CN105295280A - Transparent rubber modified polymethyl methacrylate resin composition and preparation method thereof - Google Patents
Transparent rubber modified polymethyl methacrylate resin composition and preparation method thereof Download PDFInfo
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- CN105295280A CN105295280A CN201510846185.2A CN201510846185A CN105295280A CN 105295280 A CN105295280 A CN 105295280A CN 201510846185 A CN201510846185 A CN 201510846185A CN 105295280 A CN105295280 A CN 105295280A
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Abstract
The invention provides a transparent rubber modified polymethyl methacrylate resin composition, and belongs to the technical field of high polymer materials. The composition comprises 12-23.14 parts of rubber copolymer and 48-36.86 parts of PMMA matrix resin according to weight parts, wherein the rubber copolymer comprises 20-80 parts of nuclear copolymer and 80-20 parts of shell polymer according to weight parts; the nuclear copolymer comprises 60-75 parts of a butyl acrylate monomer, 20-40 parts of a butadiene monomer and 0-10 parts of a styrene monomer according to weight parts; the shell polymer is polymethyl methacrylate. The invention further provides a preparation method for the transparent rubber modified polymethyl methacrylate resin. The transparent resin is obtained through adjustment of biphase refraction index, so that the resin has better transparency and toughness.
Description
Technical field
The invention belongs to technical field of polymer materials, be specifically related to a kind of transparent rubber-modified plexiglass composition and method of making the same.
Background technology
With the transparent PMMA resin that copolymer particle is toughness reinforcing, there are good shock-resistance, the transparency, processibility etc.Therefore they can be widely used for the various fields such as electric appliance casing, refrigerator interior trim, food product containers.Along with the demand of transparent resin increases day by day, more and more need the balance of PMMA resin physicals between shock-resistance and the transparency of modified rubber.But, at present large quantifier elimination still do not reach make us well-content degree.
Such as, Chinese patent CN101870794B disclosed in Shenzhen Keju New Material Co., Ltd., disclosed is a kind of transparent toughened polymethyl methacrylate (PMMA) material and preparation method thereof.This material has the good transparency, but shock-resistance is not but very good.For another example, Chinese publication CN104559003A, disclosed is a kind of high tenacity height printing opacity diffusion PMMA material and preparation method thereof.The light diffusion PMMA material transmissivity that the method obtains is high, mist degree is low, good weatherability, but poor toughness.
Summary of the invention
The object of this invention is to provide a kind of transparent rubber-modified plexiglass composition and method of making the same, this resin combination has the transparency and toughness preferably.
First the present invention provides a kind of transparent rubber-modified plexiglass composition, according to parts by weight, comprising:
Rubbery copolymer 12-23.14 weight part and PMMA matrix resin 48-36.86 weight part;
Described rubbery copolymer, according to parts by weight, comprising: stratum nucleare multipolymer 20-80 weight part and sheath polymers 80-20 weight part;
Described stratum nucleare multipolymer, according to parts by weight, comprising: Butyl Acrylate Monomer 60-75 weight part, divinylic monomer 20-40 weight part and styrene monomer 0-10 weight part;
Described sheath polymers is polymethylmethacrylate.
Preferably, the preparation method of described rubbery copolymer, comprising:
Deionized water is injected there-necked flask, then trisodium phosphate, glucose and ferrous sulfate is added successively, potassium hydroxide is added again after abundant dissolving, emulsifying agent and stratum nucleare multipolymer, there-necked flask is put into water bath with thermostatic control constant temperature to 60-70 DEG C, in there-necked flask, pass into nitrogen and stir 10-20 minute simultaneously, taking methyl methacrylate monomer and initiator preparation methyl methacrylate dropping monomer;
Adopt continuously feeding method that the methyl methacrylate prepared is dripped monomer dropping in there-necked flask, add initiator before dropping, time for adding is 10-60 minute, drips and terminates to add initiator again, reaction 30-90 minute, after reacting completely, cool to 60 DEG C, add oxidation inhibitor, continue to stir 1-30 minute, discharging, adds flocculation agent, can obtain rubbery copolymer.
Preferably, the preparation method of described stratum nucleare multipolymer, comprising:
Emulsifying agent, molecular weight regulator, initiator, Butyl Acrylate Monomer, styrene monomer and water are joined in reactor, then divinylic monomer is added after reactor is airtight, reactor is placed in revolution water bath with thermostatic control and carries out polyreaction, and reaction end obtains butyl acrylate/Butadiene/Styrene latex.
Preferably, described emulsifying agent is the blending emulsifiers of rosin soap lye and fatty acid soaps.
Preferably, described rosin soap lye and the weight ratio of fatty acid soaps are 1:1.
Preferably, described initiator comprises Potassium Persulphate or Ammonium Persulfate 98.5.
Preferably, described oxidation inhibitor comprises β-(4-hydroxyl-3,5-di-tert-butyl-phenyl) positive octadecyl ester of propionic acid or 2,2 '-methylene-bis (4-methyl-6-tert-butylphenol).
Preferably, described flocculation agent is selected from one or more in sulfuric acid, hydrochloric acid, phosphoric acid, acetic acid, calcium chloride, magnesium chloride, bariumchloride, aluminum chloride, magnesium sulfate or Tai-Ace S 150.
The present invention also provides a kind of preparation method of transparent rubber modified thenylethylene resin, comprising: take rubbery copolymer and PMMA matrix resin carries out melt blending, can obtain transparent rubber-modified plexiglass composition.
Preferably, described melt blending temperature is 170-180 DEG C, and the melt blending time is 5-10 minute.
Beneficial effect of the present invention
First the present invention provides a kind of transparent rubber-modified plexiglass composition, according to parts by weight, comprising: rubbery copolymer 12-23.14 weight part and PMMA matrix resin 48-36.86 weight part; Described rubbery copolymer, according to parts by weight, comprising: stratum nucleare multipolymer 20-80 weight part and sheath polymers 80-20 weight part; Described stratum nucleare multipolymer, according to parts by weight, comprising: Butyl Acrylate Monomer 60-75 weight part, divinylic monomer 20-40 weight part and styrene monomer 0-10 weight part; Described sheath polymers is polymethylmethacrylate monomer.The present invention obtains transparent resin by regulating the refractive index of two-phase, makes this resin have the transparency and toughness preferably.
The present invention also provides a kind of preparation method of transparent rubber modified thenylethylene resin, and rubbery copolymer and PMMA matrix resin are carried out melt blending by the method, can obtain transparent rubber-modified plexiglass composition.Preparation method of the present invention is simple, raw material is easy to get, and the composition prepared has the good transparency and toughness.
Embodiment
First the present invention provides a kind of transparent rubber-modified plexiglass composition, according to parts by weight, comprising: rubbery copolymer 12-23.14 weight part, is preferably 14-20 weight part, is more preferably 15-18 weight part; PMMA matrix resin 48-36.86 weight part, is preferably 46-40 weight part, is more preferably 45-42 weight part;
Wherein rubbery copolymer, according to parts by weight, comprising: stratum nucleare multipolymer 60-90 weight part, is preferably 65-80 weight part, is more preferably 70-75 weight part; Sheath polymers 40-10 weight part, is preferably 35-20 weight part, is more preferably 30-25 weight part;
Wherein stratum nucleare multipolymer is according to parts by weight, comprising: Butyl Acrylate Monomer 60-75 weight part, is preferably 63-72 weight part, is more preferably 65-70 weight part; Divinylic monomer 20-40 weight part, is preferably 23-35 weight part, is more preferably 25-30 weight part; Styrene monomer 0-10 weight part, is preferably 3-8 weight part, is more preferably 5-7 weight part.
Described sheath polymers is polymethylmethacrylate.
According to the present invention, the preparation method of described rubbery copolymer, preferably includes:
100-300 parts by weight of deionized water is injected there-necked flask, then 0.1-0.7 weight part trisodium phosphate is added successively, 0.3-0.9 weight part glucose and 0.001-0.03 parts by weight of ferrous sulfate, 0.01-0.10 weight part potassium hydroxide is added again after abundant dissolving, 1-6 parts by weight Emulsifier and 100-300 weight part stratum nucleare multipolymer, there-necked flask is put into water bath with thermostatic control constant temperature to 60-70 DEG C, in there-necked flask, pass into nitrogen and stir 10-20 minute simultaneously, take 10-40 parts by weight of methylmethacrylate monomer and 0.10-0.35 weight part initiator preparation methyl methacrylate dropping monomer, described emulsifying agent is preferably the blending emulsifiers of rosin soap lye and fatty acid soaps, and described rosin soap lye and the weight ratio of fatty acid soaps are preferably 1:1,
Adopt continuously feeding method that the methyl methacrylate prepared is dripped monomer dropping in there-necked flask, add 0.01-0.20 weight part initiator before dropping, time for adding is 10-60 minute, drips and terminates to add 0.01-0.20 weight part initiator again, reaction 30-90 minute, after reacting completely, cool to 60 DEG C, add 1-20 weight part oxidation inhibitor, continue to stir 1-30 minute, discharging, adds 5 weight part flocculation agents, can obtain rubbery copolymer; The preferred persulfuric acid salt of described initiator, more preferably comprises Potassium Persulphate and Ammonium Persulfate 98.5; The preferred single phenolic antioxidant of described oxidation inhibitor and Polyphenols oxidation inhibitor, more preferably comprise β-(4-hydroxyl-3,5-di-tert-butyl-phenyl) positive octadecyl ester of propionic acid and 2,2 '-methylene-bis (4-methyl-6-tert-butylphenol); Described flocculation agent is preferably selected from one or more in sulfuric acid, hydrochloric acid, phosphoric acid, acetic acid, calcium chloride, magnesium chloride, bariumchloride, aluminum chloride, magnesium sulfate or Tai-Ace S 150.
According to the present invention, described stratum nucleare multipolymer is butyl acrylate/Butadiene/Styrene latex, and concrete preparation method, comprising:
Emulsifying agent, molecular weight regulator, initiator, Butyl Acrylate Monomer, styrene monomer and water are joined in reactor, then divinylic monomer is added after reactor is airtight, reactor is placed in revolution water bath with thermostatic control and carries out polyreaction, and reaction end obtains butyl acrylate/Butadiene/Styrene latex.
According to the present invention, described emulsifying agent is the blending emulsifiers of rosin soap lye and fatty acid soaps, and described rosin soap lye and the mass ratio of fatty acid soaps are preferably 1:1; Described molecular weight regulator is preferably selected from one or more in methyl mercaptan, cyclohexanethiol, n-dodecyl mercaptan, tertiary lauryl mercaptan, n-tetradecane base mercaptan; Described initiator is preferably persulfuric acid salt initiator, is more preferably Potassium Persulphate and Ammonium Persulfate 98.5.
According to the present invention, the weight ratio of described emulsifying agent, molecular weight regulator, initiator, Butyl Acrylate Monomer, styrene monomer and divinylic monomer is (150-300): (0.1-2): (0.1-2): (300-375): (0-50): (100-200).According to the present invention, described polymerization temperature is preferably 60-75 DEG C, and polymerization time is preferably 20-30 hour.
The present invention also provides a kind of preparation method of transparent rubber modified thenylethylene resin, comprising: take rubbery copolymer and PMMA matrix resin carries out melt blending, can obtain transparent rubber-modified plexiglass composition.Described melt blending temperature is preferably 170-180 DEG C, and the melt blending time is preferably 5-10 minute.
The present invention is described in further detail for following embodiment, but it is to be noted that these embodiments should be counted as limitation of the scope of the invention in no instance.
Embodiment 1
The preparation of stratum nucleare multipolymer
The blending emulsifiers (weight ratio 1:1) of 150 weight part rosin soap lyes and fatty acid soaps, the tertiary lauryl mercaptan of 1 weight part, 1.27 weight part Potassium Persulphates, 350 parts by weight propylene acid butyl ester monomers, 25 weight parts of styrene monomer, 217 parts by weight of deionized water are joined in reactor, then 125 weight parts of butadiene monomers are added after reactor is airtight, reactor is placed in revolution water bath with thermostatic control, react 26 hours at 65 DEG C, reaction end obtains stratum nucleare copolymer emulsion.
The preparation of rubbery copolymer
100 parts by weight of deionized water are injected 1000ml there-necked flask, then trisodium phosphate 0.4 weight part, glucose 0.6 weight part and ferrous sulfate 0.01 weight part is added successively, potassium hydroxide 0.10 weight part is added again after abundant dissolving, blending emulsifiers 3 weight part of rosin soap lye and fatty acid soaps and stratum nucleare copolymer emulsion 196 weight part, there-necked flask is put into water bath with thermostatic control constant temperature to 65 DEG C, in there-necked flask, pass into nitrogen and stir 10 minutes simultaneously.Take methyl methacrylate monomer 30 weight part, initiator potassium persulfate 0.25 weight part preparation methyl methacrylate drips monomer;
Adopt continuously feeding method that the methyl methacrylate prepared is dripped monomer dropping in there-necked flask, initiator potassium persulfate 0.05 weight part is added before dropping, time for adding is 45 minutes, drip the initiator potassium persulfate terminating to add 0.05 weight part again, react 60 minutes, after reacting completely, cooling, add oxidation inhibitor 2,2 '-methylene-bis (4-methyl-6-tert-butylphenol) 5 weight parts, continue stirring 20 minutes, discharging, add 5 parts sulfuric acid magnesium, can rubbery copolymer be obtained.
The preparation of transparent rubber-modified plexiglass
Take rubbery copolymer 12.86 weight part and PMMA resin 47.14 weight part mixes, HAAKE Banbury mixer carries out melt blending, melting temperature is fixed as 180 DEG C, and mixing time is 5min, can obtain transparent rubber-modified plexiglass.Physical property measured by this transparent resin is as table 1.
Embodiment 2
The preparation of stratum nucleare multipolymer
The blending emulsifiers (weight ratio 1:1) of 150 weight part rosin soap lyes and fatty acid soaps, the tertiary lauryl mercaptan of 1 weight part, 1.27 weight part Potassium Persulphates, 350 parts by weight propylene acid butyl ester monomers, 25 weight parts of styrene monomer, 217 parts by weight of deionized water are joined in reactor, then 125 weight parts of butadiene monomers are added after reactor is airtight, reactor is placed in revolution water bath with thermostatic control, react 26 hours at 65 DEG C, reaction end obtains stratum nucleare copolymer emulsion.
The preparation of rubbery copolymer
100 parts by weight of deionized water are injected 1000ml there-necked flask, then trisodium phosphate 0.4 weight part, glucose 0.6 weight part and ferrous sulfate 0.01 weight part is added successively, potassium hydroxide 0.10 weight part is added again after abundant dissolving, blending emulsifiers 3 weight part of rosin soap lye and fatty acid soaps and stratum nucleare copolymer emulsion 196 weight part, there-necked flask is put into water bath with thermostatic control constant temperature to 65 DEG C, in there-necked flask, pass into nitrogen and stir 10 minutes simultaneously.Take methyl methacrylate monomer 30 weight part, initiator potassium persulfate 0.25 weight part preparation methyl methacrylate drips monomer;
Adopt continuously feeding method that the methyl methacrylate prepared is dripped monomer dropping in there-necked flask, initiator potassium persulfate 0.05 weight part is added before dropping, time for adding is 45 minutes, drip the initiator potassium persulfate terminating to add 0.05 weight part again, react 60 minutes, after reacting completely, cooling, add oxidation inhibitor 2,2 '-methylene-bis (4-methyl-6-tert-butylphenol) 5 weight parts, continue stirring 20 minutes, discharging, add 5 parts sulfuric acid magnesium, can rubbery copolymer be obtained.
The preparation of transparent rubber-modified plexiglass
Take rubbery copolymer 15.43 weight part and PMMA resin 44.57 weight part mixes, HAAKE Banbury mixer carries out melt blending, melting temperature is fixed as 180 DEG C, and mixing time is 5min, can obtain transparent rubber-modified plexiglass.Physical property measured by this transparent resin is as table 1.
Embodiment 3
The preparation of stratum nucleare multipolymer
The blending emulsifiers (weight ratio 1:1) of 150 weight part rosin soap lyes and fatty acid soaps, the tertiary lauryl mercaptan of 1 weight part, 1.27 weight part Potassium Persulphates, 350 parts by weight propylene acid butyl ester monomers, 25 weight parts of styrene monomer, 217 parts by weight of deionized water are joined in reactor, then 125 weight parts of butadiene monomers are added after reactor is airtight, reactor is placed in revolution water bath with thermostatic control, react 26 hours at 65 DEG C, reaction end obtains stratum nucleare copolymer emulsion.
The preparation of rubbery copolymer
100 parts by weight of deionized water are injected 1000ml there-necked flask, then trisodium phosphate 0.4 weight part, glucose 0.6 weight part and ferrous sulfate 0.01 weight part is added successively, potassium hydroxide 0.10 weight part is added again after abundant dissolving, blending emulsifiers 3 weight part of rosin soap lye and fatty acid soaps and stratum nucleare copolymer emulsion 196 weight part, there-necked flask is put into water bath with thermostatic control constant temperature to 65 DEG C, in there-necked flask, pass into nitrogen and stir 10 minutes simultaneously.Take methyl methacrylate monomer 30 weight part, initiator potassium persulfate 0.25 weight part preparation methyl methacrylate drips monomer;
Adopt continuously feeding method that the methyl methacrylate prepared is dripped monomer dropping in there-necked flask, initiator potassium persulfate 0.05 weight part is added before dropping, time for adding is 45 minutes, drip the initiator potassium persulfate terminating to add 0.05 weight part again, react 60 minutes, after reacting completely, cooling, add oxidation inhibitor 2,2 '-methylene-bis (4-methyl-6-tert-butylphenol) 5 weight parts, continue stirring 20 minutes, discharging, add 5 parts sulfuric acid magnesium, can rubbery copolymer be obtained.
The preparation of transparent rubber-modified plexiglass
Take rubbery copolymer 18 weight part and PMMA resin 42 weight part mixes, HAAKE Banbury mixer carries out melt blending, and melting temperature is fixed as 180 DEG C, and mixing time is 5min, can obtain transparent rubber-modified plexiglass.Physical property measured by this transparent resin is as table 1.
Embodiment 4
The preparation of stratum nucleare multipolymer
The blending emulsifiers (weight ratio 1:1) of 150 weight part rosin soap lyes and fatty acid soaps, the tertiary lauryl mercaptan of 1 weight part, 1.27 weight part Potassium Persulphates, 350 parts by weight propylene acid butyl ester monomers, 25 weight parts of styrene monomer, 217 parts by weight of deionized water are joined in reactor, then 125 weight parts of butadiene monomers are added after reactor is airtight, reactor is placed in revolution water bath with thermostatic control, react 26 hours at 65 DEG C, reaction end obtains stratum nucleare copolymer emulsion.
The preparation of rubbery copolymer
100 parts by weight of deionized water are injected 1000ml there-necked flask, then trisodium phosphate 0.4 weight part, glucose 0.6 weight part and ferrous sulfate 0.01 weight part is added successively, potassium hydroxide 0.10 weight part is added again after abundant dissolving, blending emulsifiers 3 weight part of rosin soap lye and fatty acid soaps and stratum nucleare copolymer emulsion 196 weight part, there-necked flask is put into water bath with thermostatic control constant temperature to 65 DEG C, in there-necked flask, pass into nitrogen and stir 10 minutes simultaneously.Take methyl methacrylate monomer 30 weight part, initiator potassium persulfate 0.25 weight part preparation methyl methacrylate drips monomer;
Adopt continuously feeding method that the methyl methacrylate prepared is dripped monomer dropping in there-necked flask, initiator potassium persulfate 0.05 weight part is added before dropping, time for adding is 45 minutes, drip the initiator potassium persulfate terminating to add 0.05 weight part again, react 60 minutes, after reacting completely, cooling, add oxidation inhibitor 2,2 '-methylene-bis (4-methyl-6-tert-butylphenol) 5 weight parts, continue stirring 20 minutes, discharging, add 5 parts sulfuric acid magnesium, can rubbery copolymer be obtained.
The preparation of transparent rubber-modified plexiglass
Take rubbery copolymer 20.57 weight part and PMMA resin 39.43 weight part mixes, HAAKE Banbury mixer carries out melt blending, melting temperature is fixed as 180 DEG C, and mixing time is 5min, can obtain transparent rubber-modified plexiglass.Physical property measured by this transparent resin is as table 1.
Embodiment 5
The preparation of stratum nucleare multipolymer
The blending emulsifiers (weight ratio 1:1) of 150 weight part rosin soap lyes and fatty acid soaps, the tertiary lauryl mercaptan of 1 weight part, 1.27 weight part Potassium Persulphates, 350 parts by weight propylene acid butyl ester monomers, 25 weight parts of styrene monomer, 217 parts by weight of deionized water are joined in reactor, then 125 weight parts of butadiene monomers are added after reactor is airtight, reactor is placed in revolution water bath with thermostatic control, react 26 hours at 65 DEG C, reaction end obtains stratum nucleare copolymer emulsion.
The preparation of rubbery copolymer
100 parts by weight of deionized water are injected 1000ml there-necked flask, then trisodium phosphate 0.4 weight part, glucose 0.6 weight part and ferrous sulfate 0.01 weight part is added successively, potassium hydroxide 0.10 weight part is added again after abundant dissolving, blending emulsifiers 3 weight part of rosin soap lye and fatty acid soaps and stratum nucleare copolymer emulsion 196 weight part, there-necked flask is put into water bath with thermostatic control constant temperature to 65 DEG C, in there-necked flask, pass into nitrogen and stir 10 minutes simultaneously.Take methyl methacrylate monomer 30 weight part, initiator potassium persulfate 0.25 weight part preparation methyl methacrylate drips monomer;
Adopt continuously feeding method that the methyl methacrylate prepared is dripped monomer dropping in there-necked flask, initiator potassium persulfate 0.05 weight part is added before dropping, time for adding is 45 minutes, drip the initiator potassium persulfate terminating to add 0.05 weight part again, react 60 minutes, after reacting completely, cooling, add oxidation inhibitor 2,2 '-methylene-bis (4-methyl-6-tert-butylphenol) 5 weight parts, continue stirring 20 minutes, discharging, add 5 parts sulfuric acid magnesium, can rubbery copolymer be obtained.
The preparation of transparent rubber-modified plexiglass
Take rubbery copolymer 23.14 weight part and PMMA resin 36.86 weight part mixes, HAAKE Banbury mixer carries out melt blending, melting temperature is fixed as 180 DEG C, and mixing time is 5min, can obtain transparent rubber-modified plexiglass.Physical property measured by this transparent resin is as table 1.
Embodiment 6
The preparation of stratum nucleare multipolymer
The blending emulsifiers (weight ratio 1:1) of 300 weight part rosin soap lyes and fatty acid soaps, the tertiary lauryl mercaptan of 1 weight part, 1.27 weight part Potassium Persulphates, 350 parts by weight propylene acid butyl ester monomers, 25 weight parts of styrene monomer, 636 parts by weight of deionized water are joined in reactor, then 125 weight parts of butadiene monomers are added after reactor is airtight, reactor is placed in revolution water bath with thermostatic control, react 26 hours at 65 DEG C, reaction end obtains stratum nucleare copolymer emulsion.
The preparation of rubbery copolymer
100 parts by weight of deionized water are injected 1000ml there-necked flask, then trisodium phosphate 0.4 weight part, glucose 0.6 weight part and ferrous sulfate 0.01 weight part is added successively, potassium hydroxide 0.10 weight part is added again after abundant dissolving, blending emulsifiers 3 weight part of rosin soap lye and fatty acid soaps and stratum nucleare copolymer emulsion 196 weight part, there-necked flask is put into water bath with thermostatic control constant temperature to 65 DEG C, in there-necked flask, pass into nitrogen and stir 10 minutes simultaneously.Take methyl methacrylate monomer 30 weight part, initiator potassium persulfate 0.25 weight part preparation methyl methacrylate drips monomer;
Adopt continuously feeding method that the methyl methacrylate prepared is dripped monomer dropping in there-necked flask, initiator potassium persulfate 0.05 weight part is added before dropping, time for adding is 45 minutes, drip the initiator potassium persulfate terminating to add 0.05 weight part again, react 60 minutes, after reacting completely, cooling, add oxidation inhibitor 2,2 '-methylene-bis (4-methyl-6-tert-butylphenol) 5 weight parts, continue stirring 20 minutes, discharging, add 5 parts sulfuric acid magnesium, can rubbery copolymer be obtained.
The preparation of transparent rubber-modified plexiglass
Take rubbery copolymer 15.43 weight part and PMMA resin 44.57 weight part mixes, HAAKE Banbury mixer carries out melt blending, melting temperature is fixed as 180 DEG C, and mixing time is 5min, can obtain transparent rubber-modified plexiglass.Physical property measured by this transparent resin is as table 1.
Embodiment 7
The preparation of stratum nucleare multipolymer
The blending emulsifiers (weight ratio 1:1) of 150 weight part rosin soap lyes and fatty acid soaps, the tertiary lauryl mercaptan of 1 weight part, 1.27 weight part Potassium Persulphates, 350 parts by weight propylene acid butyl ester monomers, 25 weight parts of styrene monomer, 280 parts by weight of deionized water are joined in reactor, then 125 weight parts of butadiene monomers are added after reactor is airtight, reactor is placed in revolution water bath with thermostatic control, react 26 hours at 65 DEG C, reaction end obtains stratum nucleare copolymer emulsion.
The preparation of rubbery copolymer
100 parts by weight of deionized water are injected 1000ml there-necked flask, then trisodium phosphate 0.4 weight part, glucose 0.6 weight part and ferrous sulfate 0.01 weight part is added successively, potassium hydroxide 0.10 weight part is added again after abundant dissolving, blending emulsifiers 3 weight part of rosin soap lye and fatty acid soaps and stratum nucleare copolymer emulsion 196 weight part, there-necked flask is put into water bath with thermostatic control constant temperature to 65 DEG C, in there-necked flask, pass into nitrogen and stir 10 minutes simultaneously.Take methyl methacrylate monomer 30 weight part, initiator potassium persulfate 0.25 weight part preparation methyl methacrylate drips monomer;
Adopt continuously feeding method that the methyl methacrylate prepared is dripped monomer dropping in there-necked flask, initiator potassium persulfate 0.05 weight part is added before dropping, time for adding is 45 minutes, drip the initiator potassium persulfate terminating to add 0.05 weight part again, react 60 minutes, after reacting completely, cooling, add oxidation inhibitor 2,2 '-methylene-bis (4-methyl-6-tert-butylphenol) 5 weight parts, continue stirring 20 minutes, discharging, add 5 parts sulfuric acid magnesium, can rubbery copolymer be obtained.
The preparation of transparent rubber-modified plexiglass
Take rubbery copolymer 15.43 weight part and PMMA resin 44.57 weight part mixes, HAAKE Banbury mixer carries out melt blending, melting temperature is fixed as 180 DEG C, and mixing time is 5min, can obtain transparent rubber-modified plexiglass.Physical property measured by this transparent resin is as table 1.
Embodiment 8
The preparation of stratum nucleare multipolymer
The blending emulsifiers (weight ratio 1:1) of 150 weight part rosin soap lyes and fatty acid soaps, the tertiary lauryl mercaptan of 1 weight part, 1.27 weight part Potassium Persulphates, 350 parts by weight propylene acid butyl ester monomers, 25 weight parts of styrene monomer, 210 parts by weight of deionized water are joined in reactor, then 125 weight parts of butadiene monomers are added after reactor is airtight, reactor is placed in revolution water bath with thermostatic control, react 26 hours at 65 DEG C, reaction end obtains stratum nucleare copolymer emulsion.
The preparation of rubbery copolymer
100 parts by weight of deionized water are injected 1000ml there-necked flask, then trisodium phosphate 0.4 weight part, glucose 0.6 weight part and ferrous sulfate 0.01 weight part is added successively, potassium hydroxide 0.10 weight part is added again after abundant dissolving, blending emulsifiers 3 weight part of rosin soap lye and fatty acid soaps and stratum nucleare copolymer emulsion 196 weight part, there-necked flask is put into water bath with thermostatic control constant temperature to 65 DEG C, in there-necked flask, pass into nitrogen and stir 10 minutes simultaneously.Take methyl methacrylate monomer 30 weight part, initiator potassium persulfate 0.25 weight part preparation methyl methacrylate drips monomer;
Adopt continuously feeding method that the methyl methacrylate prepared is dripped monomer dropping in there-necked flask, initiator potassium persulfate 0.05 weight part is added before dropping, time for adding is 45 minutes, drip the initiator potassium persulfate terminating to add 0.05 weight part again, react 60 minutes, after reacting completely, cooling, add oxidation inhibitor 2,2 '-methylene-bis (4-methyl-6-tert-butylphenol) 5 weight parts, continue stirring 20 minutes, discharging, add 5 parts sulfuric acid magnesium, can rubbery copolymer be obtained.
The preparation of transparent rubber-modified plexiglass
Take rubbery copolymer 15.43 weight part and PMMA resin 44.57 weight part mixes, HAAKE Banbury mixer carries out melt blending, melting temperature is fixed as 180 DEG C, and mixing time is 5min, can obtain transparent rubber-modified plexiglass.Physical property measured by this transparent resin is as table 1.
Embodiment 9
The preparation of stratum nucleare multipolymer
The blending emulsifiers (weight ratio 1:1) of 150 weight part rosin soap lyes and fatty acid soaps, the tertiary lauryl mercaptan of 1 weight part, 1.27 weight part Potassium Persulphates, 300 parts by weight propylene acid butyl ester monomers, 25 weight parts of styrene monomer, 217 parts by weight of deionized water are joined in reactor, then 175 weight parts of butadiene monomers are added after reactor is airtight, reactor is placed in revolution water bath with thermostatic control, react 26 hours at 65 DEG C, reaction end obtains stratum nucleare copolymer emulsion.
The preparation of rubbery copolymer
100 parts by weight of deionized water are injected 1000ml there-necked flask, then trisodium phosphate 0.4 weight part, glucose 0.6 weight part and ferrous sulfate 0.01 weight part is added successively, potassium hydroxide 0.10 weight part is added again after abundant dissolving, blending emulsifiers 3 weight part of rosin soap lye and fatty acid soaps and stratum nucleare copolymer emulsion 196 weight part, there-necked flask is put into water bath with thermostatic control constant temperature to 65 DEG C, in there-necked flask, pass into nitrogen and stir 10 minutes simultaneously.Take methyl methacrylate monomer 30 weight part, initiator potassium persulfate 0.25 weight part preparation methyl methacrylate drips monomer;
Adopt continuously feeding method that the methyl methacrylate prepared is dripped monomer dropping in there-necked flask, initiator potassium persulfate 0.05 weight part is added before dropping, time for adding is 45 minutes, drip the initiator potassium persulfate terminating to add 0.05 weight part again, react 60 minutes, after reacting completely, cooling, add oxidation inhibitor 2,2 '-methylene-bis (4-methyl-6-tert-butylphenol) 5 weight parts, continue stirring 20 minutes, discharging, add 5 parts sulfuric acid magnesium, can rubbery copolymer be obtained.
The preparation of transparent rubber-modified plexiglass
Take rubbery copolymer 15.43 weight part and PMMA resin 44.57 weight part mixes, HAAKE Banbury mixer carries out melt blending, melting temperature is fixed as 180 DEG C, and mixing time is 5min, can obtain transparent rubber-modified plexiglass.Physical property measured by this transparent resin is as table 1.
Embodiment 10
The preparation of stratum nucleare multipolymer
The blending emulsifiers (weight ratio 1:1) of 150 weight part rosin soap lyes and fatty acid soaps, the tertiary lauryl mercaptan of 1 weight part, 1.27 weight part Potassium Persulphates, 325 parts by weight propylene acid butyl ester monomers, 25 weight parts of styrene monomer, 217 parts by weight of deionized water are joined in reactor, then 125 weight parts of butadiene monomers are added after reactor is airtight, reactor is placed in revolution water bath with thermostatic control, react 26 hours at 65 DEG C, reaction end obtains stratum nucleare copolymer emulsion.
The preparation of rubbery copolymer
100 parts by weight of deionized water are injected 1000ml there-necked flask, then trisodium phosphate 0.4 weight part, glucose 0.6 weight part and ferrous sulfate 0.01 weight part is added successively, potassium hydroxide 0.10 weight part is added again after abundant dissolving, blending emulsifiers 3 weight part of rosin soap lye and fatty acid soaps and stratum nucleare copolymer emulsion 196 weight part, there-necked flask is put into water bath with thermostatic control constant temperature to 65 DEG C, in there-necked flask, pass into nitrogen and stir 10 minutes simultaneously.Take methyl methacrylate monomer 30 weight part, initiator potassium persulfate 0.25 weight part preparation methyl methacrylate drips monomer;
Adopt continuously feeding method that the methyl methacrylate prepared is dripped monomer dropping in there-necked flask, initiator potassium persulfate 0.05 weight part is added before dropping, time for adding is 45 minutes, drip the initiator potassium persulfate terminating to add 0.05 weight part again, react 60 minutes, after reacting completely, cooling, add oxidation inhibitor 2,2 '-methylene-bis (4-methyl-6-tert-butylphenol) 5 weight parts, continue stirring 20 minutes, discharging, add 5 parts sulfuric acid magnesium, can rubbery copolymer be obtained.
The preparation of transparent rubber-modified plexiglass
Take rubbery copolymer 15.43 weight part and PMMA resin 44.57 weight part mixes, HAAKE Banbury mixer carries out melt blending, melting temperature is fixed as 180 DEG C, and mixing time is 5min, can obtain transparent rubber-modified plexiglass.Physical property measured by this transparent resin is as table 1.
Embodiment 11
The preparation of stratum nucleare multipolymer
The blending emulsifiers (weight ratio 1:1) of 150 weight part rosin soap lyes and fatty acid soaps, the tertiary lauryl mercaptan of 1 weight part, 1.27 weight part Potassium Persulphates, 375 parts by weight propylene acid butyl ester monomers, 25 weight parts of styrene monomer, 217 parts by weight of deionized water are joined in reactor, then 100 weight parts of butadiene monomers are added after reactor is airtight, reactor is placed in revolution water bath with thermostatic control, react 26 hours at 65 DEG C, reaction end obtains stratum nucleare copolymer emulsion.
The preparation of rubbery copolymer
100 parts by weight of deionized water are injected 1000ml there-necked flask, then trisodium phosphate 0.4 weight part, glucose 0.6 weight part and ferrous sulfate 0.01 weight part is added successively, potassium hydroxide 0.10 weight part is added again after abundant dissolving, blending emulsifiers 3 weight part of rosin soap lye and fatty acid soaps and stratum nucleare copolymer emulsion 196 weight part, there-necked flask is put into water bath with thermostatic control constant temperature to 65 DEG C, in there-necked flask, pass into nitrogen and stir 10 minutes simultaneously.Take methyl methacrylate monomer 30 weight part, initiator potassium persulfate 0.25 weight part preparation methyl methacrylate drips monomer;
Adopt continuously feeding method that the methyl methacrylate prepared is dripped monomer dropping in there-necked flask, initiator potassium persulfate 0.05 weight part is added before dropping, time for adding is 45 minutes, drip the initiator potassium persulfate terminating to add 0.05 weight part again, react 60 minutes, after reacting completely, cooling, add oxidation inhibitor 2,2 '-methylene-bis (4-methyl-6-tert-butylphenol) 5 weight parts, continue stirring 20 minutes, discharging, add 5 parts sulfuric acid magnesium, can rubbery copolymer be obtained.
The preparation of transparent rubber-modified plexiglass
Take rubbery copolymer 15.43 weight part and PMMA resin 44.57 weight part mixes, HAAKE Banbury mixer carries out melt blending, melting temperature is fixed as 180 DEG C, and mixing time is 5min, can obtain transparent rubber-modified plexiglass.Physical property measured by this transparent resin is as table 1.
Embodiment 12
The preparation of stratum nucleare multipolymer
The blending emulsifiers (weight ratio 1:1) of 150 weight part rosin soap lyes and fatty acid soaps, the tertiary lauryl mercaptan of 1 weight part, 1.27 weight part Potassium Persulphates, 350 parts by weight propylene acid butyl ester monomers, 25 weight parts of styrene monomer, 217 parts by weight of deionized water are joined in reactor, then 125 weight parts of butadiene monomers are added after reactor is airtight, reactor is placed in revolution water bath with thermostatic control, react 26 hours at 65 DEG C, reaction end obtains stratum nucleare copolymer emulsion.
The preparation of rubbery copolymer
100 parts by weight of deionized water are injected 1000ml there-necked flask, then trisodium phosphate 0.4 weight part, glucose 0.6 weight part and ferrous sulfate 0.01 weight part is added successively, potassium hydroxide 0.10 weight part is added again after abundant dissolving, blending emulsifiers 3 weight part of rosin soap lye and fatty acid soaps and stratum nucleare copolymer emulsion 168 weight part, there-necked flask is put into water bath with thermostatic control constant temperature to 65 DEG C, in there-necked flask, pass into nitrogen and stir 10 minutes simultaneously.Take methyl methacrylate monomer 40 weight part, initiator potassium persulfate 0.35 weight part preparation methyl methacrylate drips monomer;
Adopt continuously feeding method that the methyl methacrylate prepared is dripped monomer dropping in there-necked flask, initiator potassium persulfate 0.05 weight part is added before dropping, time for adding is 60 minutes, drip the initiator potassium persulfate terminating to add 0.05 weight part again, react 60 minutes, after reacting completely, cooling, add oxidation inhibitor 2,2 '-methylene-bis (4-methyl-6-tert-butylphenol) 5 weight parts, continue stirring 20 minutes, discharging, add 5 parts sulfuric acid magnesium, can rubbery copolymer be obtained.
The preparation of transparent rubber-modified plexiglass
Take rubbery copolymer 15.43 weight part and PMMA resin 44.57 weight part mixes, HAAKE Banbury mixer carries out melt blending, melting temperature is fixed as 180 DEG C, and mixing time is 5min, can obtain transparent rubber-modified plexiglass.Physical property measured by this transparent resin is as table 1.
Embodiment 13
The preparation of stratum nucleare multipolymer
The blending emulsifiers (weight ratio 1:1) of 150 weight part rosin soap lyes and fatty acid soaps, the tertiary lauryl mercaptan of 1 weight part, 1.27 weight part Potassium Persulphates, 350 parts by weight propylene acid butyl ester monomers, 25 weight parts of styrene monomer, 217 parts by weight of deionized water are joined in reactor, then 125 weight parts of butadiene monomers are added after reactor is airtight, reactor is placed in revolution water bath with thermostatic control, react 26 hours at 65 DEG C, reaction end obtains stratum nucleare copolymer emulsion.
The preparation of rubbery copolymer
100 parts by weight of deionized water are injected 1000ml there-necked flask, then trisodium phosphate 0.4 weight part, glucose 0.6 weight part and ferrous sulfate 0.01 weight part is added successively, potassium hydroxide 0.10 weight part is added again after abundant dissolving, blending emulsifiers 3 weight part of rosin soap lye and fatty acid soaps and stratum nucleare copolymer emulsion 223 weight part, there-necked flask is put into water bath with thermostatic control constant temperature to 65 DEG C, in there-necked flask, pass into nitrogen and stir 10 minutes simultaneously.Take methyl methacrylate monomer 20 weight part, initiator potassium persulfate 0.20 weight part preparation methyl methacrylate drips monomer;
Adopt continuously feeding method that the methyl methacrylate prepared is dripped monomer dropping in there-necked flask, initiator potassium persulfate 0.05 weight part is added before dropping, time for adding is 30 minutes, drip the initiator potassium persulfate terminating to add 0.05 weight part again, react 60 minutes, after reacting completely, cooling, add oxidation inhibitor 2,2 '-methylene-bis (4-methyl-6-tert-butylphenol) 5 weight parts, continue stirring 20 minutes, discharging, add 5 parts sulfuric acid magnesium, can rubbery copolymer be obtained.
The preparation of transparent rubber-modified plexiglass
Take rubbery copolymer 15.43 weight part and PMMA resin 44.57 weight part mixes, HAAKE Banbury mixer carries out melt blending, melting temperature is fixed as 180 DEG C, and mixing time is 5min, can obtain transparent rubber-modified plexiglass.Physical property measured by this transparent resin is as table 1.
Embodiment 14
The preparation of stratum nucleare multipolymer
The blending emulsifiers (weight ratio 1:1) of 150 weight part rosin soap lyes and fatty acid soaps, the tertiary lauryl mercaptan of 1 weight part, 1.27 weight part Potassium Persulphates, 350 parts by weight propylene acid butyl ester monomers, 25 weight parts of styrene monomer, 217 parts by weight of deionized water are joined in reactor, then 125 weight parts of butadiene monomers are added after reactor is airtight, reactor is placed in revolution water bath with thermostatic control, react 26 hours at 65 DEG C, reaction end obtains stratum nucleare copolymer emulsion.
The preparation of rubbery copolymer
100 parts by weight of deionized water are injected 1000ml there-necked flask, then trisodium phosphate 0.4 weight part, glucose 0.6 weight part and ferrous sulfate 0.01 weight part is added successively, potassium hydroxide 0.10 weight part is added again after abundant dissolving, blending emulsifiers 3 weight part of rosin soap lye and fatty acid soaps and stratum nucleare copolymer emulsion 251 weight part, there-necked flask is put into water bath with thermostatic control constant temperature to 65 DEG C, in there-necked flask, pass into nitrogen and stir 10 minutes simultaneously.Take methyl methacrylate monomer 10 weight part, initiator potassium persulfate 0.10 weight part preparation methyl methacrylate drips monomer;
Adopt continuously feeding method that the methyl methacrylate prepared is dripped monomer dropping in there-necked flask, initiator potassium persulfate 0.05 weight part is added before dropping, time for adding is 15 minutes, drip the initiator potassium persulfate terminating to add 0.05 weight part again, react 60 minutes, after reacting completely, cooling, add oxidation inhibitor 2,2 '-methylene-bis (4-methyl-6-tert-butylphenol) 5 weight parts, continue stirring 20 minutes, discharging, add 5 parts sulfuric acid magnesium, can rubbery copolymer be obtained.
The preparation of transparent rubber-modified plexiglass
Take rubbery copolymer 15.43 weight part and PMMA resin 44.57 weight part mixes, HAAKE Banbury mixer carries out melt blending, melting temperature is fixed as 180 DEG C, and mixing time is 5min, can obtain transparent rubber-modified plexiglass.Physical property measured by this transparent resin is as table 1.
Table 1
The foregoing is only the several better possible embodiments of the present invention, all technician being familiar with this, its modification done according to scope of the present invention or change, all ought to be included within the scope of technical solution of the present invention.
Claims (10)
1. a transparent rubber-modified plexiglass composition, is characterized in that, according to parts by weight, comprising:
Rubbery copolymer 12-23.14 weight part and PMMA matrix resin 48-36.86 weight part;
Described rubbery copolymer, according to parts by weight, comprising: stratum nucleare multipolymer 20-80 weight part and sheath polymers 80-20 weight part;
Described stratum nucleare multipolymer, according to parts by weight, comprising: Butyl Acrylate Monomer 60-75 weight part, divinylic monomer 20-40 weight part and styrene monomer 0-10 weight part;
Described sheath polymers is polymethylmethacrylate.
2. the transparent rubber-modified plexiglass composition of one according to claim 1, it is characterized in that, the preparation method of described rubbery copolymer, comprising:
Deionized water is injected there-necked flask, then trisodium phosphate, glucose and ferrous sulfate is added successively, potassium hydroxide is added again after abundant dissolving, emulsifying agent and stratum nucleare multipolymer, there-necked flask is put into water bath with thermostatic control constant temperature to 60-70 DEG C, in there-necked flask, pass into nitrogen and stir 10-20 minute simultaneously, taking methyl methacrylate monomer and initiator preparation methyl methacrylate dropping monomer;
Adopt continuously feeding method that the methyl methacrylate prepared is dripped monomer dropping in there-necked flask, add initiator before dropping, time for adding is 10-60 minute, drips and terminates to add initiator again, reaction 30-90 minute, after reacting completely, cool to 60 DEG C, add oxidation inhibitor, continue to stir 1-30 minute, discharging, adds flocculation agent, can obtain rubbery copolymer.
3. the transparent rubber-modified plexiglass composition of one according to claim 2, is characterized in that, the preparation method of described stratum nucleare multipolymer, comprising:
Emulsifying agent, molecular weight regulator, initiator, Butyl Acrylate Monomer, styrene monomer and water are joined in reactor, then divinylic monomer is added after reactor is airtight, reactor is placed in revolution water bath with thermostatic control and carries out polyreaction, and reaction end obtains butyl acrylate/Butadiene/Styrene latex.
4. the transparent rubber-modified plexiglass composition of one according to claim 2, is characterized in that, described emulsifying agent is the blending emulsifiers of rosin soap lye and fatty acid soaps.
5. the transparent rubber-modified plexiglass composition of one according to claim 4, is characterized in that, described rosin soap lye and the weight ratio of fatty acid soaps are 1:1.
6. the transparent rubber-modified plexiglass composition of one according to claim 2, it is characterized in that, described initiator comprises Potassium Persulphate or Ammonium Persulfate 98.5.
7. the transparent rubber-modified plexiglass composition of one according to claim 2, it is characterized in that, described oxidation inhibitor comprises β-(4-hydroxyl-3,5-di-tert-butyl-phenyl) the positive octadecyl ester of propionic acid or 2,2 '-methylene-bis (4-methyl-6-tert-butylphenol).
8. the transparent rubber-modified plexiglass composition of one according to claim 2, it is characterized in that, described flocculation agent is selected from one or more in sulfuric acid, hydrochloric acid, phosphoric acid, acetic acid, calcium chloride, magnesium chloride, bariumchloride, aluminum chloride, magnesium sulfate or Tai-Ace S 150.
9. the preparation method of a kind of transparent rubber modified thenylethylene resin according to claim 1, it is characterized in that, comprise: take rubbery copolymer and PMMA matrix resin carries out melt blending, transparent rubber-modified plexiglass composition can be obtained.
10. the preparation method of a kind of transparent rubber modified thenylethylene resin according to claim 9, is characterized in that, described melt blending temperature is 170-180 DEG C, and the melt blending time is 5-10 minute.
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| CN109456440B (en) * | 2018-09-27 | 2020-08-28 | 科邦石化(连云港)有限公司 | Modified acrylate material and preparation method thereof |
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| WO2021008321A1 (en) * | 2019-07-12 | 2021-01-21 | 金发科技股份有限公司 | Polyacrylate polymer composite material and preparation method therefor |
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