CN101125904A - Polyacrylates interpenetrating network polymer emulsion and high damping material thereof - Google Patents
Polyacrylates interpenetrating network polymer emulsion and high damping material thereof Download PDFInfo
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- CN101125904A CN101125904A CNA2007100559148A CN200710055914A CN101125904A CN 101125904 A CN101125904 A CN 101125904A CN A2007100559148 A CNA2007100559148 A CN A2007100559148A CN 200710055914 A CN200710055914 A CN 200710055914A CN 101125904 A CN101125904 A CN 101125904A
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Abstract
The invention provides polyacrylic ester interpenetrating network polymer emulsion and highly damped materials, pertaining to the high molecular polymer technological field. The polymer emulsion group consists of protecting adhesive, emulsifier, activator, buffering agent, cross-linking agent, water and monomers, wherein, the monomers comprises butyl acrylate, methacrylic acid, acrylic acid epoxy propyl ester, cinnamene, etc., and polymerize in an interpenetrating network shape. The highly damped materials used for decreasing vibration of vehicles are prepared by the emulsion after addition agent, filing materials and water are added. Since the emulsion of the invention, hollow glass microbeads and talc are used as the important components of the filling materials, the high molecular adhesive and elastic material of the invention has better damped performance, the tenacity and elasticity of the material are enhanced, the intensity of tension, and flexural rigidity resistance and wearing resistance of the material are improved, therefore, the effects of vibration decreasing, noise decreasing, sound and heat insulation can be achieved under various complicated conditions.
Description
Technical field
The invention belongs to the technical field of high molecular polymer, particularly a kind of interpenetrating network polymer emulsion, and with the synthetic damping material that is used for the water-based wide temperature zone high damping of Vehicle damper of this emulsion.
Background technology
Be applied to aspect the damping material of Vehicle damper, du pont company is made and is reduced internal car noise and vibration damper composition, see CN88102579, by vinyl monomer, as compositions such as vinylchlorid, vinylformic acid, vinylidene chlorides, its filler is a mica, 20-90%, and its feature is can use continuously at high temperature and sub-zero zero.U.S. Rohm ﹠ Haas Corp, Ford Motor Co. declare patent jointly, see CN1047679, the new vehicle vibration damper composition, form by at least two kinds of thermoplastic elastomer polymers (wherein elastomerics is by alpha-olefin nucleoid unsaturated monomer), blend polymer, its ratio of components is 1: 2, is used for the vibration damping of Ford Motor.The vibration damping sound-proof material of being made up of polyvinyl chloride and clorafin has been made by Japan Sekisui Fine Chemical Co., Ltd., sees CN1530924, is used for the vibration damping of automobile.
With the immediate prior art of the present invention be a patent of invention that on June 8th, 2005 is disclosed, publication number is CN1624015.The applicant discloses the water-base emulsion that a kind of vibroshock is used, this water-base emulsion comprises nuclear part that is formed by acrylic copolymer (A) and the particle that is formed and covered the shell part of nuclear part by acrylic copolymer (B), the second-order transition temperature of acrylic copolymer (B) is not less than-9 ℃, and the difference of the second-order transition temperature of the second-order transition temperature of acrylic copolymer (B) and acrylic copolymer (A) is not less than 20 ℃.Perhaps water-base emulsion comprises the particle that the acrylic copolymer (D) of the particle that formed by second-order transition temperature-30-0 ℃ acrylic copolymer (C) and second-order transition temperature-300 ℃ forms, and forms in the certain quality ratio.
This piece patent is by the formation nucleocapsid structure for the control of the second-order transition temperature of emulsion, and the method that makes nuclear part (A) and shell part (B) have different second-order transition temperatures realizes; Another kind method is by the multipolymer that second-order transition temperature is different (C) and the particle that (D) forms mixes the second-order transition temperature of controlling emulsion.These two kinds of methods are all wayward.And by forming the method for polymer interpenetration network, can be by calculating the formula of multipolymer second-order transition temperature, make multipolymer that the second-order transition temperature close with calculated value be arranged with the amount difference of different monomers.
Summary of the invention
The technical problem to be solved in the present invention is that employing is different from interpenetrating net polymer (IPN) technology of background technology, generates interpenetrating net polymer by multiple monomer, makes emulsion have the warm territory scope of broad; Add multiple filler, can improve the damping capacity of damping material well, improved the damping value of damping material.
The present invention is achieved in that
A kind of polyacrylates interpenetrating network polymer emulsion, component has protection glue, emulsifying agent, initiator, buffer reagent, linking agent, water and monomer, it is characterized in that, said monomer reaches and comprises butyl acrylate by mass ratio: methacrylic acid: acrylic acid epoxy propyl ester: vinylbenzene=15.3～18.8: 1.3～3.0: 0.22～0.43: 6.3～18.4, and monomer becomes the polymerization of interpenetrating(polymer)networks shape in the emulsion; Said initiator is ammonium persulphate or Potassium Persulphate; Said buffer reagent is a sodium bicarbonate aqueous solution; Said linking agent is an ethylene glycol dimethacrylate.
Said monomer also comprises: methyl methacrylate or butyl methacrylate, its content are butyl acrylate: methyl methacrylate: butyl methacrylate=15.3～18.8: 0～1.01: 0～8.25; Said monomer can also comprise Propylene glycol monoacrylate, n-methylolacrylamide, glycidyl acrylate, alpha-methyl styrene etc.
These monomeric various combinations can be regulated the second-order transition temperature of material and widen the damping temperature domain of damping material.
The synthesis technique of aforesaid polyacrylates interpenetrating network polymer emulsion may further comprise the steps:
(a) with the ammonium persulphate be the performed polymer of initiator synthesize methyl acrylic acid; Can be in the container that agitator, reflux exchanger and heating in water bath are arranged (as the 250ml three-necked bottle), add suitable quantity of water and initiator, temperature is risen to 80 ℃, add methacrylic acid monomer, react be clamminess to system in 0.8～1.8 hour till, stand-by.
(b) with the synthetic interpenetrating net polymer of method of emulsion polymerization: with ammonium persulphate, Potassium Persulphates etc. are initiator, OS, MS-1, Sodium dodecylbenzene sulfonatees etc. are emulsifying agent, ethylene glycol dimethacrylate is a linking agent, methacrylic acid, butyl acrylate, methyl methacrylate, butyl methacrylate, Propylene glycol monoacrylate, n-methylolacrylamide, glycidyl acrylate, the acrylic acid epoxy propyl ester, alpha-methyl styrene and vinylbenzene etc. are monomer, aggregate into interpenetrating net polymer with the performed polymer of methacrylic acid, temperature of reaction is 75～90 ℃.
Use polyacrylates interpenetrating network polymer emulsion of the present invention, add auxiliary agent, filler and water, can access the high damping material (coating) that is used for Vehicle damper.
The composition of said polyacrylates interpenetrating network polymer emulsion, auxiliary agent, filler and water and consumption by mass percentage are as follows:
Solid content is that 25～40% polyacrylates interpenetrating network polymer emulsions account for 36～45%;
Dispersion agent 1.0～2.0%; Wetting agent 0.3～1.0%; Defoamer 1.3～2.0; Ethylene glycol 3.0～4.0.%; Membrane-forming agent 2.4～3.0%; Thickening material 2.5～3.0%; Flow agent 0.5～2.0%; Multifunctional assistant 0.2～1.0%;
Fine particle calcium carbonate 10.2～12.5%; Hollow glass micropearl 0～6.0%; Talcum powder 8.0-10.0%; Mica 5.0～7.5%; Titanium dioxide 9.0～12.5%; Pure aluminium silicate 2.12～4.42%; Calcined kaolin 0～2.2%; Silica powder 0～2.3%; Water-ground limestone 0～2.2%; Wollastonite powder 0～2.3%.
The synthetic method that is used for the damping material of Vehicle damper of the present invention is by adding other filler and emulsion realizations such as dispersion agent, wetting agent, defoamer, ethylene glycol, fine particle calcium carbonate, hollow glass micropearl, talcum powder, mica, titanium dioxide, pure aluminium silicate, membrane-forming agent, thickening material, flow agent, multifunctional assistant, calcined kaolin, silica powder, water-ground limestone, silica ashes in water under the high-speed stirring.
In the damping material composition of the present invention, hollow glass micropearl is important.The granularity of hollow glass micropearl should be 10～400 microns, and consumption can account for 2～6% of damping material by quality.
Characteristics of the present invention are, preferred employed monomer and proportioning, and preferred initiator, buffer reagent, linking agent have made polyacrylates interpenetrating network polymer emulsion; Use interpenetrating net polymer of the present invention, use hollow glass micropearl and mica important component as filler.Thereby be that damping material of the present invention has kept the good physical and chemical index of the due water-based wide temperature zone high damping of damping material, strengthened the toughness and the elasticity of material simultaneously, improved the mechanical property of material, comprise tensile strength, counter-bending rigidity and wear resistance.Under various complicated technology conditions, can both play vibration damping, noise reduction, sound insulation, heat insulation effect.Therefore, this water-based material can satisfy environment and vehicle and use requirement to damping material, can substitute existing automobile-used asphaltic base damping material, is specially adapted to automobile chassis, covering inner panel and car door etc.
Description of drawings
Fig. 1 is the dynamic viscoelasticity spectrum figure of the embodiment of the invention 1 and embodiment 2 emulsions.
Fig. 2 is the damping value of the embodiment of the invention 1 coating and the graph of a relation of temperature.
Fig. 3 is the damping value of the embodiment of the invention 2 coating and the graph of a relation of temperature.
Fig. 4 is the dynamic viscoelasticity spectrum figure of the embodiment of the invention 3 and embodiment 4 emulsions.
Fig. 5 is the damping value of the embodiment of the invention 3 coating and the graph of a relation of temperature.
Fig. 6 is the damping value of the embodiment of the invention 4 coating and the graph of a relation of temperature.
Embodiment
Each reagent dosage of following examples 2～7 is calculated by percentage to the quality.
Embodiment 1
The preparation of methacrylic acid performed polymer: in the 250ml three-necked bottle of agitator, reflux exchanger and heating in water bath is housed, add 150ml water and 0.5g ammonium persulfate initiator, temperature is risen to 80 ℃, add methacrylic acid monomer 20.0g, react be clamminess to system in about 1 hour till, obtain the methacrylic acid performed polymer.
Embodiment 2
With the methacrylic acid performed polymer (1.09%) of embodiment 1 preparation as protecting glue; MS-1 is emulsifying agent (1.91%); ammonium persulphate is initiator (0.38%); sodium bicarbonate is buffer reagent (0.26%); ethylene glycol dimethacrylate is linking agent (0.3%); butyl acrylate (15.7%), methyl methacrylate (1.01%), methacrylic acid (2.15%), acrylic acid epoxy propyl ester (0.22%) and vinylbenzene (8.3%) are for monomer prepares polyacrylates interpenetrating network polymer emulsion, and surplus is a water in the system.
The process of preparation polyacrylates interpenetrating network polymer emulsion is, the methacrylic acid performed polymer that an amount of water and initiator and embodiment 1 are obtained adds and has agitator, in the container of condenser and heating in water bath (as 500 milliliters of there-necked flasks), be warming up to 75 ℃, reacted 10 minutes, be warming up to 85 ℃, slow dropwise addition of acrylic acid butyl ester, methyl methacrylate, methacrylic acid, the acrylic acid epoxy propyl ester, monomer such as butyl acrylate and vinylbenzene and linking agent, an amount of initiator, the aqueous solution of emulsifying agent, rise to 90 ℃ after dropwising, reacted 1 hour, cooling, repeat the process of front, hard monomer and an amount of initiators such as dropwise addition of acrylic acid butyl ester, emulsifying agent etc., temperature reaction 1.5 hours.
This emulsion is measured its dynamic mechanical spectra with the torsion braid instrument, measures frequency 10Hz; Range of measuring temp: 25 ℃～170 ℃; Temperature rise rate: 2 ℃/min.Concrete collection of illustrative plates is seen Fig. 1.
As seen from Figure 1, the damping value of emulsion in room temperature to 150 ℃ scope all than higher, warm territory broad.
After emulsion preparation is finished, Xiang Shuizhong adds dispersion agent (2.0%), wetting agent (0.32%), defoamer (1.34%), ethylene glycol (3.0%), fine particle calcium carbonate (12.46%), talcum powder (8.55%), mica (6.48%), titanium dioxide (12.46%), pure aluminium silicate (2.82%), membrane-forming agent (2.4%), thickening material (2.54%), flow agent (0.55%), multifunctional assistant filler and polyacrylates interpenetrating network polymer emulsions (44.86%) such as (0.22%), makes coating (damping material).
Behind the synthetic paint (damping material), the steel plate bar is of a size of 220*10*1.2mm, and damping fin is of a size of 220*10*7.5mm.Progressively heat up and dry, use BK company noise tester, record damping value as shown in Figure 2.
As seen from Figure 2, the damping value of coating is higher, 10～50 ℃ of scope internal damping better performances, meets the requirement to the wide temperature of material territory, high damping.
Embodiment 3
With the methacrylic acid performed polymer (1.09%) of embodiment 1 preparation as protecting glue; MS-1 is emulsifying agent (1.91%); ammonium persulphate is initiator (0.38%); sodium bicarbonate is buffer reagent (0.26%); ethylene glycol dimethacrylate is linking agent (0.3%); butyl acrylate (15.7%); methyl methacrylate (1.01%); methacrylic acid (2.15%); acrylic acid epoxy propyl ester (0.22%) and vinylbenzene (8.3%) are for monomer prepares polyacrylates interpenetrating network polymer emulsion, and surplus is water (composition of polyacrylates interpenetrating network polymer emulsion is fully identical with embodiment 2) in the system.
Preparation process is identical with embodiment 2.
This emulsion is measured its dynamic mechanical spectra with the torsion braid instrument, measures frequency 10Hz; Range of measuring temp: 25 ℃～170 ℃; Temperature rise rate: 2 ℃/min.Concrete same Fig. 1 of collection of illustrative plates.
After emulsion preparation is finished, Xiang Shuizhong adds dispersion agent (2.0%), wetting agent (0.32%), defoamer (1.34%), ethylene glycol (3.0%), fine particle calcium carbonate (12.0%), talcum powder (8.0%), mica (6.48%), titanium dioxide (9.0%), pure aluminium silicate (2.82%), glass microballon (5.46%), membrane-forming agent (2.41%), thickening material (2.54%), flow agent (0.55%), multifunctional assistant filler and polyacrylates interpenetrating network polymer emulsions (44.86%) such as (0.22%), makes coating (damping material).
Behind the synthetic paint (damping material), the steel plate bar is of a size of 220*10*1.2mm, and damping fin is of a size of 220*10*7.5mm.Progressively heat up and dry, use BK company noise tester, record damping value as shown in Figure 3.
As shown in Figure 3, added glass microballon in the filler after, the damping value of material is improved, because used emulsion is identical with embodiment 1, so the Applicable temperature scope of material is constant substantially, is 10～50 ℃ of scope internal damping better performances equally.
Embodiment 4
With the methacrylic acid performed polymer (1.09%) of embodiment 1 preparation as protecting glue; MS-1 is emulsifying agent (1.91%); Potassium Persulphate is initiator (0.38%); sodium bicarbonate is buffer reagent (0.16%); ethylene glycol dimethacrylate is linking agent (0.1%); with butyl acrylate (18.8%), methyl methacrylate (0.98%), methacrylic acid (1.32%), acrylic acid epoxy propyl ester (0.43%) and vinylbenzene (6.3%) is that monomer prepares polyacrylates interpenetrating network polymer emulsion, and surplus is a water in the system.
Preparation process is identical with embodiment 2.
This emulsion is measured its dynamic mechanical spectra with the torsion braid instrument, measures frequency 10Hz; Range of measuring temp: 25 ℃～170 ℃; Temperature rise rate: 2 ℃/min.Concrete collection of illustrative plates is seen Fig. 4.
As seen from Figure 4, this emulsion all has higher damping value in Range of measuring temp.
After emulsion preparation is finished, Xiang Shuizhong adds dispersion agent (1.03%), wetting agent (1.0%), defoamer (2.0%), ethylene glycol (4.0%), fine particle calcium carbonate (12.46%), talcum powder (10.0%), mica (7.5%), titanium dioxide (12.46%), pure aluminium silicate (4.42%), membrane-forming agent (3.0%), thickening material (2.54%), flow agent (2.0%), multifunctional assistant filler and polyacrylates interpenetrating network polymer emulsions (36.59%) such as (1.0%), makes coating (damping material).
Behind the synthetic paint (damping material), the steel plate bar is of a size of 220*10*1.2mm, and damping fin is of a size of 220*10*7.5mm.Progressively heat up and dry, use BK company noise tester, record damping value as shown in Figure 5.
As seen from Figure 5, material all has higher damping value in 30～70 ℃ of scopes, can the better temperature requirement that must satisfy use.Compare with embodiment 2, warm territory scope moves to high temperature, makes material can adapt to how different use temperatures.
Embodiment 5
With the methacrylic acid performed polymer (1.09%) of embodiment 1 preparation as protecting glue; OS is emulsifying agent (1.91%); Potassium Persulphate is initiator (0.38%); sodium bicarbonate is buffer reagent (0.16%); ethylene glycol dimethacrylate is linking agent (0.1%); butyl acrylate (18.8), methyl methacrylate (0.98%), methacrylic acid (1.32%), acrylic acid epoxy propyl ester (0.43%) and vinylbenzene (14.82%) are for monomer prepares polyacrylates interpenetrating network polymer emulsion, and surplus is a water in the system.
Preparation process is identical with embodiment 2.
After emulsion preparation is finished, Xiang Shuizhong adds dispersion agent (1.03%), wetting agent (0.32%), defoamer (1.34%), ethylene glycol (3.0%), fine particle calcium carbonate (10.26%), coarse whiting (2.2%), talcum powder (8.55%), mica (6.48%), titanium dioxide (10.02%), pure aluminium silicate (2.12%), glass microballon (2.44%), wollastonite powder (2.3%), membrane-forming agent (2.41%), thickening material (2.54%), flow agent (0.55%), multifunctional assistant filler and polyacrylates interpenetrating network polymer emulsions (44.85%) such as (0.22%) make coating (damping material).
Behind the synthetic paint (damping material), the steel plate bar is of a size of 220*10*1.2mm, and damping fin is of a size of 220*10*7.5mm.Progressively heat up and dry, use BK company noise tester, record damping value as shown in Figure 6.
As shown in Figure 6, because cinnamic increment and adding glass microballon, with relatively damping value raising of Fig. 5, damping temperature range widens.
Embodiment 6
With the methacrylic acid performed polymer (1.07%) of embodiment 1 preparation as protecting glue; OS is emulsifying agent (0.96%); Potassium Persulphate is initiator (0.49%); sodium bicarbonate is buffer reagent (0.16%); ethylene glycol dimethacrylate is linking agent (0.1%); with butyl acrylate (15.7%), methacrylic acid (1.3%), acrylic acid epoxy propyl ester (0.42%), butyl methacrylate (8.25%) and vinylbenzene (10.1%) is that monomer prepares polyacrylates interpenetrating network polymer emulsion, and surplus is a water in the system.
Preparation process is identical with embodiment 2.
After emulsion preparation is finished, Xiang Shuizhong adds dispersion agent (1.03%), wetting agent (1.0%), defoamer (1.34%), ethylene glycol (3.0%), fine particle calcium carbonate (10.26%), calcined kaolin (2.2%), talcum powder (8.55%), mica (5.0%), titanium dioxide (10.02%), pure aluminium silicate (2.12%), glass microballon (6.0%), silica powder (2.3%), membrane-forming agent (2.41%), thickening material (3.0%), flow agent (0.55%), multifunctional assistant filler and polyacrylates interpenetrating network polymer emulsions (41.0%) such as (0.22%) make coating (damping material).
Embodiment 7
With the methacrylic acid performed polymer (1.13%) of embodiment 1 preparation as protecting glue; OS is emulsifying agent (1.907%); Potassium Persulphate is initiator (0.18%); sodium bicarbonate is buffer reagent (0.16%); ethylene glycol dimethacrylate is linking agent (0.1%); with butyl acrylate (15.31%), methacrylic acid (1.32%), acrylic acid epoxy propyl ester (0.43%) and vinylbenzene (18.33%) is that monomer prepares polyacrylates interpenetrating network polymer emulsion, and surplus is a water in the system.
Preparation process is identical with embodiment 2.
After emulsion preparation is finished, Xiang Shuizhong adds dispersion agent (1.03%), wetting agent (0.32%), defoamer (1.34%), ethylene glycol (3.0%), fine particle calcium carbonate (10.26%), calcined kaolin (2.2%), talcum powder (8.55%), mica (6.48%), titanium dioxide (10.02%), pure aluminium silicate (2.12%), glass microballon (2.44%), silica powder (2.3%), membrane-forming agent (2.41%), thickening material (2.54%), flow agent (0.55%), multifunctional assistant filler and polyacrylates interpenetrating network polymer emulsions (44.85%) such as (0.22%) make coating (damping material).
Claims (5)
1. polyacrylates interpenetrating network polymer emulsion, component has protection glue, emulsifying agent, initiator, buffer reagent, linking agent, water and monomer, it is characterized in that, said monomer reaches and comprises butyl acrylate by mass ratio: methacrylic acid: acrylic acid epoxy propyl ester: vinylbenzene=15.3～18.8: 1.3～3.0: 0.22～0.43: 6.3～18.4, and monomer becomes the polymerization of interpenetrating(polymer)networks shape in the emulsion; Said initiator is ammonium persulphate or Potassium Persulphate; Said buffer reagent is a sodium bicarbonate aqueous solution; Said linking agent is an ethylene glycol dimethacrylate.
2. according to the described polyacrylates interpenetrating network polymer emulsion of claim 1, it is characterized in that, said monomer also comprises: methyl methacrylate or butyl methacrylate, its content are butyl acrylate: methyl methacrylate: butyl methacrylate=15.3～18.8: 0～1.01: 0～8.25.
3. the purposes of the polyacrylates interpenetrating network polymer emulsion of a claim 1 adds auxiliary agent, filler and water, obtains being used for the damping material of Vehicle damper.
4. according to the purposes of the described polyacrylates interpenetrating network polymer emulsion of claim 3, it is characterized in that said filler comprises hollow glass micropearl, its granularity is 10～400 microns, and consumption accounts for 2～6% of damping material by quality.
5. according to the purposes of claim 3 or 4 described polyacrylates interpenetrating network polymer emulsions, it is characterized in that the composition of said polyacrylates interpenetrating network polymer emulsion, auxiliary agent, filler and water and consumption by mass percentage are as follows:
Solid content is that 25～40% polyacrylates interpenetrating network polymer emulsions account for 36～45%;
Dispersion agent 1.0～2.0%; Wetting agent 0.3～1.0%; Defoamer 1.3～2.0; Ethylene glycol 3.0～4.0.%; Membrane-forming agent 2.4～3.0%; Thickening material 2.5～3.0%; Flow agent 0.5～2.0%; Multifunctional assistant 0.2～1.0%;
Fine particle calcium carbonate 10.2～12.5%; Hollow glass micropearl 0～6.0%; Talcum powder 8.0-10.0%; Mica 5.0～7.5%; Titanium dioxide 9.0～12.5%; Pure aluminium silicate 2.12～4.42%; Calcined kaolin 0～2.2%; Silica powder 0～2.3%; Water-ground limestone 0～2.2%; Wollastonite powder 0～2.3%.
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