CN1554681A - Acrylic ester modifier and preparation and use in bisphenol A poly carbonate - Google Patents
Acrylic ester modifier and preparation and use in bisphenol A poly carbonate Download PDFInfo
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- CN1554681A CN1554681A CNA2003101097307A CN200310109730A CN1554681A CN 1554681 A CN1554681 A CN 1554681A CN A2003101097307 A CNA2003101097307 A CN A2003101097307A CN 200310109730 A CN200310109730 A CN 200310109730A CN 1554681 A CN1554681 A CN 1554681A
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Abstract
The acrylic ester modifier is prepared through drying nano silica, nano calcium carbonate, nano zinc oxide, nano zinc sulfide, nano titania or nano cadmium sulfide, adding silane as coupling agent and xylene to react under the xylene refluxing temperature, letting stand to separate lower layer matter, drying the lower layer matter to obtain nano alkylated particle as the acrylic ester modifier. The nano alkylated particle is mixed with emulsifier and deionized water, and through heating under nitrogen protection to 70 deg.c, dropping initiator, acrylic ester monomer to react, cooling, spray drying, modified acrylic ester is obtained. The weight ratio between modifier and the acrylic ester monomer is 2-10 to 90-98. The present invention can raise the performance of polymer.
Description
Technical field
The invention belongs to a kind of acrylic ester modifier, relate in particular to a kind of nanoparticle and be nuclear, acrylic acid esters co-polymer is the acrylic ester modifier of the organic-inorganic hybridized material preparation of shell.
Background technology
The impact modifying agent product of China's production at present mainly contains chlorinatedpolyethylene (CPE), acrylics (ACR) and MBS (MBS), these properties-correcting agent can improve the shock strength of other polymkeric substance, but make the tensile strength of polymkeric substance, heat-drawn wire reduces, flexural strength can not make the over-all properties of polymkeric substance improve.Along with the raising that polymer performance is required and the functionalization of polymkeric substance, the modification of polymkeric substance is had higher requirement.
Polycarbonate resin has good resistance toheat, optical property and mechanical property generally, therefore has widely in industry and daily life and uses.But the shock strength of polycarbonate can not meet the demands in some occasion, simultaneously, and polycarbonate viscosity height, difficult forming; Breach is very responsive; Organic solvent resistance is poor.For above-mentioned reasons, the range of application of polycarbonate is very limited.
Present polycarbonate alloy, though increase on a certain item or a few performances, over-all properties is still waiting to improve.With polycarbonate and ABS is example, and the PC/ABS alloy can improve shock strength and the processing characteristics of PC, but the PC/ABS alloy has reduced the resistance toheat of PC, and optical property reduces, and has also reduced tensile strength and the modulus in flexure of PC simultaneously, and effect is not ideal.
Summary of the invention
The purpose of this invention is to provide a kind of acrylic ester modifier that can improve the polycarbonate over-all properties and method for making and in the application of bisphenol-a polycarbonate.
Carry out spraying drying by the hybrid material of selecting for use different alkylating nanoparticles and acrylic ester monomer to carry out the nucleocapsid structure that multi-step emulsion polymerization makes, obtain white powder, then with PC and properties-correcting agent in two roller mills, Banbury mixer, mix in single screw extrusion machine or the twin screw extruder, granulation enters the various battens of injection moulding mechanism at last, tests its performance.
The part by weight of properties-correcting agent of the present invention is:
Alkylating nanoparticle: acrylic ester monomer=2-10: 98-90.
Alkylating nanoparticle can be alkylation nano silicon, alkylation nano-calcium carbonate, alkylation nano zine oxide, alkylation nano-zinc sulfide, alkylation nano-titanium oxide or alkylation Nano cadmium sulphide etc.
Preparation method of the present invention comprises the steps:
1) prepare alkylating nanoparticle:
At first with nano silicon; nano-calcium carbonate; nano zine oxide; nano-zinc sulfide; nano-titanium oxide or Nano cadmium sulphide are in 100-120 ℃ baking oven after dry 2-5 hour; in the exsiccant nanoparticle, add silane coupling agent KH-570 and dimethylbenzene, in air, stir 20-60min, logical nitrogen protection; in oil bath, be heated to 130 ℃-140 ℃ again; the reflux temperature that temperature of reaction is controlled at dimethylbenzene is 140 ℃, reacts after 8-12 hour, and product is left standstill; after treating layering; vacuum-drying lower floor material obtains the alkylation nanoparticle, and wherein the weight ratio between each material is:
Nano silicon, nano-calcium carbonate, nano zine oxide, nano-zinc sulfide, nano-titanium oxide or Nano cadmium sulphide: KH-570: dimethylbenzene=5-20: 1-4: 100-400;
2) preparation properties-correcting agent
Then alkylating nanoparticle and emulsifying agent are joined in the deionized water; logical nitrogen protection; start stirring; when being raised to 70 ℃, temperature drips initiator, acrylic ester monomer etc. step by step; after reacting completely, cool to room temperature is with the emulsion spraying drying; obtain white powder, wherein the weight ratio between each material is:
Alkylating nanoparticle: emulsifying agent: ionized water=5-20: 1-10: 500-1000.
Alkylating nanoparticle: acrylic ester monomer=5-20: 50-100.
Acrylic ester monomer: initiator=50-100: 0.1-1.
Aforesaid emulsifying agent is a Sodium dodecylbenzene sulfonate.
Aforesaid initiator is an ammonium persulphate.
Aforesaid silane coupling agent KH-570 is that dawn chemical plant, Nanjing produces.
Aforesaid acrylic ester monomer is a vinylbenzene, methyl methacrylate, butyl acrylate, one or more in ethyl propenoate or the 2-ethylhexyl acrylate.
Properties-correcting agent of the present invention is at the application method of bisphenol-a polycarbonate
At first with polycarbonate and properties-correcting agent by weight in homogenizer, carrying out blend for polycarbonate: properties-correcting agent=90-98: 2-10, then that blend is mixing, granulation, make polycarbonate alloy.
Advantage of the present invention is as follows:
1) utilize the properties-correcting agent of this method preparation can the over-all properties of polymkeric substance be improved, its performance has obtained embodiment in polycarbonate.
2) by selecting different nanoparticles for use, make polymkeric substance have special function, can select for use nanoparticle to give polymkeric substance different functions with different functions.
3) can select different polymer monomers for use, make polymer properties obtain in various degree raising.
4) this technological process is fairly simple, changes prescription easily.
5) functionalization for polymkeric substance provides a feasible method.
6) this modified particle does not influence the optical property of polycarbonate.
Embodiment
Embodiment 1
At first, in 105 ℃ baking oven, after dry 2 hours, in the exsiccant nanoparticle, add silane coupling agent KH-570 and dimethylbenzene with nano silicon; stir 20min in air, logical nitrogen protection is heated to 140 ℃ again in oil bath; stir; 140 ℃ of the reflux temperatures that temperature of reaction is controlled at dimethylbenzene reacted after 10 hours, and product is left standstill; after treating layering; vacuum-drying lower floor material obtains the alkylation nano silicon, and wherein the weight ratio between each material is:
Nano silicon: KH-570: dimethylbenzene=10: 2: 250;
Joining in the deionized water alkylating nanoparticle and emulsifying agent then; logical nitrogen protection; start stirring; when being raised to 70 ℃, temperature drips ammonium persulphate, butyl acrylate and methyl methacrylate step by step; after reacting completely, cool to room temperature is with the emulsion spraying drying; obtain white powder, wherein the weight ratio between each material is:
Alkylating nano silicon: butyl acrylate: methyl methacrylate: deionized water: emulsifying agent: initiator=10: 60: 30: 500: 5: 0.4.
With polycarbonate and properties-correcting agent by weight being polycarbonate: properties-correcting agent=95: 5 carries out blend in homogenizer, then that blend is mixing, granulation, make polycarbonate alloy.Test the results are shown in Table 1.
Embodiment 2
At first, in 105 ℃ baking oven, after dry 2 hours, in the exsiccant nanoparticle, add silane coupling agent KH-570 and dimethylbenzene with nano silicon; stir 20min in air, logical nitrogen protection is heated to 140 ℃ again in oil bath; stir; 140 ℃ of the reflux temperatures that temperature of reaction is controlled at dimethylbenzene reacted after 10 hours, and product is left standstill; after treating layering; vacuum-drying lower floor material obtains the alkylation nano silicon, and wherein the weight ratio between each material is:
Nano silicon: KH-570: dimethylbenzene=10: 2: 250;
With the joining in the deionized water of alkylating nano silicon and emulsifying agent, stirring is started in logical nitrogen protection then; when being raised to 70 ℃, temperature drips ammonium persulphate and methyl methacrylate step by step, after reacting completely, and cool to room temperature; with the emulsion spraying drying, obtain white powder
Wherein the weight ratio between each material is: alkylating nano silicon: methyl methacrylate: deionized water: emulsifying agent: initiator=10: 90: 500: 5: 0.4.
With polycarbonate and properties-correcting agent by weight being polycarbonate: properties-correcting agent=95: 5 carries out blend in homogenizer, then that blend is mixing, granulation, make polycarbonate alloy.Test the results are shown in Table 1.
Embodiment 3
At first, in 105 ℃ baking oven, after dry 2 hours, in the exsiccant nanoparticle, add KH-570 and dimethylbenzene with nano zine oxide; stir 20min in air, logical nitrogen protection is heated to 140 ℃ again in oil bath; stir; 140 ℃ of the reflux temperatures that temperature of reaction is controlled at dimethylbenzene reacted after 10 hours, and product is left standstill; after treating layering; vacuum-drying lower floor material obtains the alkylation nano zine oxide, and wherein the weight ratio between each material is:
Nano zine oxide: KH-570: dimethylbenzene=10: 2: 250;
Joining in the deionized water alkylating nanoparticle and emulsifying agent then; logical nitrogen protection; start stirring; when being raised to 70 ℃, temperature drips ammonium persulphate, 2-ethylhexyl acrylate and methyl methacrylate step by step; after reacting completely, cool to room temperature is with the emulsion spraying drying; obtain white powder, wherein the weight ratio between each material is:
Wherein the weight ratio between each material is: alkylating nano zine oxide: 2-ethylhexyl acrylate: methyl methacrylate: deionized water: emulsifying agent: initiator=5: 75: 20: 500: 5: 0.4.
With polycarbonate and properties-correcting agent by weight being polycarbonate: properties-correcting agent=92: 8 carries out blend in homogenizer, then that blend is mixing, granulation, make polycarbonate alloy.Test the results are shown in Table 1.
Embodiment 4
At first, in 100 ℃ baking oven, after dry 4 hours, in the exsiccant nanoparticle, add silane coupling agent KH-570 and dimethylbenzene with nano zine oxide; stir 40min in air, logical nitrogen protection is heated to 140 ℃ again in oil bath; stir; 140 ℃ of the reflux temperatures that temperature of reaction is controlled at dimethylbenzene reacted after 10 hours, and product is left standstill; after treating layering; vacuum-drying lower floor material obtains the alkylation nano zine oxide, and wherein the weight ratio between each material is:
Nano zine oxide: KH-570: dimethylbenzene=10: 2: 250;
Joining in the deionized water alkylating nano zine oxide and emulsifying agent then; logical nitrogen protection; start stirring; when being raised to 70 ℃, temperature drips ammonium persulphate, ethyl propenoate and methyl methacrylate step by step; after reacting completely, cool to room temperature is with the emulsion spraying drying; obtain white powder
Wherein the weight ratio between each material is: alkylating nano zine oxide: ethyl propenoate: methyl methacrylate: deionized water: emulsifying agent: initiator=10: 20: 40: 500: 5: 0.4.
With polycarbonate and properties-correcting agent by weight being polycarbonate: properties-correcting agent=95: 5 carries out blend in homogenizer, then that blend is mixing, granulation, make polycarbonate alloy.Test the results are shown in Table 1.
Embodiment 5
At first, in 110 ℃ baking oven, after dry 2 hours, in the exsiccant nanoparticle, add silane coupling agent KH-570 and dimethylbenzene with nano-calcium carbonate; stir 40min in air, logical nitrogen protection is heated to 140 ℃ again in oil bath; stir; 140 ℃ of the reflux temperatures that temperature of reaction is controlled at dimethylbenzene reacted after 12 hours, and product is left standstill; after treating layering; vacuum-drying lower floor material obtains the alkylation nanoparticle, and wherein the weight ratio between each material is:
Nano silicon: KH-570: dimethylbenzene=10: 2: 250;
Then alkylating nano-calcium carbonate and emulsifying agent are joined in the deionized water; logical nitrogen protection; start stirring; when being raised to 70 ℃, temperature drips ammonium persulphate, butyl acrylate and methyl methacrylate step by step; after reacting completely, cool to room temperature is with the emulsion spraying drying; obtain white powder
Wherein the weight ratio between each material is: alkylating nano-calcium carbonate: butyl acrylate: methyl methacrylate: deionized water: emulsifying agent: initiator=10: 60: 30: 500: 5: 0.4.
With polycarbonate and properties-correcting agent by weight being polycarbonate: properties-correcting agent=95: 5 carries out blend in homogenizer, then that blend is mixing, granulation, make polycarbonate alloy.Test the results are shown in Table 1.
Embodiment 6
At first, in 105 ℃ baking oven, after dry 2 hours, in the exsiccant nanoparticle, add silane coupling agent KH-570 and dimethylbenzene with nano-zinc sulfide; stir 60min in air, logical nitrogen protection is heated to 140 ℃ again in oil bath; stir; 140 ℃ of the reflux temperatures that temperature of reaction is controlled at dimethylbenzene reacted after 10 hours, and product is left standstill; after treating layering; vacuum-drying lower floor material obtains the alkylation nanoparticle, and wherein the weight ratio between each material is:
Nano-zinc sulfide: KH-570: dimethylbenzene=10: 2: 250;
Joining in the deionized water alkylating nano-zinc sulfide and emulsifying agent then; logical nitrogen protection; start stirring; when being raised to 70 ℃, temperature drips ammonium persulphate, 2-ethylhexyl acrylate and methyl methacrylate step by step; after reacting completely, cool to room temperature is with the emulsion spraying drying; obtain white powder
Wherein the weight ratio between each material is: alkylating nano-zinc sulfide: 2-ethylhexyl acrylate: methyl methacrylate: deionized water: emulsifying agent: initiator=15: 60: 25: 500: 5: 0.4.
With polycarbonate and properties-correcting agent by weight being polycarbonate: properties-correcting agent=95: 5 carries out blend in homogenizer, then that blend is mixing, granulation, make polycarbonate alloy.Test the results are shown in Table 1.
The notch shock performance of each sample and tensile property are tested with homemade JB6 type shock-testing machine and homemade LT-1000 type tension testing machine according to GB GB/T 1043-93 and GB/T 1040-92 respectively.Heat-drawn wire is measured according to GB1634-79.
The prescription and the performance table look-up of table 1PC alloy
Claims (8)
1, a kind of acrylic ester modifier is characterized in that the part by weight of properties-correcting agent is:
Alkylating nanoparticle: acrylic ester monomer=2-10: 98-90.
2, a kind of acrylic ester modifier as claimed in claim 1, it is characterized in that described alkylating nanoparticle is the alkylation nano silicon, the alkylation nano-calcium carbonate, the alkylation nano zine oxide, alkylation nano-zinc sulfide, alkylation nano-titanium oxide or alkylation Nano cadmium sulphide.
3, a kind of acrylic ester modifier as claimed in claim 1 is characterized in that described acrylic ester monomer comprises vinylbenzene, methyl methacrylate, butyl acrylate, one or more in ethyl propenoate or the 2-ethylhexyl acrylate.
4,, it is characterized in that comprising the steps: as the preparation method of each described a kind of acrylic ester modifier of claim 1-3
(1) prepare alkylating nanoparticle:
At first with nano silicon; nano-calcium carbonate; nano zine oxide; nano-zinc sulfide; nano-titanium oxide or Nano cadmium sulphide are in 100-120 ℃ baking oven after dry 2-5 hour; in the exsiccant nanoparticle, add silane coupling agent KH-570 and dimethylbenzene, in air, stir 20-60min, logical nitrogen protection; in oil bath, be heated to 130 ℃-140 ℃ again; the reflux temperature that temperature of reaction is controlled at dimethylbenzene is 140 ℃, reacts after 8-12 hour, and product is left standstill; after treating layering; vacuum-drying lower floor material obtains the alkylation nanoparticle, and wherein the weight ratio between each material is:
Nano silicon, nano-calcium carbonate, nano zine oxide, nano-zinc sulfide, nano-titanium oxide or Nano cadmium sulphide: KH-570: dimethylbenzene=5-20: 1-4: 100-400;
(2) preparation properties-correcting agent
Then alkylating nanoparticle and emulsifying agent are joined in the deionized water; logical nitrogen protection; start stirring; when being raised to 70 ℃, temperature drips initiator, acrylic ester monomer etc. step by step; after reacting completely, cool to room temperature is with the emulsion spraying drying; obtain white powder, wherein the weight ratio between each material is:
Alkylating nanoparticle: emulsifying agent: ionized water=5-20: 1-10: 500-1000.
Alkylating nanoparticle: acrylic ester monomer=5-20: 50-100.
Acrylic ester monomer: initiator=50-100: 0.1-1.
5, the preparation method of a kind of acrylic ester modifier as claimed in claim 4 is characterized in that described emulsifying agent is a Sodium dodecylbenzene sulfonate.
6, the preparation method of a kind of acrylic ester modifier as claimed in claim 4 is characterized in that described initiator is an ammonium persulphate.
7, the preparation method of a kind of acrylic ester modifier as claimed in claim 4 is characterized in that described silane coupling agent KH-570 is that dawn chemical plant, Nanjing produces.
8, as the application method of each described a kind of acrylic ester modifier of claim 1-3, it is characterized in that at first polycarbonate and properties-correcting agent by weight in homogenizer, carrying out blend, then that blend is mixing, granulation, make polycarbonate alloy for polycarbonate: properties-correcting agent=90-98: 2-10.
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| CNA2003101097307A CN1554681A (en) | 2003-12-26 | 2003-12-26 | Acrylic ester modifier and preparation and use in bisphenol A poly carbonate |
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| CNA2003101097307A CN1554681A (en) | 2003-12-26 | 2003-12-26 | Acrylic ester modifier and preparation and use in bisphenol A poly carbonate |
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| CN1323092C (en) * | 2005-01-20 | 2007-06-27 | 辽宁大学 | Modification method for graft polymerization of acrylic ester of silicane coupled to Nano SiO2 |
| CN102060702A (en) * | 2010-10-28 | 2011-05-18 | 华南理工大学 | Visible light curing fluorine-containing dental resin monomer/composite material and preparation method thereof |
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| CN103183771B (en) * | 2011-12-30 | 2016-01-20 | 山东世拓高分子材料股份有限公司 | Nano zinc dioxide impact-resistant modification acrylate class linear macromolecule polymkeric substance and method for making |
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