CN102501506B - PVC (Poly Vinyl Chloride) wood-plastic foaming composite and preparation method thereof - Google Patents
PVC (Poly Vinyl Chloride) wood-plastic foaming composite and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a PVC (Poly Vinyl Chloride) wood-plastic foaming composite and a preparation method of the wood-plastic foaming composite. The PVC wood-plastic foaming composite comprises a PVC wood-plastic foaming base material layer and an ASA (Acrylonitrile Styrene Acrylate) layer which is co-extruded and formed on at least one side of the PVC wood-plastic foaming base material layer, wherein the PVC wood-plastic foaming base material layer comprises the following components in parts by weight: 100 parts of PVC, 50-100 parts of paddings, 1-1.5 parts of coupling agents, 5-7 parts of compound stabilizers, 1.0-1.5 parts of compound foaming agents and 6-8 parts of blowing promoters. The PVC wood-plastic foaming composite disclosed by the invention has the characteristics of light weight, high specific strength, water prevention, corrosion prevention, heat preservation, good weather resistance, low formula cost and low material density, and can be widely used in outdoor product markets such as exterior decoration of buildings, garden landscapes, fences, plank ways and the like.
Description
Technical field
The present invention relates to a kind of PVC Wood-plastic foam composite and preparation method thereof.
Background technology
Wood-plastic material has the double grading of timber and plastics concurrently: mechanical property is good, be not afraid of and damage by worms, mildewproof bacterium, do not absorb moisture, the advantage such as can reuse.Application number is the coextrusion forming process that 00132561.2 patent has recorded a kind of plastic-wood section, the shortcoming of this technique is: the density of profile shapes prepared by wood plastic composite is at 1.1 ~ 1.4g/ cm3, make material deadweight higher, cannot meet lightweight, shock resistance, high heat insulation requirement, product cost is high simultaneously, is unfavorable for the marketing of product.
And, mould at present woodwork and be applied to outdoor its main shortcoming and be;
1, the whiting of easily fading after solar radiation, rainwater shower for a long time, weatherability is poor;
2, service life short, effect is poor, need to regularly whitewash protection, maintenance cost is high.
The people that just more come the more based on this co-extrusion technology attempt to be applied in the production and processing of outdoor wood plastic product, but the application that wooden co-extrusion product is also moulded impact in the raising of subsidiary next product cost.
Summary of the invention
In order to solve the problems of the technologies described above, the invention provides a kind of PVC Wood-plastic foam composite and preparation method thereof, organically foaming technique and co-extrusion technology are combined, realize reduction product cost, improve again the weatherability of material.
PVC Wood-plastic foam composite provided by the invention, comprises that PVC Wood-plastic foam base material and coextrusion mold are at least ASA layer of one side of described PVC Wood-plastic foam substrate layer, and wherein, described PVC Wood-plastic foam substrate layer comprises the component of following parts by weight:
100 parts of polyvinyl chloride;
50 ~ 100 parts of fillers;
1 ~ 1.5 part of coupling agent;
5 ~ 7 parts of compound stabilizers;
1.0 ~ 1.5 parts of composite foamable agents;
6 ~ 8 parts of blowing promotors.
Preferably, the K value 61 of described polyvinyl chloride, the degree of polymerization is 750 ~ 850; Described filler is one or more any mixture in calcium carbonate, talcum powder or granule or fibrous material rice wheat husk powder, wood chips, bamboo bits, crops tangerine bar powder, beans, cornstarch, cotton shell, nut duricrust or coconut husk; Described compound stabilizer is one or more any mixture in calcium-zinc composite stabilizing agent or lead salt compound stabilizer; Described coupling agent is silane coupling agent or aluminium titante coupling agent; Described composite foamable agent contains Celogen Az, sodium acid carbonate and zinc oxide; Described blowing promotor is the multiple copolymer of molecular weight 5,000,000 ~ 6,000,000 esters of acrylic acid.
Wherein, described calcium-zinc composite stabilizing agent contains calcium stearate, zinc stearate, hydrotalcite, Tissuemat E, stearic acid, antioxidant and OPE compound; Described lead salt compound stabilizer contains dibasic Lead Phosphite, lead stearate, tribasic lead sulfate, Tissuemat E, stearic acid, antioxidant and OPE compound.
Preferably, the thickness of described ASA layer is 0.25 ~ 0.45mm, and PVC Wood-plastic foam substrate layer thickness is 5 ~ 50mm.
The invention provides the method for the above-mentioned PVC Wood-plastic foam composite of preparation: each component of described PVC Wood-plastic foam base material is extruded Wood-plastic foam melt by extruder and entered foaming co-extruding mould after dehumidifying, the mixing that heats up; Described ASA particle enters foaming co-extruding mould after extruder is extruded ASA melt; The composite molding in foaming co-extruding mould of described Wood-plastic foam melt and described ASA melt, cooling.
Particularly, above-mentioned method, comprises the steps:
A. the filler of getting described amount is dried, and adds coupling agent to activate described filler, and mixture is cooled to room temperature;
B. polyvinyl chloride and the compound stabilizer of getting described amount mix, stirring is warming up to 90 ~ 95 DEG C, then add the blowing promotor of step a gained mixture and described amount, stirring is warming up to 100 ~ 105 DEG C, add the composite foamable agent of described amount, continue stirring and be warming up to 115 ~ 125 DEG C, be then cooled to below 40 DEG C, obtain foam mixture;
C. foam mixture step b being obtained drops in extruder, and the Wood-plastic foam melt of extruding through extruder enters foaming co-extruding mould;
D. get ASA particulate material and drop in extruder, the ASA melt of extruding through extruder enters the foaming co-extruding mould described in step c;
E. the Wood-plastic foam melt of step c and ASA melt composite molding in described foaming co-extruding mould, cooling, cutting, to obtain final product.
Preferably, the water content of compound is below 1% described in step b, and bulk density is 0.65 ~ 0.75g/mL.
Wherein, the foam mixture described in step c drops into conical double screw extruder, engine speed 10-15rpm/min.
Wherein, the ASA particulate material described in steps d drops into single screw extrusion machine, engine speed 8-12rpm/min.
Wherein, the co-extruding mould that foams described in step e is for releasing pattern progressively, and die gap multiplication factor is 1.5 ~ 2.5.
PVC Wood-plastic foam composite provided by the invention is after thermal forming device heating and melting, in mould, be shaped to the product of a kind of core with the novel wood-plastic foaming body layer of continuous uniform distribution micropore and the surperficial fine and close ASA surface layer composite integrated forming through co-extrusion, can reach following effect:
1, PVC Wood-plastic foam composite have that light weight, specific strength are high, the feature of waterproof, anticorrosion, insulation, and the processing characteristic that has timber can follow closely, can saw, can dig.
2, this PVC Wood-plastic foam composite has high weatherability, can be widely used in the outdoor goods markets such as building external decoration, garden landscape, fence plank road.
3, this PVC Wood-plastic foam composite has the distinguishing feature that formulation cost is low, density of material is low, can significantly reduce the comprehensive cost of product.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described, can be implemented, but illustrated embodiment is not as a limitation of the invention so that those skilled in the art can better understand the present invention also.
PVC Wood-plastic foam composite provided by the invention, comprise PVC Wood-plastic foam substrate layer and coextrusion mold described PVC Wood-plastic foam substrate layer at least one side ASA(propylene fine-Acrylate-styrene bipolymer terpolymer) layer, (, the one side of PVC Wood-plastic foam substrate layer or upper and lower two-sided coextrusion mold have ASA layer), wherein, described PVC Wood-plastic foam substrate layer comprises the component of following parts by weight:
100 parts of polyvinyl chloride;
50 ~ 100 parts of fillers;
1 ~ 1.5 part of coupling agent;
5 ~ 7 parts of compound stabilizers;
1.0 ~ 1.5 parts of composite foamable agents;
6 ~ 8 parts of blowing promotors.
Wherein, preferably, the K value 61 of described polyvinyl chloride, the degree of polymerization is 750 ~ 850.
Described filler is not particularly limited, and can be one or more any mixture in calcium carbonate, talcum powder or granule or fibrous material rice wheat husk powder, wood chips, bamboo bits, crops tangerine bar powder, beans, cornstarch, cotton shell, nut duricrust or coconut husk.
Described compound stabilizer can be one or more any mixture in PVC calcium-zinc composite stabilizing agent or lead salt compound stabilizer.Commercially available the obtaining of described PVC calcium-zinc composite stabilizing agent, contains calcium stearate, zinc stearate, hydrotalcite, Tissuemat E, stearic acid, antioxidant and OPE compound in composition; Commercially available the obtaining of described lead salt compound stabilizer, contains dibasic Lead Phosphite, lead stearate, tribasic lead sulfate, Tissuemat E, stearic acid, antioxidant and OPE compound in composition.
Described coupling agent is not particularly limited, and can be silane coupling agent or aluminium titante coupling agent;
Described composite foamable agent is commercially available to be obtained, and contains Celogen Az, sodium acid carbonate and zinc oxide etc. in composition.
Described blowing promotor is the multiple copolymer of molecular weight 5,000,000 ~ 6,000,000 esters of acrylic acid.
The thickness of ASA layer is 0.25 ~ 0.45mm, and PVC Wood-plastic foam substrate layer thickness is 5 ~ 50mm.
The processing and forming technology of this PVC Wood-plastic foam co-extrusion section bar is:
A, filler is added in high speed mixing smelting machine, at 110-120 DEG C of temperature, filler is dried to 8-10 minute, then add coupling agent Activation filling 5 minutes, enter and be coldly mixedly cooled to room temperature, discharge cold for subsequent use after mixed.
B, start high mixed and by the PVC(100Kg measuring) and compound stabilizer drops into high mixing by feeding system, after material is warming up to 90 ~ 95 DEG C by high-speed stirred, activated filler (50 ~ 100 Kg) and blowing promotor are added simultaneously and highly mixedly add composite foamable agent after continuing to be mixed to 100 ~ 105 DEG C, continuing to be mixed to 115 ~ 125 DEG C enters cold mixed, compound enters after cold mixing, while being fully cooled to below 40 DEG C through stirring, entering truck one-tenth can foam mixture.
Foam mixture requires: outward appearance: be uniformly dispersed, color and luster is consistent, does not have the phenomenon such as conglomeration, variable color.Water content: water content should be controlled at below 1%.
Bulk density: the bulk density of compound should be controlled at 0.65 ~ 0.75g/mL.
C, this compound is dropped in conical double screw extruder hopper, extrude Wood-plastic foam melt through extruder and enter foaming co-extruding mould.
D, ASA particulate material is added in single screw rod hopper, extrude ASA melt through extruder and enter foaming co-extruding mould.
E, PVC Wood-plastic foam melt and ASA melt enter same foaming co-extruding mould by different runners respectively, and in specially designed co-extruding mould, carry out composite molding.
After f, extrusion molding in cooler-shaper cooling and shaping, then obtain product through traction, cutting.
In technique, should be noted that: foaming mould is releasing pattern progressively, die gap multiplication factor can be 1.5 ~ 2.5 times, determines burst size according to different foaming floor desired density, and extruded foaming materials is through cooling and shaping sync pulling, customized cut-off becomes required size, and expanded material density is at 0.6-0.7g/cm
3between.
Embodiment 1
PVC Wood-plastic foam substrate layer raw material:
100 parts of polyvinyl chloride;
50 parts of wood powders;
1.0 parts of coupling agents (silane coupling agent);
5 parts of compound stabilizers (PVC calcium-zinc composite stabilizing agent);
1.0 parts of composite foamable agents;
6 parts of blowing promotors.
A, wood powder is added in high speed mixing smelting machine, at 110-120 DEG C of temperature, wood powder is dried to 8-10 minute, then add coupling agent activation wood powder 5 minutes, enter and be coldly mixedly cooled to room temperature, discharge cold for subsequent use after mixed.
B, start high mixed and by the PVC(100Kg measuring) and compound stabilizer drops into high mixing by feeding system, after material is warming up to 90 ~ 95 DEG C by high-speed stirred, activated wood powder (50 Kg) and blowing promotor are added simultaneously and highly mixedly add composite foamable agent after continuing to be mixed to 100 ~ 105 DEG C, continuing to be mixed to 115 ~ 125 DEG C enters cold mixed, compound enters after cold mixing, while being fully cooled to below 40 DEG C through stirring, entering truck one-tenth can foam mixture.
Foam mixture requires: outward appearance: be uniformly dispersed, color and luster is consistent, does not have the phenomenon such as conglomeration, variable color.Water content: water content should be controlled at below 1%.
Bulk density: the bulk density of compound should be controlled at 0.65 ~ 0.75g/mL.
C, this compound is dropped in Φ 65/132 conical double screw extruder.Extrude Wood-plastic foam melt through extruder and enter foaming co-extruding mould.
Heating-up temperature is: 165 DEG C, a district, 170 DEG C, 2nd district, 175 DEG C, 3rd district, 180 DEG C, 4th district, 170 DEG C of merging cores, 180 DEG C of heads
Melt pressure 12-15Mpa;
Melt temperature 165-170 DEG C;
Engine speed 10-15rpm/min.
D, ASA particulate material is added in single screw rod hopper, extrude ASA melt through extruder and enter foaming co-extruding mould
Heating-up temperature is: 165 DEG C, a district, 175 DEG C, 2nd district, 185 DEG C, 3rd district, 180 DEG C of merging cores, 190 DEG C of heads, engine speed 8 ~ 12 rpm/min.
E, PVC Wood-plastic foam melt and ASA melt enter 26 plate foaming co-extruding moulds by runner separately respectively, and in co-extruding mould, carry out composite molding.
After f, extrusion molding in cooler-shaper cooling and shaping, be shaped to continuous uniform Wood-plastic foam co-extrusion 26 plates of foaming micropore that distribute, then obtain product through traction, cutting.
The equal coextrusion mold of upper and lower surface of the PVC Wood-plastic foam substrate layer of products obtained therefrom has ASA layer, and ASA layer thickness is 0.25 ~ 0.45mm, PVC Wood-plastic foam substrate layer thickness 26mm, and the heavy 2.35-2.45kg/m of product rice, density is 0.65-0.70 g/cm
3.After measured, the physical property of product is as follows:
Nail-holding ability plate face 1780N;
Edges of boards 1620N;
0 of falling ball impact test at low temperature;
Surface abrasion resistance 0.072g/100r;
Thermal coefficient of expansion 1.54 × 10
-5;
Oxygen index (OI) 29;
Thermal conductivity factor 0.062W/(m.k);
1000 hours aging Δ E 0.62.
Embodiment 2
PVC Wood-plastic foam substrate layer raw material:
100 parts of polyvinyl chloride;
75 parts of wood powders;
1.25 parts of coupling agents (aluminium titante coupling agent);
6 parts of compound stabilizers (PVC calcium-zinc composite stabilizing agent);
1.25 parts of composite foamable agents;
7 parts of blowing promotors.
A, wood powder is added in high speed mixing smelting machine, at 110-120 DEG C of temperature, wood powder is dried to 8-10 minute, then add coupling agent activation wood powder 5 minutes, enter and be coldly mixedly cooled to room temperature, discharge cold for subsequent use after mixed.
B, start high mixed and by the PVC(100Kg measuring) and compound stabilizer drops into high mixing by feeding system, after material is warming up to 90 ~ 95 DEG C by high-speed stirred, activated wood powder (75 Kg) and blowing promotor are added simultaneously and highly mixedly add composite foamable agent after continuing to be mixed to 100 ~ 105 DEG C, continuing to be mixed to 115 ~ 125 DEG C enters cold mixed, compound enters after cold mixing, while being fully cooled to below 40 DEG C through stirring, entering truck one-tenth can foam mixture.
Foam mixture requires: outward appearance: be uniformly dispersed, color and luster is consistent, does not have the phenomenon such as conglomeration, variable color.Water content: water content should be controlled at below 1%.
Bulk density: the bulk density of compound should be controlled at 0.65 ~ 0.75g/mL.
C, this compound is dropped in Φ 65/132 conical double screw extruder.Extrude Wood-plastic foam melt through extruder and enter foaming co-extruding mould.
Heating-up temperature is: 165 DEG C, a district, 170 DEG C, 2nd district, 175 DEG C, 3rd district, 180 DEG C, 4th district, 170 DEG C of merging cores, 180 DEG C of heads
Melt pressure 12-15Mpa;
Melt temperature 165-170 DEG C;
Engine speed 10-15rpm/min.
D, ASA particulate material is added in single screw rod hopper, extrude ASA melt through extruder and enter foaming co-extruding mould
Heating-up temperature is: 165 DEG C, a district, 175 DEG C, 2nd district, 185 DEG C, 3rd district, 180 DEG C of merging cores, and 190 DEG C of heads, engine speed 6 ~ 8 turns.
E, PVC Wood-plastic foam melt and ASA melt enter chair batten foaming co-extruding mould by runner separately respectively, and in co-extruding mould, carry out composite molding.
After f, extrusion molding in cooler-shaper cooling and shaping, be shaped to the continuous uniform Wood-plastic foam co-extrusion chair bar of foaming micropore that distributes, then obtain product through traction, cutting.
The equal coextrusion mold of upper and lower surface of the PVC Wood-plastic foam substrate layer of products obtained therefrom has ASA layer, and ASA layer thickness is 0.25 ~ 0.45mm, PVC Wood-plastic foam substrate layer thickness 25.4mm, and product rice weighs 1.45 ~ 1.50kg/m, and density is 0.65 ~ 0.70 g/cm
3.After measured, the physical property of product is as follows:
Nail-holding ability plate face 1780N;
Edges of boards 1620N;
0 of falling ball impact test at low temperature;
Surface abrasion resistance 0.072g/100r;
Thermal coefficient of expansion 1.54 × 10
-5;
Oxygen index (OI) 29;
Thermal conductivity factor 0.062W/(m.k);
1000 hours aging Δ E 0.62.
Embodiment 3
PVC Wood-plastic foam substrate layer raw material:
100 parts of polyvinyl chloride;
100 parts of wood powders;
1.5 parts of coupling agents (silane coupling agent);
7 parts of compound stabilizers (lead salt compound stabilizer);
1.5 parts of composite foamable agents;
8 parts of blowing promotors.
A, wood powder is added in high speed mixing smelting machine, at 110-120 DEG C of temperature, wood powder is dried to 8-10 minute, then add coupling agent activation wood powder 5 minutes, enter and be coldly mixedly cooled to room temperature, discharge cold for subsequent use after mixed.
B, start high mixed and by the PVC(100Kg measuring) and compound stabilizer drops into high mixing by feeding system, after material is warming up to 90 DEG C by high-speed stirred, activated wood powder (100 Kg) and blowing promotor are added simultaneously and highly mixedly add composite foamable agent after continuing to be mixed to 100 ~ 110 DEG C, continuing to be mixed to 115--125 DEG C enters cold mixed, compound enters after cold mixing, while being fully cooled to below 40 DEG C through stirring, entering truck one-tenth can foam mixture.
C, this compound is dropped in Φ 65/132 conical double screw extruder.Extrude Wood-plastic foam melt through extruder and enter foaming co-extruding mould.
Heating-up temperature is: 165 DEG C, a district, 170 DEG C, 2nd district, 175 DEG C, 3rd district, 180 DEG C, 4th district, 170 DEG C of merging cores, 180 DEG C of heads
Melt pressure 12-15Mpa;
Melt temperature 165-170 DEG C;
Engine speed 10-15rpm/min.
D, ASA particulate material is added in single screw rod hopper, extrude ASA melt through extruder and enter foaming co-extruding mould.
Heating-up temperature is: 165 DEG C, a district, 175 DEG C, 2nd district, 185 DEG C, 3rd district, 180 DEG C of merging cores, 190 DEG C of heads, engine speed 6 ~ 8 rpm/min.
E, PVC Wood-plastic foam melt and ASA melt enter shiplap lagging wallboard foaming co-extruding mould by runner separately respectively, and in co-extruding mould, carry out composite molding.
After f, extrusion molding in cooler-shaper cooling and shaping, be shaped to the continuous uniform Wood-plastic foam co-extrusion shiplap lagging wall panels of foaming micropore that distributes, then obtain product through traction, cutting.
The upper surface coextrusion mold of the PVC Wood-plastic foam substrate layer of products obtained therefrom has ASA layer, and ASA layer thickness is 0.25 ~ 0.45mm, PVC Wood-plastic foam substrate layer thickness 12mm, and the heavy 1.15-1.20 kg/m of product rice, density is 0.65 ~ 0.75 g/cm
3.After measured, the physical property of product is as follows, Fundamental Physical Properties:
Nail-holding ability plate face 1780N;
Edges of boards 1620N;
0 of falling ball impact test at low temperature;
Surface abrasion resistance 0.072g/100r;
Thermal coefficient of expansion 1.54 × 10
-5;
Combustibility B1 level;
Thermal conductivity factor 0.062W/(m.k);
1000 hours aging Δ E 0.62.
The above embodiment is only the preferred embodiment for absolutely proving that the present invention lifts, and protection scope of the present invention is not limited to this.What those skilled in the art did on basis of the present invention is equal to alternative or conversion, all within protection scope of the present invention.Protection scope of the present invention is as the criterion with claims.
Claims (8)
1. prepare the method for PVC Wood-plastic foam composite for one kind, described PVC Wood-plastic foam composite, comprise PVC Wood-plastic foam substrate layer and the coextrusion mold at least ASA layer of one side at described PVC Wood-plastic foam substrate layer, wherein, described PVC Wood-plastic foam substrate layer comprises the component of following parts by weight:
100 parts of polyvinyl chloride;
50 ~ 100 parts of fillers;
1 ~ 1.5 part of coupling agent;
5 ~ 7 parts of compound stabilizers;
1.0 ~ 1.5 parts of composite foamable agents;
6 ~ 8 parts of blowing promotors;
It is characterized in that, comprise the steps:
A. the filler of getting described amount is dried, and adds coupling agent to activate described filler, and mixture is cooled to room temperature;
B. polyvinyl chloride and the compound stabilizer of getting described amount mix, stirring is warming up to 90 ~ 95 DEG C, then add the blowing promotor of step a gained mixture and described amount, stirring is warming up to 100 ~ 105 DEG C, add the composite foamable agent of described amount, continue stirring and be warming up to 115 ~ 125 DEG C, be then cooled to below 40 DEG C, obtain foam mixture;
C. foam mixture step b being obtained drops in extruder, and the Wood-plastic foam melt of extruding through extruder enters foaming co-extruding mould;
D. get ASA particulate material and drop in extruder, the ASA melt of extruding through extruder enters the foaming co-extruding mould described in step c;
E. the Wood-plastic foam melt of step c and the composite molding in described foaming co-extruding mould of the ASA melt of steps d, cooling, and cutting, to obtain final product.
2. method according to claim 1, is characterized in that, the water content of foam mixture is below 1% described in step b, and bulk density is 0.65 ~ 0.75g/mL.
3. method according to claim 1, is characterized in that, the foam mixture described in step c drops into conical double screw extruder, engine speed 10-15rpm/min.
4. method according to claim 3, is characterized in that, the ASA particulate material described in steps d drops into single screw extrusion machine, engine speed 8-12rpm/min.
5. method according to claim 1, is characterized in that, the co-extruding mould that foams described in step e is for releasing pattern progressively, and die gap multiplication factor is 1.5 ~ 2.5.
6. method according to claim 1, is characterized in that, the K value 61 of described polyvinyl chloride, and the degree of polymerization is 750 ~ 850; Described filler is one or more any mixture in calcium carbonate, talcum powder or granule or fibrous material rice wheat husk powder, wood chips, bamboo bits, crops tangerine bar powder, beans, cornstarch, cotton shell, nut duricrust or coconut husk; Described compound stabilizer is one or more any mixture in PVC calcium-zinc composite stabilizing agent or lead salt compound stabilizer; Described coupling agent is silane coupling agent or aluminium titante coupling agent; Described composite foamable agent contains Celogen Az, sodium acid carbonate and zinc oxide; Described blowing promotor is the multiple copolymer of molecular weight 5,000,000 ~ 6,000,000 esters of acrylic acid.
7. method according to claim 6, is characterized in that, described calcium-zinc composite stabilizing agent contains calcium stearate, zinc stearate, hydrotalcite, Tissuemat E, stearic acid, antioxidant and OPE compound; Described lead salt compound stabilizer contains dibasic Lead Phosphite, lead stearate, tribasic lead sulfate, Tissuemat E, stearic acid, antioxidant and OPE compound.
8. method according to claim 1, is characterized in that, the thickness of described ASA layer is 0.25 ~ 0.45mm, and PVC Wood-plastic foam substrate layer thickness is 5 ~ 50mm.
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| CN201110320450.5A CN102501506B (en) | 2011-10-20 | 2011-10-20 | PVC (Poly Vinyl Chloride) wood-plastic foaming composite and preparation method thereof |
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| CN102501506A (en) | 2012-06-20 |
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