is preferably water more than organic solvent.Be understandable that, " surplus " refers to that water add-on will be more than organic solvent, and is enough to make flatting silica, flow agent, stripper and aqueous polyurethane fully to soak or dissolve the effect that it is fully disperseed to reach.The amount that it is concrete, those skilled in the art can obtain by simple practice.
In polyurethane film of the present invention, organic solvent and water are in the process of dry formation film, both polarity differences cause volatility different, thereby can leave micropore in mutually at urethane, by adjusting the proportioning of organic solvent/water ratio between two, organic solvent/water and urethane, can realize the size of micropore is controlled, the specified range by the size control of micropore between the molecule of liquid hydration gaseous state, reaches the effect of waterproof and breathable.
Bridging agent is called again solidifying agent or linking agent, the crosslinked group containing can with polyurethane high molecule chain in avtive spot key and put forward high molecular degree of crosslinking, with the webbed molecular structure of shape.The present invention is preferably aliphatic polymeric isocyanate, and contained NCO group can react with hydroxyl, carboxyl, amino groups on waterborne polyurethane resin molecular chain quickly at normal temperatures and form crosslinking structure, can significantly improve water-base resin performance.
Flatting silica is the glossiness that reduces mould material, makes it reach half light or unglazed effect.OK-412 flatting silica is a kind of white powder, take silicon-dioxide as main component, and composition is up to more than 98%, and its median size is at several microns.It has advantages of that easy dispersion, extinction are good, increase slip, suspension is good.
Flow agent is to impel glue in drying and forming-film process, to form smooth, smooth, a uniform film.C
1～ 10alkyl-modified organopolysiloxane is in macromolecular chain, to contain the polymkeric substance that a class of alkyl contains silicon-oxide structure unit.Alkyl wherein can improve thermostability, consistency and foam stability not, even has their defoaming function.
Help stripping agent to be called again release agent, add that can to impel dry filming to be easy to from coated substrate separated.Polyether-modified polydimethylsiloxane is to adopt ethers oligopolymer and polydimethylsiloxane to carry out condensation reaction to obtain.It had both been dissolvable in water oil type solvent, was dissolvable in water again water.It can anti, increases wear resistance, increases separate-type paper and obtains glossiness, weathering resistance and the vividness that access times can obviously improve coating, and this external enwergy gives leather smooth feel, can effectively improve the dispersiveness of pigment and filler, improves the homogeneity of color; Can be used as the waterproof processing of fabric coating.
The present invention provides a kind of method of preparing above-mentioned polyurethane film on the other hand, and the polyurethane film that the method obtains has good water-repellancy and ventilation property.
Prepare the method as above-mentioned polyurethane film, comprise the following steps:
(1) waterborne polyurethane resin is added to and in water, is thoroughly mixed to form dispersion liquid with the tensio-active agent in the quality 1～5% of waterborne polyurethane resin, 30～50% organic solvent;
(2) waterborne polyurethane resin is thoroughly mixed to form to hybrid resin with the flow agent in the quality 0.4～0.6% of waterborne polyurethane resin, 0.4～0.6% the stripping agent that helps, the bridging agent of the quality in waterborne polyurethane resin 9～15%, 1～2% flatting silica are added in dispersion liquid through being mixed to form mixed solution;
(3) in hybrid resin, add mixed solution, be thoroughly mixed to form glue
(4) glue is inserted and make foaming formation aqueous polyurethane foam in bubble machine;
(5) after aqueous polyurethane foam is coated on coated substrate, coated substrate is dried, obtains polyurethane film.
Wherein, mixed solution described in step (3) successively divides and is added to hybrid resin three times according to 30%, 30% and 40% add-on; Described in step (4), the blowing ratio of foaming is 4～6, and flow is 8～12g/s.
Wherein, described in step (5), dry being specially inserted coated substrate in the baking oven of 60～150 ℃ and passes through baking oven with the speed of 10～20M/min; Described in step (5), the glue spread of coating is 140～180g/m
2, coated substrate is separate-type paper.
In polyurethane film of the present invention, organic solvent and water are in the process of dry formation film, both polarity differences cause volatilization to differ greatly, thereby when volatilizing mutually, urethane can leave micropore, by adjusting the proportioning of the proportioning of organic solvent/water ratio between two, organic solvent/water and urethane and flatting silica, flow agent, flow agent, can realize and make polyurethane film there is good water-repellancy and ventilation property to the size control of micropore.
Embodiment
The present invention is described in further detail in conjunction with the embodiments respectively below.
In below implementing, related each industrial chemicals source place is as follows:
Waterborne polyurethane resin is the DL-1537 that Bayer A.G becomes to produce; Flow agent is white general the produced ZBJ-002 in Tianjin.Helping stripping agent is white general the produced ZBJ-003 in Tianjin; OK-412 organosilicon flatting silica is degussa(Degussa) produced; Bridging agent is commercially available LJ3300.
Embodiment 1: first waterborne polyurethane resin is added to and in water, fully dissolves and be mixed to form dispersion liquid with take tensio-active agent (SDS and the OP-9 that are 3/2:1 by mass ratio form), 15% butanone and 15% toluene of quality 1% of waterborne polyurethane resin.Then, by waterborne polyurethane resin with take the ZBJ-002 of quality 0.4% of waterborne polyurethane resin, be mixed to form hybrid resin under the stirring of stirrer that 0.4% ZBJ-003 is 1000rpm at rotating speed.And, the LJ3300 bridging agent of the quality in waterborne polyurethane resin 9%, 1% OK-412 flatting silica are joined in dispersion liquid under the stirring of the homogenizer of 2500rpm and fully stir and obtain mixed solution.Then, according to 30%, 30% and 40% add-on, divide and three times mixed solution be added in hybrid resin and obtain glue in the stirring of the stirrer of 200rpm.Then, glue is inserted and is made in bubble machine, and the foaming according to the 4 when flow of 8g/s is carried out fully foaming and obtaining aqueous polyurethane foam.Then, aqueous polyurethane foam is coated in separate-type paper, inserted in baking oven, at 60 ℃, with the speed of 10M/min, by baking oven, make to be dried to polyurethane film.Finally, polyurethane film is separated and carry out trimming from separate-type paper, obtain the finished product.
Embodiment 2: first waterborne polyurethane resin is added to and in water, fully dissolves and be mixed to form dispersion liquid with take tensio-active agent (SDS and the NP-9 that are 1.6:1 by mass ratio form), 15% butanone and 20% toluene of quality 2% of waterborne polyurethane resin.Then, by waterborne polyurethane resin with take the ZBJ-002 of quality 0.6% of waterborne polyurethane resin, be mixed to form hybrid resin under the stirring of stirrer that 0.6% ZBJ-003 is 1200rpm at rotating speed.And, the LJ3300 bridging agent of the quality in waterborne polyurethane resin 10%, 2% OK-412 flatting silica are joined in dispersion liquid under the stirring of the homogenizer of 2800rpm and fully stir and obtain mixed solution.Then, according to 30%, 30% and 40% add-on, divide and three times mixed solution be added in hybrid resin and obtain glue in the stirring of the stirrer of 220rpm.Then, glue is inserted and is made in bubble machine, and the foaming according to the 4.5 when flow of 9g/s is carried out fully foaming and obtaining aqueous polyurethane foam.Then, aqueous polyurethane foam is coated in separate-type paper, inserted in baking oven, at 80 ℃, with the speed of 11M/min, by baking oven, make to be dried to polyurethane film.Finally, polyurethane film is separated and carry out trimming from separate-type paper, obtain the finished product.
Embodiment 3: first waterborne polyurethane resin is added to and in water, fully dissolves and be mixed to form dispersion liquid with take tensio-active agent (SDS and the NP-10 that are 1.7:1 by mass ratio form), 15% butanone and 25% toluene of quality 3% of waterborne polyurethane resin.Then, by waterborne polyurethane resin with take the ZBJ-002 of quality 0.45% of waterborne polyurethane resin, be mixed to form hybrid resin under the stirring of stirrer that 0.4% ZBJ-003 is 1500rpm at rotating speed.And, the LJ3300 bridging agent of the quality in waterborne polyurethane resin 12%, 1% OK-412 flatting silica are joined in dispersion liquid under the stirring of the homogenizer of 3000rpm and fully stir and obtain mixed solution.Then, according to 30%, 30% and 40% add-on, divide and three times mixed solution be added in hybrid resin and obtain glue in the stirring of the stirrer of 250rpm.Then, glue is inserted and is made in bubble machine, and the foaming according to the 5 when flow of 10g/s is carried out fully foaming and obtaining aqueous polyurethane foam.Then, aqueous polyurethane foam is coated in separate-type paper, inserted in baking oven, at 110 ℃, with the speed of 12M/min, by baking oven, make to be dried to polyurethane film.Finally, polyurethane film is separated and carry out trimming from separate-type paper, obtain the finished product.
Embodiment 4: first waterborne polyurethane resin is added to and in water, fully dissolves and be mixed to form dispersion liquid with take tensio-active agent (SDBS and the NP-10 that are 1.7:1 by mass ratio form), 15% butanone and 15% toluene of quality 4% of waterborne polyurethane resin.Then, by waterborne polyurethane resin with take the ZBJ-002 of quality 0.4% of waterborne polyurethane resin, be mixed to form hybrid resin under the stirring of stirrer that 0.45% ZBJ-003 is 1200rpm at rotating speed.And, the LJ3300 bridging agent of the quality in waterborne polyurethane resin 15%, 1.3% OK-412 flatting silica are joined in dispersion liquid under the stirring of the homogenizer of 3200rpm and fully stir and obtain mixed solution.Then, according to 30%, 30% and 40% add-on, divide and three times mixed solution be added in hybrid resin and obtain glue in the stirring of the stirrer of 300rpm.Then, glue is inserted and is made in bubble machine, and the foaming according to the 6 when flow of 11g/s is carried out fully foaming and obtaining aqueous polyurethane foam.Then, aqueous polyurethane foam is coated in separate-type paper, inserted in baking oven, at 120 ℃, with the speed of 15M/min, by baking oven, make to be dried to polyurethane film.Finally, polyurethane film is separated and carry out trimming from separate-type paper, obtain the finished product.
Embodiment 5: first waterborne polyurethane resin is added to and in water, fully dissolves and be mixed to form dispersion liquid with take tensio-active agent (SDBS and the OP-10 that are 2:1 by mass ratio form), 20% butanone and 15% toluene of quality 5% of waterborne polyurethane resin.Then, by waterborne polyurethane resin with take the ZBJ-002 of quality 0.4% of waterborne polyurethane resin, be mixed to form hybrid resin under the stirring of stirrer that 0.45% ZBJ-003 is 1200rpm at rotating speed.And, the LJ3300 bridging agent of the quality in waterborne polyurethane resin 14%, 1.6% OK-412 flatting silica are joined in dispersion liquid under the stirring of the homogenizer of 3000rpm and fully stir and obtain mixed solution.Then, according to 30%, 30% and 40% add-on, divide and three times mixed solution be added in hybrid resin and obtain glue in the stirring of the stirrer of 300rpm.Then, glue is inserted and is made in bubble machine, and the foaming according to the 5 when flow of 12g/s is carried out fully foaming and obtaining aqueous polyurethane foam.Then, aqueous polyurethane foam is coated in separate-type paper, inserted in baking oven, at 140 ℃, with the speed of 18M/min, by baking oven, make to be dried to polyurethane film.Finally, polyurethane film is separated and carry out trimming from separate-type paper, obtain the finished product.
Embodiment 6: first waterborne polyurethane resin is added to and in water, fully dissolves and be mixed to form dispersion liquid with take tensio-active agent (SDS and the OP-10 that are 1.9:1 by mass ratio form), 25% butanone and 15% toluene of quality 4.5% of waterborne polyurethane resin.Then, by waterborne polyurethane resin with take the ZBJ-002 of quality 0.55% of waterborne polyurethane resin, be mixed to form hybrid resin under the stirring of stirrer that 0.55% ZBJ-003 is 1200rpm at rotating speed.And, the LJ3300 bridging agent of the quality in waterborne polyurethane resin 13%, 1.8% OK-412 flatting silica are joined in dispersion liquid under the stirring of the homogenizer of 3000rpm and fully stir and obtain mixed solution.Then, according to 30%, 30% and 40% add-on, divide and three times mixed solution be added in hybrid resin and obtain glue in the stirring of the stirrer of 300rpm.Then, glue is inserted and is made in bubble machine, and the foaming according to the 5.5 when flow of 10g/s is carried out fully foaming and obtaining aqueous polyurethane foam.Then, aqueous polyurethane foam is coated in separate-type paper, inserted in baking oven, at 150 ℃, with the speed of 20M/min, by baking oven, make to be dried to polyurethane film.Finally, polyurethane film is separated and carry out trimming from separate-type paper, obtain the finished product.
Embodiment 7: first waterborne polyurethane resin is added to and in water, fully dissolves and be mixed to form dispersion liquid with take tensio-active agent (SDS and the OP-10 that are 1.8:1 by mass ratio form), 25% butanone and 15% toluene of quality 3% of waterborne polyurethane resin.Then, by waterborne polyurethane resin with take the ZBJ-002 of quality 0.5% of waterborne polyurethane resin, be mixed to form hybrid resin under the stirring of stirrer that 0.5% ZBJ-003 is 1200rpm at rotating speed.And, the LJ3300 bridging agent of the quality in waterborne polyurethane resin 13%, 1.5% OK-412 flatting silica are joined in dispersion liquid under the stirring of the homogenizer of 3000rpm and fully stir and obtain mixed solution.Then, according to 30%, 30% and 40% add-on, divide and three times mixed solution be added in hybrid resin and obtain glue in the stirring of the stirrer of 300rpm.Then, glue is inserted and is made in bubble machine, and the foaming according to the 5.5 when flow of 6g/s is carried out fully foaming and obtaining aqueous polyurethane foam.Then, aqueous polyurethane foam is coated in separate-type paper, inserted in baking oven, at 100 ℃, with the speed of 16M/min, by baking oven, make to be dried to polyurethane film.Finally, polyurethane film is separated and carry out trimming from separate-type paper, obtain the finished product.
The polyurethane film obtaining according to embodiment 1～7 is tested ventilation property (take vapor transfer rate as index) according to ASTM D737 standard.According to JIS L1099B standard to water-repellancy (take resistance to hydrostatic pressure as index).Endwise tensile strength and transverse tensile strength are tested according to GB/T4757-1997.Above-mentioned test result is as following table:
As can be seen from the above table, the vapor transfer rate of embodiment 7 and resistance to hydrostatic pressure all want large compared with other embodiment, illustrate that implementing 7 has good ventilation property and water-repellancy.Except this, the endwise tensile strength of embodiment 7 and transverse tensile strength want large compared with other embodiment, illustrate that implementing 7 has good tensile strength.Thus, the present invention preferably implements 7 for optimum formula, in the quality of waterborne polyurethane resin, the bridging agent of the quality meter 13% of waterborne polyurethane resin, 1.5% flatting silica, 0.5% flow agent, 0.5% help stripping agent, 3% tensio-active agent (SDS and the OP-10 that are 1.8:1 by mass ratio form), the water of 25% butanone, 15% toluene and surplus.
Should be noted that and understand, in the situation that do not depart from the spirit and scope of accompanying claim the present invention for required protection, can make various modifications and improvement to the present invention of foregoing detailed description.Therefore, the scope of claimed technical scheme is not subject to the restriction of given any specific exemplary teachings.
Applicant's statement, the present invention illustrates detailed process equipment and process flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and process flow process, do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow process and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to the selection of the interpolation of the equivalence replacement of each raw material of product of the present invention and ancillary component, concrete mode etc., within all dropping on protection scope of the present invention and open scope.
Claims (10)
1. a microporous polyurethane film, it is characterized in that, comprise waterborne polyurethane resin, in the bridging agent of the quality 9～15% of waterborne polyurethane resin, 1～2% flatting silica, 0.4～0.6% flow agent, 0.4～0.6% help stripping agent, 1～5% tensio-active agent, 30～50% organic solvent, and the water of surplus.
2. polyurethane film according to claim 1, it is characterized in that, comprise waterborne polyurethane resin, in the bridging agent of the quality 13% of waterborne polyurethane resin, 1.5% flatting silica, 0.5% flow agent, 0.5% help stripping agent, 3% tensio-active agent, 40% organic solvent, and the water of surplus.
3. polyurethane film according to claim 1, is characterized in that, described tensio-active agent is (3/2～2) by quality: 1 anion surfactant and nonionogenic tenside form.
4. polyurethane film according to claim 3, is characterized in that, described anion surfactant is SDS and/or SDBS; Described nonionogenic tenside is a kind of in OP-10, OP-9, NP-9 and NP-10 or at least separately plants.
5. polyurethane film according to claim 1, is characterized in that, described bridging agent is aliphatic polymeric isocyanate.
6. polyurethane film according to claim 1, is characterized in that, described flatting silica is OK-412 flatting silica, and described flow agent is C
1～10alkyl-modified organopolysiloxane, described in help stripping agent be polyether-modified polydimethylsiloxane.
7. polyurethane film according to claim 1, is characterized in that, described organic solvent is comprised of quality 15～25% butanone and 15～25% toluene in waterborne polyurethane resin.
8. prepare a method for polyurethane film as claimed in claim 1, it is characterized in that, comprise the following steps:
(1) waterborne polyurethane resin is added to and in water, is thoroughly mixed to form dispersion liquid with the tensio-active agent in the quality 1～5% of waterborne polyurethane resin, 30～50% organic solvent;
(2) waterborne polyurethane resin is thoroughly mixed to form to hybrid resin with the flow agent in the quality 0.4～0.6% of waterborne polyurethane resin, 0.4～0.6% the stripping agent that helps, the bridging agent of the quality in waterborne polyurethane resin 9～15%, 1～2% flatting silica are added in dispersion liquid through being mixed to form mixed solution;
(3) in hybrid resin, add mixed solution, be thoroughly mixed to form glue;
(4) glue is inserted and make foaming formation aqueous polyurethane foam in bubble machine;
(5) after aqueous polyurethane foam is coated on coated substrate, coated substrate is dried, obtains polyurethane film.
9. method according to claim 8, is characterized in that, mixed solution described in step (3) successively divides and is added to hybrid resin three times according to 30%, 30% and 40% add-on; Described in step (4), the blowing ratio of foaming is 4～6, and flow is 8～12g/s.
10. method according to claim 8, is characterized in that, described in step (5), dry being specially inserted coated substrate in the baking oven of 60～150 ℃ and pass through baking oven with the speed of 10～20M/min; Described in step (5), the glue spread of coating is 140～180g/m
2, coated substrate is separate-type paper.
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Application publication date: 20140716 |