CN1544521A - Method for reducing surface tension of polymeric system - Google Patents
Method for reducing surface tension of polymeric system Download PDFInfo
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- CN1544521A CN1544521A CNA2003101108937A CN200310110893A CN1544521A CN 1544521 A CN1544521 A CN 1544521A CN A2003101108937 A CNA2003101108937 A CN A2003101108937A CN 200310110893 A CN200310110893 A CN 200310110893A CN 1544521 A CN1544521 A CN 1544521A
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Abstract
A method for lowering polymer system interfacial tension comprises, preparing hydrogen containing proton donor polymer, preparing hydrogen containing proton acceptor polymer, then preparing polymer compound system, through the interaction of functional groups on the macromolecular chains of two or more complementary chemical constitutions, the polymer system interfacial tension can be lowered.
Description
One, technical field
The present invention relates to the capillary method of a kind of reduction polymeric system, belong to molecule field of compounding between polymer.
Two, background technology
Originally the development of low surface energy coat material is in order to solve the adhesion problems of aquatic adhesivity biology to object in the water.Along with the raising of people's living standard, people are more and more higher to the requirement of quality of life, and the low surface energy coat material also has been applied in the daily life gradually, as non-stick pan, anti-dirt metope etc.The low surface energy coat material belongs to environment-friendly material, thereby has broad application prospects.
For making polymeric system have lower surface tension, generally adopt following several method:
1. in polymeric system, add surfactant
Although this method can reduce the surface tension of polymeric system, because the surface tension of the surfactant of introducing is low, surfactant migration has reduced the water resistance of coating to the surface of coating in film forming procedure.
2. reduction polymer molecular weight
Though this method can reduce the surface tension of polymkeric substance, reduced the internal cohesive energy of polymkeric substance simultaneously, cause polymeric system that the sticking power of stromal surface is reduced.
3. in polymeric system, introduce low surface energy polymeric by copolymerization or blend method
The method on the polymer molecular chain that is modified of being grafted to organosilicon, fluoropolymer that will have low surface energy structures by copolymerization etc. can reduce surface tension (Huang Shiqiang, Peng Hui, the Zhu Jie etc. of polymeric system effectively, the material Leader, 1997,11 (5), 52～54; Xu Zushun, Chen Zhonghua etc., functional polymer journal, 2000,13 (2), 229～231; L.vanRavenstein, W.Ming, R.D.van de Grampel, R.van der Linde, G.de With, T.Loontjes, P.C.Th ü ne, J.W.Niemantsverdriet, Pol.Mater.Sci.Eng., 2003,88,266-267), but polymerization process has certain degree of difficulty.And with low surface energy polymeric and the direct blend of polymeric system that is modified, low surface energy polymeric can move, be gathered in the surface of coating in film forming procedure.
Three, summary of the invention
The objective of the invention is provides a kind of reduction polymeric system capillary method at the deficiencies in the prior art.Be characterized at first preparing the polymer compositional system of chemical constitution complementation, interacting by Coulomb force stronger between the macromolecular chain of these chemical constitution complementations, hydrogen bond etc. forms polymer composites again.The surface tension that formed polymer composite body is can be lower than the surface tension of two compositional systems, i.e. the interaction of the polymer molecule interchain of complementary structure can reduce the surface tension of system.
Purpose of the present invention is realized that by following technical measures wherein said umber is parts by weight except that specified otherwise.
Reduce the capillary preparation method of polymeric system
1) the chemical structure complementary is formed the preparation of polymkeric substance
(1) preparation of hydrogeneous protophobe polymkeric substance
A takes by weighing DBSA 5-12 part by weight, octamethylcy-clotetrasiloxane 10-30 part, coupling agent 1-5 part and deionized water 53-84 part join with thermometer, agitator, in the three-necked bottle of dropping funel and reflux condenser, temperature 70-90 ℃ of reaction 5-10 hour, be down to then room temperature, regulate pH=5-6 with alkali lye, discharging, obtain dimethyl silicone polymer seeding polymerization objects system PDMS, take by weighing by weight again PDMS15-50 part, deionized water 10-20 part, acrylic ester monomer 5-10 part and acrylic monomer 1-3 part are to the same equipment, temperature 30-50 ℃ swelling 0.5-1 hour, be warming up to 70-90 ℃, drip then persulfate solution 10-15 part that the mix monomer that is made up of acrylic ester monomer 15-20 part and acrylic monomer 1-7 part and concentration are 0.5-2.5wt%, adding concentration is 1.5-2.5wt% sodium bicarbonate solution 8-10 part, reacted 3-5 hour, and be down to the room temperature discharging, obtain the polymeric system PA of hydrogeneous proton donor
1
B takes by weighing acrylic monomer 10-15 part by weight, persulfate 0.1-0.5 part, and deionized water 85-90 part joins in the same equipment, stirs and is warming up to 70-90 ℃, reacts 2-5 hour, is down to the room temperature discharging, obtains the polymeric system PA of hydrogeneous proton donor
2
(2) preparation of hydrogeneous proton accepting polymer
A takes by weighing above-mentioned (1) prepared PDMS15-50 part by weight, deionized water 10-20 part, vinylacetate 4-8 part and acrylic ester monomer 2-5 part, add in the same equipment, temperature 30-50 ℃ swelling 0.5-1 hour, be warming up to 70-80 ℃, the mix monomer and the concentration that drip then vinylacetate 8-15 part and acrylic ester monomer 8-12 part composition are 0.5-2.5wt% persulfate solution 10-15 part, adding concentration is 1.5-2.5wt% sodium bicarbonate solution 8-10 part, reacted 3-5 hour, be down to the room temperature discharging, obtain the polymeric system PB of hydrogeneous proton acceptor
1
B takes by weighing vinyl pyrrolidone 60-80 part by weight, persulfate 0.1-0.5 part, deionized water 20-40 part, join in the same equipment, stir and be warming up to 60-80 ℃, reacted 2-5 hour, be down to the room temperature discharging, obtain the polymeric system PB of hydrogeneous proton acceptor
2
2) preparation of polymer composites
(1) with PA
110-90 part and PB
190-10 part joins in the three-necked bottle with agitator gradually, stirs, and makes polymer composites PA
1/ PB
1
(2) with PA
2, PB
2Be mixed with respectively 0.04,0.02, the solution of 0.0005g/ml, and with the PA of same concentrations
2And PB
2By 1: 9-9: 1 volume ratio is mixed respectively, makes polymer composites PA
2/ PB
2
3) performance
(1) surface tension of system
Polymeric system PA
1, PB
1And different composite is than compound system PA
1/ PB
1Surface tension test comparative result see for details shown in Figure 1.The result shows: compound ratio is 1: 9 compound system PA
1/ PB
1Surface tension be lower than two compositional system PA
1, PB
1Surface tension.Under the different concns, polymeric system PA
2, PB
2And different composite is than compound system PA
2/ PB
2Surface tension test comparative result sees Fig. 2 for details.The result shows: no matter the concentration of system is 0.04g/ml, 0.02g/ml or 0.0005g/ml, certain compound than scope in, compound system PA
2/ PB
2Surface tension be starkly lower than two compositional system PA
2, PB
2Surface tension.Thus, can reduce the surface tension of compound system by the compound method of molecule between macromolecule.
(2) mechanical property of coating
Polymeric system PA
1, PB
1And different composite is than compound system PA
1/ PB
1The Mechanics Performance Testing result of the coating that forms sees Fig. 3 for details.The result shows: still keep higher elongation at break by the compound coating that can make of molecule between macromolecule when obtaining than high tensile.Thus, can improve the mechanical property of coating by the compound method of molecule between macromolecule.
(3) water resistance of coating
Polymeric system PA
1, PB
1And compound ratio is respectively the compound system PA of 4: 6 and 2: 8
1/ PB
1The water resistance test result of the coating that forms in 300 hours see Fig. 4 for details.The result shows: by compound system PA
1/ PB
1The water resistance of the coating that forms is higher than two and forms polymeric system PA
1, PB
1Water resistance.Thus, can improve the water resistance of coating by the compound method of molecule between macromolecule.
The present invention has following advantage:
1. by the compound polymeric system surface tension that reduces of the molecule between polymer, be the capillary novel method of a kind of reduction polymeric system.
2. by the compound cohesive energy that can improve polymeric system of the molecule between macromolecule, the mechanical property of the coating material that forms and water resistance are all obviously improved.
3. the inventive method is simple, and cost is low, easily realizes.
Four, description of drawings
Fig. 1 is polymeric system PA
1, PB
1And different composite is than compound system PA
1/ PB
1Surface tension test result figure.
Fig. 2 is under the different concns, polymeric system PA
2, PB
2And different composite is than compound system PA
2/ PB
2Surface tension test result figure.
Fig. 3 is polymeric system PA
1, PB
1And different composite is than compound system PA
1/ PB
1The Mechanics Performance Testing of the coating that forms is figure as a result.
Fig. 4 is polymeric system PA
1, PB
1And different composite is than compound system PA
1/ PB
1The water resistance test result figure of the coating that forms.Sample1 and sample2 represent respectively by polymeric system PA
1And PB
1Formed coating; It is the formed coating of compound system of 4: 6 and 2: 8 that sample3 and sample4 represent respectively by compound ratio.
Five, embodiment
Below by embodiment the present invention is specifically described; be necessary to be pointed out that at this this experimental example only is used for that the present invention will be described; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment according to the content of foregoing invention.
Embodiment 1:
1) the chemical structure complementary is formed the preparation of polymkeric substance
(1) preparation of hydrogeneous protophobe polymkeric substance
A takes by weighing DBSA 8 grams by weight, octamethylcy-clotetrasiloxane 10 grams, VTES 2 grams and deionized water 67 grams join with thermometer, agitator, in the three-necked bottle of dropping funel and reflux condenser, 75 ℃ of reactions of temperature 10 hours, be down to then room temperature, regulate pH=5-6 with NaOH solution, discharging, obtain dimethyl silicone polymer seeding polymerization objects system PDMS, take by weighing by weight again the PDMS45 gram, deionized water 12 grams, methyl methacrylate 3 grams, butyl acrylate 2 grams, methacrylic acid 3 gram adds in the same equipment, in 40 ℃ of swellings of temperature after 0.5 hour, be warming up to 75 ℃, drip then by methyl methacrylate 5 grams, mix monomer and concentration that butyl acrylate 10 grams and methacrylic acid 2 grams form are 1.5wt% potassium persulfate solution 10 grams, and adding concentration is 1.5wt% sodium bicarbonate solution 8 grams, reacts 3 hours, be down to the room temperature discharging, obtain the polymeric system PA of hydrogeneous proton donor
1
B takes by weighing methacrylic acid 10 grams by weight, potassium peroxydisulfate 0.2 gram, and deionized water 90 grams join in the same equipment, stir and are warming up to 75 ℃, react 3 hours, are down to the room temperature discharging, obtain the polymeric system PA of hydrogeneous proton donor
2
(2) preparation of hydrogeneous proton accepting polymer
A takes by weighing above-mentioned (1) prepared PDMS45 gram by weight, deionized water 12 grams, vinylacetate 5 grams and butyl acrylate 3 grams, add in the same equipment, in 40 ℃ of swellings of temperature after 0.5 hour, be warming up to 75 ℃, dripping then the mix monomer and the concentration that are made up of vinylacetate 9 grams and butyl acrylate 8 grams is 1.5wt% potassium persulfate solution 10 grams, adding concentration is 1.5wt% sodium bicarbonate solution 8 grams, reacted 3 hours, be down to the room temperature discharging, obtain the polymeric system PB of hydrogeneous proton acceptor
1
B takes by weighing vinyl pyrrolidone 70 grams by weight, potassium peroxydisulfate 0.3 gram, and deionized water 30 grams join in the same equipment, stir and are warming up to 75 ℃, react 3 hours, are down to the room temperature discharging, obtain the polymeric system PB of hydrogeneous proton acceptor
2
2) preparation of polymer composites
(1) with PA
110-90 part and PB
190-10 part joins in the three-necked bottle with agitator gradually, stirs, and makes polymer composites PA
1/ PB
1Left standstill three days, under the room temperature, with the surface tension of the digital surface tension instrument test compound of K10ST system.
(2) with PA
2, PB
2Be mixed with 0.04,0.02 respectively, the solution of 0.0005g/ml, and with the PA of same concentrations
2And PB
2By 1: 9-9: 1 volume ratio thorough mixing, making polymer composite body is PA
2/ PB
2Left standstill three days, under the room temperature, with the surface tension of JzhY1-180 surface tension instrument test compound system.
Embodiment 2:
1) the chemical structure complementary is formed the preparation of polymkeric substance
(1) preparation of hydrogeneous protophobe polymkeric substance
A takes by weighing DBSA 5 grams, octamethylcy-clotetrasiloxane 17 grams, vinyltrimethoxy silane 3 grams and deionized water 75 grams join with thermometer, agitator, in the three-necked bottle of dropping funel and reflux condenser, 80 ℃ of reactions of temperature 8 hours, be down to then room temperature, regulate pH=5-6 with NaOH solution, discharging, obtain dimethyl silicone polymer seeding polymerization objects system PDMS, take by weighing by weight again the PDMS31 gram, deionized water 16 grams, methyl methacrylate 3 grams, butyl acrylate 5 grams and methacrylic acid 2 grams are to the same equipment, after 1 hour, be warming up to 80 ℃ in the temperature 45 C swelling, drip then by methyl methacrylate 8 grams, the mix monomer that butyl acrylate 10 grams and methacrylic acid 3 grams form and concentration are 1wt% ammonium persulfate solution 13 grams, add 2.5wt% sodium bicarbonate solution 9 grams, reacted 4 hours, and be down to the room temperature discharging, obtain the polymeric system PA of hydrogeneous proton donor
1
B takes by weighing methacrylic acid 13 grams, ammonium persulfate 0.3 gram, and deionized water 87 grams join in the same equipment, stir and are warming up to 80 ℃, react 4 hours, are down to the room temperature discharging, obtain the polymeric system PA of hydrogeneous proton donor
2
(2) preparation of hydrogeneous proton accepting polymer
A takes by weighing (1) prepared PDMS 31 grams, deionized water 16 grams, vinylacetate 6 gram and butyl acrylate 4 restrain, and add in the same equipment, 45 ℃ of swellings after 1 hour, be warming up to 80 ℃, drip then the mix monomer and 1wt% ammonium persulfate solution 13 grams that are formed by vinylacetate 11 grams and butyl acrylate 10 grams, add 2.5wt% sodium bicarbonate solution 9 grams, reacted 4 hours, be down to the room temperature discharging, obtain the polymeric system PB of hydrogeneous proton acceptor
1
B takes by weighing vinyl pyrrolidone 75 grams, ammonium persulfate 0.4 gram, and deionized water 25 grams join in the same equipment, stir and are warming up to 80 ℃, react 4 hours, are down to the room temperature discharging, obtain the polymeric system PB of hydrogeneous proton acceptor
2
2) preparation of polymer composites
(1) with PA
110-90 part and PB
190-10 part joins in the three-necked bottle with agitator gradually, stirs, and makes polymer composites PA
1/ PB
1Left standstill three days, under the room temperature, with the surface tension of the digital surface tension instrument test compound of K10ST system.
(2) with PA
2, PB
2Be mixed with 0.04,0.02 respectively, the solution of 0.0005g/ml, and with the PA of same concentrations
2And PB
2By 1: 9-9: 1 volume ratio thorough mixing, making polymer composite body is PA
2/ PB
2Left standstill three days, under the room temperature, with the surface tension of JzhY1-180 surface tension instrument test compound system.
Embodiment 3:
1) the chemical structure complementary is formed the preparation of polymkeric substance
(1) preparation of hydrogeneous protophobe polymkeric substance
A takes by weighing DBSA 10 grams, octamethylcy-clotetrasiloxane 25 grams, γ-methacryloxypropyl trimethoxy silane 5 grams and deionized water 60 grams join with thermometer, agitator, in the three-necked bottle of dropping funel and reflux condenser, 85 ℃ of reactions of temperature 5 hours, be down to then room temperature, regulate pH=5-6 with NaOH solution, discharging, obtain dimethyl silicone polymer seeding polymerization objects system PDMS, take by weighing by weight again the PDMS20 gram, deionized water 20 grams, methyl methacrylate 6 grams, butyl acrylate 4 grams and methacrylic acid 1 gram are to the same equipment, temperature 50 C swelling 0.75 hour, be warming up to 85 ℃, drip then by methyl methacrylate 8 grams, the mix monomer that butyl acrylate 10 grams and methacrylic acid 5 grams form and concentration are 2wt% sodium peroxydisulfate solution 14 grams, adding concentration is 2wt% sodium bicarbonate solution 10 grams, reacted 5 hours, and be down to the room temperature discharging, obtain the polymeric system PA of hydrogeneous proton donor
1
B takes by weighing methacrylic acid 15 grams, sodium peroxydisulfate 0.5 gram, and deionized water 85 grams join in the same equipment, stir and are warming up to 85 ℃, react 5 hours, are down to the room temperature discharging, obtain the polymeric system PA of hydrogeneous proton donor
2
(2) preparation of hydrogeneous proton accepting polymer
A takes by weighing above-mentioned (1), and prepared PDMS 20 restrains, deionized water 20 grams, vinylacetate 7 gram and butyl acrylate 4 restrain, and add in the same equipment, temperature 50 C swelling 0.75 hour, be warming up to 70 ℃, dripping then the mix monomer and the concentration that are made up of vinylacetate 13 grams and butyl acrylate 12 grams is 2wt% sodium peroxydisulfate solution 14 grams, and adding concentration is 2wt% sodium bicarbonate solution 10 grams, reacts 5 hours, be down to the room temperature discharging, obtain the polymeric system PB of hydrogeneous proton acceptor
1
B takes by weighing vinyl pyrrolidone 80 grams, sodium peroxydisulfate 0.5 gram, and deionized water 20 grams join in the same equipment, stir and are warming up to 75 ℃, react 5 hours, are down to the room temperature discharging, obtain the polymeric system PB of hydrogeneous proton acceptor
2
2) preparation of polymer composites
(1) with PA
110-90 part and PB
190-10 part joins in the three-necked bottle with agitator gradually, stirs, and makes polymer composites PA
1/ PB
1Left standstill three days, under the room temperature, with the surface tension of the digital surface tension instrument test compound of K10ST system.
(2) with PA
2, PB
2Be mixed with 0.04,0.02 respectively, the solution of 0.0005g/ml, and with the PA of same concentrations
2And PB
2By 1: 9-9: 1 volume ratio thorough mixing, making polymer composite body is PA
2/ PB
2Left standstill three days, under the room temperature, with the surface tension of JzhY1-180 surface tension instrument test compound system.
Claims (4)
1. one kind is reduced the capillary method of polymeric system, it is characterized in that:
1) the chemical structure complementary is formed the preparation of polymkeric substance
(1) preparation of hydrogeneous protophobe polymkeric substance
A takes by weighing Witco 1298 Soft Acid 5-12 part by weight, octamethylcyclotetrasiloxane 10-30 part, coupling agent 1-5 part and deionized water 53-84 part join and have thermometer, agitator, in the three-necked bottle of dropping funnel and reflux exchanger, temperature 70-90 ℃ of reaction 5-10 hour, reduce to room temperature then, regulate pH=5-6 with alkali lye, discharging, obtain polydimethylsiloxane seeding polymerization objects system PDMS, take by weighing PDMS 15-50 part more by weight, deionized water 10-20 part, acrylic ester monomer 5-10 part and acrylic monomer 1-3 part are to the same equipment, temperature 30-50 ℃ swelling 0.5-1 hour, be warming up to 70-90 ℃, drip persulfate solution 10-15 part that the mix monomer be made up of acrylic ester monomer 15-20 part and acrylic monomer 1-7 part and concentration are 0.5-2.5wt% then, adding concentration is 1.5-2.5wt% sodium hydrogen carbonate solution 8-10 part, reacted 3-5 hour, and reduced to the room temperature discharging, obtain the polymeric system PA of hydrogeneous protophobe
1,
B takes by weighing acrylic monomer 10-15 part by weight, persulphate 0.1-0.5 part, and deionized water 85-90 part joins in the same equipment, stirs and is warming up to 70-90 ℃, reacts 2-5 hour, reduces to the room temperature discharging, obtains the polymeric system PA of hydrogeneous protophobe
2,
(2) preparation of hydrogeneous proton accepting polymer
A takes by weighing above-mentioned (1) prepared PDMS 15-50 part by weight, deionized water 10-20 part, vinyl acetate 4-8 part and acrylic ester monomer 2-5 part, add in the same equipment, temperature 30-50 ℃ swelling 0.5-1 hour, be warming up to 70-80 ℃, the mix monomer and the concentration that drip vinyl acetate 8-15 part and acrylic ester monomer 8-12 part composition then are 0.5-2.5wt% persulfate solution 10-15 part, adding concentration is 1.5-2.5wt% sodium hydrogen carbonate solution 8-10 part, reacted 3-5 hour, reduce to the room temperature discharging, obtain the polymeric system PB of hydrogeneous proton acceptor
1,
B takes by weighing vinyl pyrrolidone 60-80 part by weight, persulphate 0.1-0.5 part, deionized water 20-40 part, join in the same equipment, stir and be warming up to 60-80 ℃, reacted 2-5 hour, reduce to the room temperature discharging, obtain the polymeric system PB of hydrogeneous proton acceptor
2,
2) preparation of polymer composites
(1) with PA
110-90 part and PB
190-10 part joins in the three-necked bottle that has agitator gradually, stirs, and making polymer composite body is PA
1/ PB
1,
(2) with PA
2, PB
2Be mixed with respectively 0.04,0.02, the solution of 0.0005g/ml, and with the PA of same concentrations
2And PB
2By 1: 9-9: 1 volume ratio is mixed respectively, makes polymer composites PA
2/ PB
2
2. reduce the capillary method of polymeric system according to claim 1, it is characterized in that coupling agent is CH
2=C (R
1)-R
2-Si-(O-R
3)
3, wherein, R
1=H ,-CH
3Or-CH
2CH
3, R
2=O ,-COO (CH
2)
3-, R
3=-CH
3,-CH
2CH
3
3. reduce the capillary method of polymeric system according to claim 1, it is characterized in that acrylate monomer is at least a in methyl methacrylate, methyl acrylate, butyl acrylate or the ethyl propenoate monomer.
4. reduce the capillary method of polymeric system according to claim 1, it is characterized in that acrylic monomer is methacrylic acid or vinylformic acid.
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|---|---|---|---|
| CN 200310110893 CN1261500C (en) | 2003-11-10 | 2003-11-10 | Method for reducing surface tension of polymeric system |
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|---|---|---|---|
| CN 200310110893 CN1261500C (en) | 2003-11-10 | 2003-11-10 | Method for reducing surface tension of polymeric system |
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| Publication Number | Publication Date |
|---|---|
| CN1544521A true CN1544521A (en) | 2004-11-10 |
| CN1261500C CN1261500C (en) | 2006-06-28 |
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| Country | Link |
|---|---|
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2003
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Application publication date: 20041110 Assignee: Chengzhou Fengsheng Optoelectronics Co., Ltd. Assignor: Sichuan University Contract record no.: 2010320000407 Denomination of invention: Method for reducing surface tension of polymeric system Granted publication date: 20060628 License type: Exclusive License Record date: 20100416 |
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