CN104629090A - Copper powder coated polymer microspheres and preparation method and application thereof - Google Patents
Copper powder coated polymer microspheres and preparation method and application thereof Download PDFInfo
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- CN104629090A CN104629090A CN201310544186.2A CN201310544186A CN104629090A CN 104629090 A CN104629090 A CN 104629090A CN 201310544186 A CN201310544186 A CN 201310544186A CN 104629090 A CN104629090 A CN 104629090A
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Abstract
The invention discloses copper powder coated polymer microspheres. The microspheres comprise the following components: 5-80 wt% of copper powder / aqueous copper powder paste, 18-90 wt% of an aqueous polymer dispersion liquid, 0.1-5 wt% of an antioxidant corrosion inhibitor and 0.2-10 wt% of a curing agent. A preparation method includes the steps of: a) adding the antioxidant corrosion inhibitor into the aqueous polymer dispersion liquid at room temperature, stirring and dispersing for 10-25 min, slowly adding copper powder / aqueous copper powder paste subjected to surface treatment into the dispersion liquid, stirring while adding the curing agent, and continuing stirring for 30-120 min to obtain a copper powder coated polymer composite dispersion liquid; and b) conducting spray drying on the composite dispersion liquid, subjecting the copper powder coated polymer droplets formed by spray to curing crosslinking reaction through the curing agent, so as to obtain the copper powder coated polymer microspheres. The prepared copper powder coated polymer microspheres can improve the compatibility between copper powder and the matrix resin, improve the flow uniformity of copper powder with a melt in an extrusion or injection molding process and, thereby eliminating flow mark on the surface of the product, and reduce the weld bond. Therefore, the invention can be used in the preparation of free-spraying materials.
Description
Technical field
The present invention relates to field of high polymer material modification, be specifically related to microballoon of polymer overmold copper powder and preparation method thereof and application.
Background technology
For improving outward appearance, the prolongation product life of plastics, usually spray treatment need be carried out to surface of plastic products.But spraying coating process exists shortcomings: cost is high, Production Flow Chart is long, efficiency is low, defective products rate is high; Not environmentally, contaminate environment, the harm physical and mental health of operator, security risk are large; Lacquer painting easily comes off, and causes product appearance bad, affects product specification; Product and defective products reclaim difficulty.Along with people environmental problem more and more paid attention to and pay close attention to, exempting from spray material product and just progressively demonstrate its competitive power, artwork, toy, household electrical appliances, automobile, electronic product, sports goods and office appliance etc. can be widely used in.
In order to make goods have flavous metal effect, normally in matrix resin, add copper powder, interconnection between copper powder and copper powder, form the film of continuous print copper powder effect, hidden base material, presented metal-like; But by directly being added in matrix resin by copper powder, the poor compatibility of matrix resin and copper powder, is extruding or under the strong pressure of injection moulding and Strong shear condition, it is consistent that copper powder and base resin material are difficult to reach mobility, easily occurs current mark; Particularly baroque goods, copper powder along flow direction orientation turns in generation melt flow, flow velocity is unstable, during the phenomenons such as melt converges, cause copper powder skewness in the melt, even form the defect such as current mark and weld bond at product surface, seriously limit the marketing and application of exempting from spray material.
Up to the present, polymer overmold copper powder microballoon is formed by spraying dry and crosslinking reaction after copper powder being coated on aqueous polymer dispersion, again the microballoon of this polymer overmold copper powder and matrix resin are made by blending extrusion and exempt from spray material, thus the spray material of exempting from finally made without current mark, light weld bond rarely has report.
Summary of the invention
The primary and foremost purpose of invention aims to provide a kind ofly can improve the consistency of copper powder and matrix resin, improve the microballoon of the conforming polymer overmold copper powder of flowing of copper powder and melt.
Another object of the present invention is the preparation method of the microballoon providing above-mentioned polymer overmold copper powder.
The present invention is achieved by the following technical solution:
A microballoon for polymer overmold copper powder, by weight percentage, comprises following component:
Copper powder
/water-based copper powder slurry 5-80wt%
Aqueous polymer dispersion 18-90wt%
Antioxygen inhibiter 0.1-5wt%
Solidifying agent 0.2-10wt%.
The physical structure of the microballoon of described polymer overmold copper powder is the copper powder kernel containing particle diameter 3-200 μm, is coated with at the outside surface of copper powder kernel the polymer shell that thickness is 5-800 μm.
The Cu constituent content of described copper powder is no less than 60wt%, and contains Zn, Sn, Ni, Be, Mn, Fe, Pb, Si, P, B, Ti or rare earth element one or more; The shape of described copper powder is selected from one or more of spherical, dendroid, sheet; The particle diameter of described copper powder is 5-200um, is preferably 5-100um, is more preferably 5-50um.
The solid content of described water-based copper powder slurry is 10-80wt%, is preferably 20-70wt%.
The solid content of described aqueous polymer dispersion is 10-60wt%, be selected from polyaminoester emulsion, organic silicon emulsion, organic fluorine emulsion, epoxy resin latex, polyacrylate dispersion, benzene emulsion, organosilicon crylic acid latex, modified ABS resin emulsion, the modified-cellulose aqueous solution, polyvinyl alcohol and the condenses aqueous solution thereof, the polyacrylic acid aqueous solution, water-based urea-formaldehyde resin, aqueous melamine and etherified resin thereof, resol resins, aqueous alkide resin, aqueous polyester resin, aqueous polyvinyl acetate emulsion, ethene improved-vinyl acetate emulsion, nature rubber latex, styrene-butadiene emulsion, butyronitrile emulsion, one or more mixtures of vinyl acetate emulsion and mixture and modifier.
Described antioxygen inhibiter is selected from one or more mixtures of phenylpropyl alcohol triazole, phytic acid, phytate, oxine, Organophosphorous compounds, phosphoric acid and derivative thereof, pyrogallol.
Described solidifying agent comprises aliphatic polyamine, aromatic polyamine, alicyclic polyamine, ammonium chloride, Resorcinol, aziridine and derivative thereof, ammonium chloride, zinc oxide, zinc salt, Dyhard RU 100, liquid polyamide, aromatic amine, aminoresin, polyisocyanates and oligopolymer, polycarbodiimide, organo-siloxane, the complex compound of boracic, one or more mixtures of epoxy based curing agent.
The microballoon of described polymer overmold copper powder also comprises other auxiliary agent of 0-3wt%, and other auxiliary agents described comprise defoamer, dispersion agent and/or anti-settling agent; The wherein preferred silicone antifoam agent of defoamer; Dispersion agent is preferably polycarboxylate dispersant.
A preparation method for the microballoon of polymer overmold copper powder, comprises the steps:
A) in aqueous polymer dispersion, antioxygen inhibiter is added under normal temperature, dispersed with stirring 10-25min; Under agitation, surface-treated copper powder/water-based copper powder slurry is slowly added in dispersion liquid, add solidifying agent and/or other auxiliary agents while stirring, continue to stir 30-120min, copper powder is fully disperseed and coated by aqueous polymer dispersion, obtain the composite dispersion liquid of polymer overmold copper powder;
B) composite dispersion liquid step a) obtained carries out spraying dry, and in spray-drying process, the small droplets of the polymer overmold copper powder that spraying is formed is cured crosslinking reaction by solidifying agent, obtains the microballoon of polymer overmold copper powder.
Copper powder in wherein surface-treated copper powder/water-based copper powder slurry is by adding as processing of lubricant, tensio-active agent etc. obtains.
Described spray-dired intake air temperature is 150-300 DEG C, is preferably 170-250 DEG C; Air outlet temperature is 50-130 DEG C, is preferably 70-100 DEG C.
The application of microballoon in thermoplasticity and thermosetting material of the polymer overmold copper powder that the preparation method of the microballoon of described polymer overmold copper powder prepares.
Compared with prior art, beneficial effect is as follows in the present invention:
The present invention by slowly adding copper powder/water-based copper powder slurry in aqueous polymer dispersion, make the microballoon of the polymer overmold copper powder be prepared from can improve the consistency of copper powder and matrix resin, improve copper powder endurance of cutting and extrude or in injection moulding process with the flowing consistence of melt, thus eliminate product surface current mark, alleviate weld bond, can be widely used in preparing without current mark, light weld bond exempt from spraying thermoplastic material.
Embodiment
Further illustrate the present invention below by embodiment, following examples are the present invention's preferably embodiment, but embodiments of the present invention are not by the restriction of following embodiment.
embodiment 1-6 and comparative example 1-3:
By the formula of embodiment 1-6 in table 1 and comparative example 1-2, in aqueous polymer dispersion, add antioxygen inhibiter under normal temperature, dispersed with stirring 10-25min; Under agitation, surface-treated copper powder/water-based copper powder slurry is slowly added in dispersion liquid, add solidifying agent and/or other auxiliary agents while stirring, continue to stir 30-120min, copper powder is fully disperseed and coated by aqueous polymer dispersion, obtain the composite dispersion liquid of polymer overmold copper powder; The composite dispersion liquid obtained is carried out spraying dry, and in spray-drying process, the small droplets of the polymer overmold copper powder that spraying is formed is cured crosslinking reaction by solidifying agent, obtains polymer overmold copper powder microballoon; The intake air temperature of spray-drying process is 150-300 DEG C, and air outlet temperature is 50-130 DEG C.
Table 1
Note: blackening degree :+more multilist show more black.
Embodiment 1: in copper powder, the content of Cu element is 60wt%, simultaneously containing Zn, Sn and Ni; Its shape is sheet; Particle diameter is 5 μm; Aqueous polymer dispersion is polyacrylate dispersion, and its solid content is 10wt%; Antioxygen sustained release dosage is phytic acid; Solidifying agent is aminoresin.
Embodiment 2: in copper powder, the content of Cu element is 70wt%, simultaneously containing Zn, Pb and Fe; Its shape is dendroid; Particle diameter is 100 μm; Aqueous polymer dispersion is polyaminoester emulsion, and its solid content is 50wt%; Antioxygen sustained release dosage is phytic acid; Solidifying agent is polyisocyanates, and other auxiliary agent is 0.4wt% silicone antifoam agent and 0.4wt% polycarboxylate dispersant.
Embodiment 3: in copper powder, the content of Cu element is 80wt%, simultaneously containing Zn, Sn and Ni; Its shape is sheet; Particle diameter is 160 μm; Aqueous polymer dispersion is epoxy resin latex, and its solid content is 20wt%; Antioxygen sustained release dosage is phytic acid; Solidifying agent is aziridine, and other auxiliary agent is 1wt% silicone antifoam agent and 2wt% polycarboxylate dispersant.
Embodiment 4: in copper powder, the content of Cu element is 75wt%, simultaneously containing Zn, Sn and Ni; Its shape is spherical; Particle diameter is 200 μm; Aqueous polymer dispersion is polyacrylate dispersion, and its solid content is 40wt%; Antioxygen sustained release dosage is oxine; Solidifying agent is 5wt% aziridine and 5wt% polyisocyanates.
Embodiment 5: in copper powder, the content of Cu element is 65wt%, simultaneously containing Zn, Sn and Pb; Its shape is dendroid; Particle diameter is 50 μm; Aqueous polymer dispersion is ethene improved-vinyl acetate emulsion, and its solid content is 80wt%; Antioxygen sustained release dosage is phytic acid; Solidifying agent is 5wt% aminoresin and 2wt% aziridine, and other auxiliary agent is 0.4wt% silicone antifoam agent and 0.6wt% polycarboxylate dispersant.
Embodiment 6: in copper powder, the content of Cu element is 85wt%, simultaneously containing Zn, Fe and Cu; Its shape is dendroid; Particle diameter is 20 μm; Aqueous polymer dispersion is water-based urea-formaldehyde resin, and its solid content is 10wt%; Antioxygen sustained release dosage is phosphoric acid; Solidifying agent is aminoresin, and other auxiliary agent is 0.5wt% silicone antifoam agent and 0.9wt% polycarboxylate dispersant.
Comparative example 1: in copper powder, the content of Cu element is 60wt%, simultaneously containing Zn, Pb and Ni; Its shape is sheet; Particle diameter is 5 μm; Aqueous polymer dispersion is polyacrylate dispersion, and its solid content is 10wt%; Antioxygen sustained release dosage is pyrogallol; Solidifying agent is aminoresin, and other auxiliary agent is 0.4wt% silicone antifoam agent and 0.6wt% polycarboxylate dispersant.
Comparative example 2: in copper powder, the content of Cu element is 70wt%, simultaneously containing Zn, Pb and Ni; Its shape is sheet; Particle diameter is 160 μm; Aqueous polymer dispersion is polyaminoester emulsion, and its solid content is 50wt%; Antioxygen sustained release dosage is phytic acid; Solidifying agent is polyisocyanates, and other auxiliary agent is 0.4wt% silicone antifoam agent and 0.4wt% polycarboxylate dispersant.
Comparative example 3: do not carry out coated Copper powder/water-based copper powder slurry, wherein in copper powder, the content of Cu element is 60wt%, simultaneously containing Zn, Sn and Ni; Its shape is sheet; Particle diameter is 30 μm.
embodiment 7-14:
By the formula in table 2, the microballoon of 1-25wt% polymer overmold copper powder is inserted high-speed mixer mix with 70-98wt% thermoplastic resin, 0-10wt% compatilizer, 0.1-1wt% oxidation inhibitor, 0.1-0.5wt% processing aid; Insert mixing extrusion in forcing machine, pelletizing after cooling, the moulding material of obtained thermoplastic polymer.Equally, by the formula in table 2, the microballoon of 1-25wt% polymer overmold copper powder is inserted mixing machine mix with 70-98wt% thermosetting resin, 0-10wt% compatilizer, 0.1-1wt% oxidation inhibitor, 0.1-0.5wt% processing aid; Then be placed in forcing machine fusion plastification, then injecting the mould of heat, there is cross-linking and curing reaction in material at high temperature under high pressure, the moulding material of obtained thermosetting polymer.Both are distinguished sample preparation, and test its performance, test result is in table 2.
comparative example 4-9:
Copper powder/water-based copper powder the slurry of the polymer overmold copper powder microballoon of comparative example 4-7 and comparative example 8-9 is inserted mixing machine mix with matrix resin (thermoplastic resin, thermosetting resin), compatilizer, oxidation inhibitor, processing aid; Then insert fusion plastification in forcing machine, prepare the moulding material of thermoplasticity and thermosetting polymer respectively by dicing machine and die material, its performance is tested in sample preparation, and test result is in table 2.
Table 2
Embodiment 7: thermoplastic resin is PP resin, compatilizer is terpolymer EP rubber, and oxidation inhibitor is hindered phenol antioxygen 1010 and phosphoric acid ester irgasfos 168, and processing aid is organic silicone lubricant;
Embodiment 8: thermosetting resin is epoxy resin, oxidation inhibitor is hindered phenol antioxygen 1010 and phosphoric acid ester irgasfos 168, and processing aid is Zinic stearas;
Embodiment 9: thermoplastic resin is PC/ABS resin, compatilizer is acrylate copolymer, and oxidation inhibitor is hindered phenol antioxygen 1010 and phosphoric acid ester irgasfos 168, and processing aid is erucicamide;
Embodiment 10: thermosetting resin is resol, oxidation inhibitor is hindered phenol antioxygen 1010 and phosphoric acid ester irgasfos 168, and processing aid is Zinic stearas;
Embodiment 11: thermoplastic resin is ABS, compatilizer is ABS grafted maleic anhydride, and oxidation inhibitor is amine antioxidants 445, and processing aid is amine hydroxybenzene;
Embodiment 12: thermosetting resin is melamine formaldehyde resin, oxidation inhibitor is hindered phenol antioxygen 1010 and phosphoric acid ester irgasfos 168, and processing aid is Zinic stearas;
Embodiment 13: thermoplastic resin is TPU resin, oxidation inhibitor is hindered phenol antioxygen 1010, and processing aid is calcium stearate;
Embodiment 14: thermosetting resin is urethane resin, oxidation inhibitor is hindered phenol antioxygen 1010 and phosphoric acid ester irgasfos 168, and processing aid is Zinic stearas;
Comparative example 4: thermoplastic resin is PP resin, compatilizer is terpolymer EP rubber, and oxidation inhibitor is hindered phenol antioxygen 1010 and phosphoric acid ester irgasfos 168, and processing aid is organic silicone lubricant;
Comparative example 5: thermoplastic resin is thermoplastic ABS resin, compatilizer is ABS grafted maleic anhydride, and oxidation inhibitor is amine antioxidants 445, and processing aid is amine hydroxybenzene;
Comparative example 6: thermoplastic resin is PC/ABS alloy, compatilizer is acrylate copolymer, and oxidation inhibitor is hindered phenol antioxygen 1010 and phosphoric acid ester irgasfos 168, and processing aid is erucicamide;
Comparative example 7: thermosetting resin is resol, oxidation inhibitor is hindered phenol antioxygen 1010, and processing aid is calcium stearate;
Comparative example 8: thermoplastic resin is PP resin, in copper powder, the content of Cu element is 60wt%, simultaneously containing Zn, Sn and Ni; Its shape is sheet; Particle diameter is 30 μm; Compatilizer is terpolymer EP rubber, and oxidation inhibitor is hindered phenol antioxygen 1010 and phosphoric acid ester irgasfos 168, and processing aid is organic silicone lubricant;
Comparative example 9: thermosetting resin is epoxy resin, in copper powder, the content of Cu element is 60wt%, simultaneously containing Zn, Sn and Ni; Its shape is sheet; Particle diameter is 30 μm; Oxidation inhibitor is hindered phenol antioxygen 1010, and processing aid is calcium stearate.
Properties testing standard or method:
Particle diameter: adopt testing electronic microscope;
Blackening degree: range estimation ,+more multilist show more black;
Current mark: range estimation, "-" indicates without current mark, and "+" represents to there is current mark, and "+" more multilist shows that current mark is more serious;
Weld bond: range estimation, "+" more multilist show weld bond more seriously, more obvious.
Can find out from the embodiment and comparative example of table 1, by copper powder/water-based copper powder slurry with water polymer dispersion liquid carries out coated, is conducive to the consistency improving copper powder and matrix resin, can reduce the blackening degree of copper powder; Can find out from the embodiment and comparative example of table 2, the microballoon of the polymer overmold copper powder of 1-25wt% is adopted in embodiment 7-14, again with matrix resin blending extrusion, and copper powder/water-based copper powder slurry is directly added to blending extrusion in matrix resin by comparative example 8-9, ensureing under other components prerequisite consistent with content, exempting from obtained by embodiment 7-14 sprays thermoplasticity and thermosetting material and has technique effect without current mark, gently weld bond.
Claims (11)
1. a microballoon for polymer overmold copper powder, is characterized in that: by weight percentage, comprises following component:
Copper powder
/water-based copper powder slurry 5-80wt%
Aqueous polymer dispersion 18-90wt%
Antioxygen inhibiter 0.1-5wt%
Solidifying agent 0.2-10wt%.
2. the microballoon of polymer overmold copper powder according to claim 1, is characterized in that, containing the copper powder kernel of particle diameter 3-200 μm, is coated with at the outside surface of copper powder kernel the polymer shell that thickness is 5-800 μm.
3. the microballoon of polymer overmold copper powder according to claim 1, is characterized in that, the Cu constituent content of described copper powder is no less than 60wt%, and contains Zn, Sn, Ni, Be, Mn, Fe, Pb, Si, P, B, Ti or rare earth element one or more; The shape of described copper powder is selected from one or more of spherical, dendroid, sheet; The particle diameter of described copper powder is 5-200um, is preferably 5-100um, is more preferably 5-50um.
4. the microballoon of polymer overmold copper powder according to claim 1, is characterized in that, the solid content of described water-based copper powder slurry is 10-80wt%, is preferably 20-70wt%.
5. the microballoon of polymer overmold copper powder according to claim 1, it is characterized in that, the solid content of described aqueous polymer dispersion is 10-60wt%, be selected from polyaminoester emulsion, organic silicon emulsion, organic fluorine emulsion, epoxy resin latex, polyacrylate dispersion, benzene emulsion, organosilicon crylic acid latex, modified ABS resin emulsion, the modified-cellulose aqueous solution, polyvinyl alcohol and the condenses aqueous solution thereof, the polyacrylic acid aqueous solution, water-based urea-formaldehyde resin, aqueous melamine and etherified resin thereof, resol resins, aqueous alkide resin, aqueous polyester resin, aqueous polyvinyl acetate emulsion, ethene improved-vinyl acetate emulsion, nature rubber latex, styrene-butadiene emulsion, butyronitrile emulsion, one or more mixtures of vinyl acetate emulsion and mixture and modifier.
6. the microballoon of polymer overmold copper powder according to claim 1, it is characterized in that, described antioxygen inhibiter is selected from one or more mixtures of phenylpropyl alcohol triazole, phytic acid, phytate, oxine, Organophosphorous compounds, phosphoric acid and derivative thereof, pyrogallol.
7. the microballoon of polymer overmold copper powder according to claim 1, it is characterized in that, described solidifying agent comprises aliphatic polyamine, aromatic polyamine, alicyclic polyamine, ammonium chloride, Resorcinol, aziridine and derivative thereof, zinc oxide, zinc salt, Dyhard RU 100, liquid polyamide, aromatic amine, aminoresin, polyisocyanates and oligopolymer, polycarbodiimide, organo-siloxane, the complex compound of boracic, one or more mixtures of epoxy based curing agent.
8. the microballoon of polymer overmold copper powder according to claim 1, is characterized in that, also comprises other auxiliary agent of 0-3wt%, and other auxiliary agents described comprise defoamer, dispersion agent and/or anti-settling agent; Be preferably silicone antifoam agent and/or polycarboxylate dispersant.
9. the preparation method of the microballoon of the polymer overmold copper powder as described in any one of claim 1-8, is characterized in that, comprise the steps:
A) in aqueous polymer dispersion, antioxygen inhibiter is added under normal temperature, dispersed with stirring 10-25min; Under agitation, surface-treated copper powder/water-based copper powder slurry is slowly added in dispersion liquid, add solidifying agent and/or other auxiliary agents while stirring, continue to stir 30-120min, copper powder is fully disperseed and coated by aqueous polymer dispersion, obtain the composite dispersion liquid of polymer overmold copper powder;
B) composite dispersion liquid step a) obtained carries out spraying dry, and in spray-drying process, the small droplets of the polymer overmold copper powder that spraying is formed is cured crosslinking reaction by solidifying agent, obtains the microballoon of polymer overmold copper powder.
10. the preparation method of the microballoon of polymer overmold copper powder according to claim 9, is characterized in that, described spray-dired intake air temperature is 150-300 DEG C, is preferably 170-250 DEG C; Air outlet temperature is 50-130 DEG C, is preferably 70-100 DEG C.
The application of microballoon in thermoplasticity and thermosetting material of the polymer overmold copper powder that the preparation method of the microballoon of 11. polymer overmold copper powders as claimed in claim 9 prepares.
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| CN111687407A (en) * | 2020-07-28 | 2020-09-22 | 鞍山大族激光技术有限公司 | Copper powder for laser cladding of phosphorus-copper workpiece and cladding method |
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