CN103980427A - Polyvinyl chloride transparent toughening modifier and preparation method thereof - Google Patents
Polyvinyl chloride transparent toughening modifier and preparation method thereof Download PDFInfo
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- CN103980427A CN103980427A CN201410216401.0A CN201410216401A CN103980427A CN 103980427 A CN103980427 A CN 103980427A CN 201410216401 A CN201410216401 A CN 201410216401A CN 103980427 A CN103980427 A CN 103980427A
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Abstract
The invention provides a polyvinyl chloride transparent toughening modifier and a preparation method thereof, and belongs to the field of high polymer materials. The method comprises the following steps: firstly, synthesizing to obtain an SBR (Styrene Butadiene Rubber) or PB (polybutylene) seed emulsion by an emulsion polymerization method, and then grafting butyl acrylate and styrene on the SBR or PB seed emulsion by the emulsion polymerization method, so as to obtain the polyvinyl chloride transparent toughening modifier with a three-layer core-shell structure. Compared with the prior art, the polyvinyl chloride transparent toughening modifier is simple in preparation method and low in cost. The experiment result proves that the impact strength of the modified polyvinyl chloride can be up to 1200J/m, a spline is in ductile fracture, the impact strength of the modified polyvinyl chloride is improved by over 20 times in comparison with that of a pure polyvinyl chloride material, and meanwhile, good transparency of a blend can be ensured.
Description
Technical field
The invention belongs to polymeric material field, be specifically related to a kind of transparent polyvinyl chloride toughening modifier and preparation method thereof.
Background technology
Polyvinyl chloride (PVC) is have the over-all propertieies such as good rigidity, erosion resistance, electric insulating quality and cheap price and be widely used in every field, and its output occupies second in macromolecular material.Its shortcoming is that shock resistance is poor, and matter is crisp, thermostability and poor in processability.For overcoming these shortcomings, expand the commercial use of PVC, the study on the modification of polyvinyl chloride has been carried out decades, and obtained obvious achievement, really make polyvinyl chloride become more general-purpose plastics of one, oneself has brought into play vital role in industry, building, the field such as civilian.
The properties-correcting agent that polyvinyl chloride is carried out to impact modification generally adopts the copolymer elastomer that second-order transition temperature is lower and good with polyvinyl chloride consistency, as perbutan (NBR) or taking the lower elastomerics of second-order transition temperature as basis, in grafting, form nucleocapsid structure properties-correcting agent with the good top layer of body material consistency again, as acrylic acid or the like nucleocapsid properties-correcting agent (AIM), butadiene-styrene-methyl methacrylate ternary graft copolymer (MBS) properties-correcting agent.Traditional MBS nucleocapsid toughner polymerization process (publication number CN101139425A) all adopts using styrene-butadiene latex or butadiene latex as seed emulsion, the rigidity such as graft phenylethene and methyl methacrylate monomer thereon.But in the method, do not have to describe composition and the constitutional features based on changing nucleocapsid properties-correcting agent, the polyvinyl chloride shock strength after modification is not significantly improved.
Summary of the invention
The object of this invention is to provide a kind of transparent polyvinyl chloride toughening modifier and preparation method thereof, the modifier modification polyvinyl chloride obtaining by the method has excellent shock resistance and good light transmission.
First the present invention provides a kind of preparation method of transparent polyvinyl chloride toughening modifier, comprises the steps:
Step 1: according to parts by weight meter, in reaction vessel, add 0-50 parts by weight of styrene, 50-100 weight parts of butadiene, 0.1-1 weight part initiator, 2-10 weight part emulsifying agent and 100-300 parts by weight of deionized water, under nitrogen protection, polyreaction 12-24 hour at 50-85 DEG C, is gathered (styrene butadiene) (SBR) or polyhutadiene (PB) seed emulsion;
Step 2: according to parts by weight meter; in reaction vessel, add the 40-90 weight part that step 1 obtains to gather (styrene butadiene) (SBR) or polyhutadiene (PB) seed emulsion, 5-60 parts by weight of acrylic acid butyl ester, 5-55 parts by weight of styrene, 0.1-1 weight part initiator, 2-10 weight part emulsifying agent and 80-300 parts by weight of deionized water; under nitrogen protection; polyreaction 2-6 hour at 50-85 DEG C; add 0.5-2 part antioxidant; filter; cohesion; dry, obtain transparent polyvinyl chloride toughening modifier.
Preferably, the emulsifying agent of described step 1 is selected from one or more in potassium oleate, potassium stearate, nilox resin acid potassium or Sodium dodecylbenzene sulfonate.
Preferably, the initiator of described step 1 is Potassium Persulphate, benzoyl peroxide, Diisopropyl azodicarboxylate or di-isopropylbenzene hydroperoxide-ferrous sulfate.
Preferably, the temperature of reaction of described step 1 is 65 DEG C, and the reaction times is 22h.
Preferably, the emulsifying agent of described step 2 is selected from one or more in potassium oleate, potassium stearate, nilox resin acid potassium or Sodium dodecylbenzene sulfonate.
Preferably, the initiator of described step 2 is Potassium Persulphate, benzoyl peroxide, Diisopropyl azodicarboxylate or di-isopropylbenzene hydroperoxide-ferrous sulfate.
Preferably, the temperature of reaction of described step 2 is 70 DEG C, and the reaction times is 5h.
The transparent polyvinyl chloride toughening modifier that the present invention also provides above-mentioned preparation method to obtain.
Beneficial effect of the present invention
First the present invention provides a kind of preparation method of transparent polyvinyl chloride toughening modifier, the method is first synthesized and is obtained SBR or PB seed emulsion by emulsion polymerization, then in SBR or PB seed emulsion, pass through emulsion polymerization grafted propylene acid butyl ester and vinylbenzene, obtain the transparent polyvinyl chloride toughening modifier of three-layer nuclear shell structure.Compare with prior art, preparation method of the present invention is simple, cost is low, and the transparent polyvinyl chloride toughening modifier obtaining by the method has excellent shock resistance and good light transmission.
The transparent polyvinyl chloride toughening modifier that the present invention also provides above-mentioned preparation method to obtain, according to the cantilever beam impact strength value of ASTM-D256 standard testing toughened modified polyvinyl chloride batten, experimental result shows: the polyvinyl chloride impact hit intensity after modification can reach 1200J/m, batten is ductile rupture, shock strength improves more than 20 times than pure pvc material, can ensure that blend has good light transmission simultaneously.
Embodiment
First the present invention provides a kind of preparation method of transparent polyvinyl chloride toughening modifier, comprises the steps:
Step 1: according to parts by weight meter, in reaction vessel, add 0-50 parts by weight of styrene, 50-100 weight parts of butadiene, 0.1-1 weight part initiator, 2-10 weight part emulsifying agent and 100-300 parts by weight of deionized water, under nitrogen protection, polyreaction 12-24 hour at 50-85 DEG C, is gathered (styrene butadiene) (SBR) or polyhutadiene (PB) seed emulsion;
Step 2: according to parts by weight meter; in reaction vessel, add the 40-90 weight part that step 1 obtains to gather (styrene butadiene) (SBR) or polyhutadiene (PB) seed emulsion, 5-60 parts by weight of acrylic acid butyl ester, 5-55 parts by weight of styrene, 0.1-1 weight part initiator, 2-10 weight part emulsifying agent and 80-300 parts by weight of deionized water; under nitrogen protection; polyreaction 2-6 hour at 50-85 DEG C DEG C; add 0.5-2 part antioxidant; filter; cohesion; dry, obtain transparent polyvinyl chloride toughening modifier.
According to the present invention, step 1 is first prepared SBR or PB seed emulsion by emulsion polymerization, and the emulsifying agent of described step 1 is preferably selected from one or more in potassium oleate, potassium stearate, nilox resin acid potassium or Sodium dodecylbenzene sulfonate; Initiator is preferably Potassium Persulphate, benzoyl peroxide, Diisopropyl azodicarboxylate or di-isopropylbenzene hydroperoxide-ferrous sulfate.The temperature of reaction of step 1 is preferably 65 DEG C, and the reaction times is preferably 22h.
According to the present invention, obtain after SBR or PB seed emulsion, in SBR or PB seed emulsion by emulsion polymerization grafted propylene acid butyl ester and vinylbenzene as increase-volume segment, the PVC blend that is beneficial to improve institute's modification has the very high transparency and impelling strength.Preferably first butyl acrylate and styrene monomer are mixed, and then add in reaction vessel.Described vinylbenzene plays the effect that regulates plasticized modifier refractive index in plasticized modifier, is beneficial to prepare the PVC blend of high transparent and the effect that keeps core-shell polymer powder characteristics; Described butyl acrylate plays and improves and the effect of PVC consistency in plasticized modifier, is beneficial to the good dispersion of plasticized modifier in PVC matrix, and the effect that jointly improves the shock strength of PVC blend with core rubber phase.
According to the present invention, the emulsifying agent in described step 2 can with step 1 in emulsifying agent identical or different, be preferably selected from one or more in potassium oleate, potassium stearate, nilox resin acid potassium or Sodium dodecylbenzene sulfonate; Initiator in described step 2 can with step 1 in initiator identical or different, be preferably Potassium Persulphate, ammonium persulphate, benzoyl peroxide, Diisopropyl azodicarboxylate or di-isopropylbenzene hydroperoxide-ferrous sulfate; Described antioxidant is preferably phenolic antioxidant; The temperature of reaction of described step 2 is preferably 70 DEG C, and the reaction times is preferably 5h.
The transparent polyvinyl chloride toughening modifier that the present invention also provides above-mentioned preparation method to obtain.
By transparent polyvinyl chloride toughening modifier obtained above and polychloroethylene blended, prepare polyvinyl chloride blend, step and condition are as follows: take polyvinyl chloride 100 weight parts, organotin 2 weight parts, transparent polyvinyl chloride toughening modifier 6-8 weight part, fully mix and make it dispersed, on double roll mill at 180 DEG C mixing 5 minutes, obtain toughened modified polyvinyl chloride sheet material, then hot pressing moulding at 180 DEG C on vulcanizing press, carry out shock resistance test (according to ASTM-D256 standard) and light transmission test (according to GB2410-80 standard).
Below in conjunction with specific embodiment, the present invention is done to further detailed description.The raw material relating in embodiment is commercially available.
Embodiment 1
Being equipped with in the high-pressure reactor of agitator, condensing works, pass into nitrogen protection, 65 DEG C of constant temperature, add 100 parts of deionized waters, 2 parts of nilox resin acid potassium, 100 parts of divinylic monomers, 0.1 part of Potassium Persulphate, stir polymerization 22 hours, transformation efficiency is 98%, obtains PB seed emulsion;
After above-mentioned reaction finishes, in reactor, add 40 parts of PB seed emulsion, be warming up to 70 DEG C, then add 0.05 part of Potassium Persulphate initiator, 2 parts of nilox resin acid potassium, in 2h, constant speed adds St and BA mix monomer, 5 parts of St monomers, 5 parts of BA monomers, after dropping finishes, add 0.05 part of Potassium Persulphate, continue reaction 5h, add 1 part of phenol antioxidant, after 0.5h, condense, washing, dry, obtain transparent polyvinyl chloride toughening modifier.
Take 100 parts of polyvinyl chloride, 2 parts of organotins, add respectively transparent polyvinyl chloride toughening modifier 6-8 part, carry out fully mixing and making it dispersed, on double roll mill at 180 DEG C mixing 5 minutes, obtain polyvinyl chloride blend sheet material.Then hot pressing moulding at 180 DEG C on vulcanizing press, according to the cantilever beam impact strength value of ASTM-D256 canonical measure toughened modified polyvinyl chloride batten, transmittance is according to GB2410-80, thickness of sample 1.3mm, specific performance test result is in table 1.
Embodiment 2
Being equipped with in the high-pressure reactor of agitator, condensing works, pass into nitrogen protection, 85 DEG C of constant temperature, add 300 parts of deionized waters, 10 parts of potassium oleates, 50 parts of styrene monomers, 50 parts of divinylic monomers, 1 part of Potassium Persulphate, stir polymerization 12 hours, transformation efficiency is 98%, obtains SBR seed emulsion;
After above-mentioned reaction finishes, in reactor, add 90 parts of SBR seed emulsion, be warming up to 85 DEG C, then add 0.5 part of Potassium Persulphate initiator, 10 parts of potassium oleates, in 2h, constant speed adds St and BA mix monomer, 55 parts of St monomers, 60 parts of BA monomers, after dropping finishes, add 0.5 part of Potassium Persulphate, continue reaction 2h, add 0.5 part of phenol antioxidant, after 0.5h, condense, washing, dry, obtain transparent polyvinyl chloride toughening modifier.
The testing method of the properties-correcting agent that embodiment 2 obtains is with embodiment 1, and specific performance test result is in table 1.
Embodiment 3
Being equipped with in the high-pressure reactor of agitator, condensing works, pass into nitrogen protection, 50 DEG C of constant temperature, add 200 parts of deionized waters, 6 parts of potassium stearates, 25 parts of styrene monomers, 75 parts of divinylic monomers, 0.5 part of benzoyl peroxide, stirs polymerization 24 hours, transformation efficiency is 98%, obtains SBR seed emulsion;
After above-mentioned reaction finishes, in reactor, add 70 parts of SBR seed emulsion, be warming up to 50 DEG C, then add 0.25 part of benzoyl peroxide initiator, 6 parts of potassium stearates, in 2h, constant speed adds St and BA mix monomer, 30 parts of St monomers, 35 parts of BA monomers, after dropping finishes, add 0.25 part of benzoyl peroxide, continue reaction 6h, add 2 parts of phenol antioxidant, after 0.5h, condense, washing, dry, obtain transparent polyvinyl chloride toughening modifier.
The testing method of the properties-correcting agent that embodiment 3 obtains is with embodiment 1, and specific performance test result is in table 1.
Embodiment 4
Being equipped with in the high-pressure reactor of agitator, condensing works, pass into nitrogen protection, 65 DEG C of constant temperature, add 150 parts of deionized waters, 4 parts of potassium stearates, 20 parts of styrene monomers, 80 parts of divinylic monomers, 0.4 part of Diisopropyl azodicarboxylate, stirs polymerization 24 hours, transformation efficiency is 98%, obtains SBR seed emulsion;
After above-mentioned reaction finishes, in reactor, add 60 parts of SBR seed emulsion, be warming up to 70 DEG C, then add 0.2 part of Diisopropyl azodicarboxylate initiator, 4 parts of potassium stearates, in 2h, constant speed adds St and BA mix monomer, 25 parts of St monomers, 30 parts of BA monomers, after dropping finishes, add 0.2 part of Diisopropyl azodicarboxylate, continue reaction 3h, add 1 part of phenol antioxidant, after 0.5h, condense, washing, dry, obtain transparent polyvinyl chloride toughening modifier.
The testing method of the properties-correcting agent that embodiment 4 obtains is with embodiment 1, and specific performance test result is in table 1.
Embodiment 5
Being equipped with in the high-pressure reactor of agitator, condensing works, pass into nitrogen protection, 65 DEG C of constant temperature, add 250 parts of deionized waters, 8 parts of Sodium dodecylbenzene sulfonatees, 40 parts of styrene monomers, 60 parts of divinylic monomers, 0.7 part of di-isopropylbenzene hydroperoxide-ferrous sulfate, stirs polymerization 20 hours, transformation efficiency is 98%, obtains SBR seed emulsion;
After above-mentioned reaction finishes, in reactor, add 80 parts of SBR seed emulsion, be warming up to 70 DEG C, then add 0.35 part of di-isopropylbenzene hydroperoxide-ferrous sulfate initiator, 8 parts of Sodium dodecylbenzene sulfonatees, in 2h, constant speed adds St and BA mix monomer, 40 parts of St monomers, 50 parts of BA monomers, after dropping finishes, add 0.35 part of di-isopropylbenzene hydroperoxide-ferrous sulfate, continue reaction 2h, add 1 part of phenol antioxidant, after 0.5h, condense, washing, dry, obtain transparent polyvinyl chloride toughening modifier.
The testing method of the properties-correcting agent that embodiment 5 obtains is with embodiment 1, and specific performance test result is in table 1.
Embodiment 6
Being equipped with in the high-pressure reactor of agitator, condensing works, pass into nitrogen protection, 65 DEG C of constant temperature, add 250 parts of deionized waters, 7 parts of nilox resin acid potassium, 40 parts of styrene monomers, 60 parts of divinylic monomers, 0.7 part of Potassium Persulphate, stirs polymerization 20 hours, transformation efficiency is 98%, obtains SBR seed emulsion;
After above-mentioned reaction finishes, in reactor, add 80 parts of SBR seed emulsion, be warming up to 65 DEG C, then add 0.35 part of Potassium Persulphate initiator, 7 parts of nilox resin acid potassium, in 2h, constant speed adds St and BA mix monomer, 45 parts of St monomers, 55 parts of BA monomers, after dropping finishes, add 0.35 part of Potassium Persulphate, continue reaction 3h, add 1 part of phenol antioxidant, after 0.5h, condense, washing, dry, obtain transparent polyvinyl chloride toughening modifier.
The testing method of the properties-correcting agent that embodiment 6 obtains is with embodiment 1, and specific performance test result is in table 1.
Table 1
Experimental result shows, at 23 DEG C, testing pure polyvinyl chloride cantilever beam impact strength value according to ASTM-D256 standard is 55J/m, be brittle rupture, polyvinyl chloride impact hit intensity after modification of the present invention can reach 1200J/m, batten is ductile rupture, shock strength improves more than 20 times than pure pvc material, can ensure that blend has good light transmission simultaneously.
The explanation of above embodiment is just for helping to understand method of the present invention and core concept thereof.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of the claims in the present invention.
To the above-mentioned explanation of the disclosed embodiments, make professional and technical personnel in the field can realize or use the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiment, General Principle as defined herein can, in the situation that not departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (8)
1. a preparation method for transparent polyvinyl chloride toughening modifier, is characterized in that, comprises the steps:
Step 1: according to parts by weight meter, in reaction vessel, add 0-50 parts by weight of styrene, 50-100 weight parts of butadiene, 0.1-1 weight part initiator, 2-10 weight part emulsifying agent and 100-300 parts by weight of deionized water, under nitrogen protection, polyreaction 12-24 hour at 50-85 DEG C, is gathered (styrene butadiene) or polyhutadiene seed emulsion;
Step 2: according to parts by weight meter; 40-90 weight part poly-(styrene butadiene) or the polyhutadiene seed emulsion, 5-60 parts by weight of acrylic acid butyl ester, 5-55 parts by weight of styrene, 0.1-1 weight part initiator, 2-10 weight part emulsifying agent and the 80-300 parts by weight of deionized water that in reaction vessel, add step 1 to obtain; under nitrogen protection; polyreaction 2-6 hour at 50-85 DEG C; add 0.5-2 weight part antioxidant; filter; cohesion; dry, obtain transparent polyvinyl chloride toughening modifier.
2. the preparation method of a kind of transparent polyvinyl chloride toughening modifier according to claim 1, is characterized in that, the emulsifying agent of described step 1 is selected from one or more in potassium oleate, potassium stearate, nilox resin acid potassium or Sodium dodecylbenzene sulfonate.
3. the preparation method of a kind of transparent polyvinyl chloride toughening modifier according to claim 1, is characterized in that, the initiator of described step 1 is Potassium Persulphate, benzoyl peroxide, Diisopropyl azodicarboxylate or di-isopropylbenzene hydroperoxide-ferrous sulfate.
4. the preparation method of a kind of transparent polyvinyl chloride toughening modifier according to claim 1, is characterized in that, the temperature of reaction of described step 1 is 65 DEG C, and the reaction times is 22h.
5. the preparation method of a kind of transparent polyvinyl chloride toughening modifier according to claim 1, is characterized in that, the emulsifying agent of described step 2 is selected from one or more in potassium oleate, potassium stearate, nilox resin acid potassium or Sodium dodecylbenzene sulfonate.
6. the preparation method of a kind of transparent polyvinyl chloride toughening modifier according to claim 1, is characterized in that, the initiator of described step 2 is Potassium Persulphate, benzoyl peroxide, Diisopropyl azodicarboxylate or di-isopropylbenzene hydroperoxide-ferrous sulfate.
7. the preparation method of a kind of transparent polyvinyl chloride toughening modifier according to claim 1, is characterized in that, the temperature of reaction of described step 2 is 70 DEG C, and the reaction times is 5h.
8. the transparent polyvinyl chloride toughening modifier that the preparation method of claim 1-7 described in any one obtains.
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Application publication date: 20140813 |