CN101475726B - Polymethyl methacryate microsphere coating zinc oxide composite material and preparation thereof - Google Patents
Polymethyl methacryate microsphere coating zinc oxide composite material and preparation thereof Download PDFInfo
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- CN101475726B CN101475726B CN2009100954150A CN200910095415A CN101475726B CN 101475726 B CN101475726 B CN 101475726B CN 2009100954150 A CN2009100954150 A CN 2009100954150A CN 200910095415 A CN200910095415 A CN 200910095415A CN 101475726 B CN101475726 B CN 101475726B
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- Prior art keywords
- zinc oxide
- solution
- composite material
- methyl methacrylate
- sphere
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 239000004005 microsphere Substances 0.000 title claims abstract description 35
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000002131 composite material Substances 0.000 title claims abstract description 7
- 239000011248 coating agent Substances 0.000 title claims description 10
- 238000000576 coating method Methods 0.000 title claims description 10
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims abstract description 39
- 239000004926 polymethyl methacrylate Substances 0.000 claims abstract description 39
- 239000000243 solution Substances 0.000 claims abstract description 29
- 238000003756 stirring Methods 0.000 claims abstract description 18
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 9
- 150000003751 zinc Chemical class 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 210000002966 serum Anatomy 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 5
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000011159 matrix material Substances 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 5
- 239000012456 homogeneous solution Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 5
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 claims description 4
- 239000012670 alkaline solution Substances 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 2
- 239000011259 mixed solution Substances 0.000 abstract 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 abstract 1
- 239000003513 alkali Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 14
- 239000000463 material Substances 0.000 description 9
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- 230000006750 UV protection Effects 0.000 description 1
- -1 acryl Chemical group 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Manufacturing Of Micro-Capsules (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a polymethyl methacrylate microsphere coated zinc oxide composite material and a preparation method thereof. The method comprises the following steps: a PMMA microsphere is added into an aqueous ammonia solution, and the PMMA microsphere is evenly dispersed in the solution by stirring, wherein the concentration of the PMMA microsphere is between 1 and 50 gram/liter, and the concentration of the aqueous ammonia is between 20 and 880 gram/liter; soluble zinc salt is dissolved in deionized water, and an even solution can be obtained by stirring the mixed solution, wherein the concentration of zinc ions is between 0.01 and 0.5 mol/liter; the two solutions are mixed; pH value of the mixed solution is adjusted at between 7.5 and 10 by aqueous alkali; the mixed serum is subjected to a water-bath reaction at a temperature of between 60 and 100 DEG C at a stirring speed of between 0 and 1,000 revolution/minute for 30 minutes to 24 hours; and the treated solution is centrifugated and dried to obtain the polymethyl methacrylate microsphere coated zinc oxide composite material. An obtained zinc oxide coated layer of the product is compact and even.
Description
Technical field
The present invention relates to matrix material of a kind of polymethyl methacryate microsphere coating zinc oxide and preparation method thereof.
Background technology
In recent years, the matrix material of inorganic particulate and organic polymer assembling formation is one of important topic of chemistry, physics, material science concern with its excellent comprehensive performance and synergistic effect always.Matrix material has property or the function that stock blend does not possess.Utilize the interaction of inorganic materials and polymeric matrix to produce new effect, realize the mutual supplement with each other's advantages between the two, can develop the type material of excellent performance.
Polymethylmethacrylate is called for short PMMA, is commonly called as synthetic glass, is acryl or acrylic again, is a kind of exploitation important thermoplastics early, has the transparency preferably, and transmittance reaches more than 92%, easy dyeing, and easily processing, the outward appearance grace, cheap.In addition, PMMA has splendid weathering resistance, and higher surface hardness and surface luster and excellent high all have a wide range of applications in fields such as aviation, building, agricultural, opticinstruments [old Lu Song et al. plastics, 36 (2007): 89-95].The consumption of the existing synthetic glass of China increases very fast.But since China's synthetic glass range of product dullness, comparatively small amt, second-rate, product structure is very unreasonable, can only production common variety product, lack high value added product, in the demand that all can not satisfy market aspect kind and the quality, most of products also need dependence on import.
Zinc oxide is a kind of environmentally friendly wide-band-gap semiconductor material, have the band gap (3.37eV) and the exciton bind energy (60meV) that are higher than general forbidden band material, it is luminous to produce shortwave when room temperature, it is a kind of self activation semiconductor material, can be widely used in numerous areas such as short wavelength light electrical part, varistor, transmitter, photochemical catalysis, be described as modern functions material geared to the 21st century.Thermal conductivity when in addition, the specific refractory power of zinc oxide at 589nm wavelength place is 2.02,50 ℃ is 1.16Wm
-1K
-1, specific conductivity 0.02Scm
-1, these character all are better than PMMA.Zinc oxide is compound in the surface of PMMA material, at contact clothing, the ultraviolet protection film, there is the potential application prospect in fields such as protective clear layer and fire-retardant material.And up to now, the matrix material that zinc oxide is coated on the stable nucleocapsid structure of poly (methyl methacrylate) micro-sphere surface formation does not also have bibliographical information.
Summary of the invention
The object of the present invention is to provide matrix material of a kind of poly (methyl methacrylate) micro-sphere coated with zinc oxide and preparation method thereof, with soluble zinc salt and PMMA microballoon is raw material, by the PMMA microballoon is carried out surface treatment, adopt the matrix material of the synthetic PMMA microsphere surface coating zinc oxide of solution reaction method.
The technical solution used in the present invention step is as follows:
One, a kind of poly (methyl methacrylate) micro-sphere coated with zinc oxide matrix material:
This matrix material is a nucleocapsid structure, and kernel is a poly (methyl methacrylate) micro-sphere, and shell is a zinc oxide coated layer, and the diameter of poly (methyl methacrylate) micro-sphere is 1 micron～20 microns.
Two, a kind of preparation method's of poly (methyl methacrylate) micro-sphere coated with zinc oxide matrix material step is as follows:
It is characterized in that:
1) poly (methyl methacrylate) micro-sphere is added in the ammonia soln, stirring is dispersed in the solution it, and the concentration of poly (methyl methacrylate) micro-sphere is 1～50 grams per liter, and ammonia concn is 20～880 grams per liters;
2) soluble zinc salt is dissolved in the deionized water, stirs and obtain homogeneous solution, zinc ion concentration is 0.01～0.5 mol;
3) two kinds of above-mentioned solution are mixed; Mixing solutions is regulated pH value to 7.5～10 with alkaline solution;
4) above-mentioned mixed serum is carried out water-bath, the water-bath temperature is controlled at 60 ℃～100 ℃, and stir speed (S.S.) is 0～1000 rev/min; 30 minutes～24 hours reaction times;
5), just obtained the matrix material of polymethyl methacryate microsphere coating zinc oxide with solution centrifugal, the drying handled well.
Described soluble zinc salt is the nitrate or the chlorate of zinc.
Described alkaline solution is ammoniacal liquor or sodium hydroxide solution.
The beneficial effect that the present invention has is: the present invention prepares the matrix material of poly (methyl methacrylate) micro-sphere coated with zinc oxide by a kind of simple, gentle solution methods.The product that obtains is a nucleocapsid structure, and kernel is a micron order PMMA microballoon, and shell is a zinc oxide coated layer.Have good dispersiveness, the zinc oxide coated layer densification, evenly.This method is a raw material with soluble zinc salt and PMMA microballoon, by the PMMA microsphere surface is handled, Zinc oxide particles is coated on spheric PMMA surface.The product that obtains is a nucleocapsid structure, has good dispersiveness, the zinc oxide coated layer densification, evenly.
Description of drawings
Fig. 1 is the structural representation of poly (methyl methacrylate) micro-sphere coated with zinc oxide matrix material; Among the figure, 1. zinc oxide coated layer; 2.PMMA microballoon.
Fig. 2 is the electromicroscopic photograph of used poly (methyl methacrylate) micro-sphere among the embodiment.
Fig. 3 is the XRD figure spectrum of embodiment 1 products therefrom.
Fig. 4 is the electromicroscopic photograph of embodiment 1 products therefrom.
Fig. 5 is the electromicroscopic photograph of embodiment 2 products therefroms.
Embodiment
Embodiment 1:
It is in the 20 grams per liter ammoniacal liquor that the methyl methacrylate microballoon of 5～10 microns of 0.0100g diameters is dissolved in 10mL concentration, stirs it is dispersed in the solution; The 0.1190g zinc nitrate hexahydrate is dissolved in the 40mL deionized water, stirs and obtain homogeneous solution, the zine ion total concn is 0.01 mol; Above-mentioned two kinds of solution are mixed; It is 7.5 that mixing solutions is regulated the pH value with ammoniacal liquor; This mixed serum is carried out water-bath, and the water-bath temperature is controlled at 80 ℃, and stir speed (S.S.) is 0 rev/min, 30 minutes reaction times; With solution centrifugal, the drying of handling well, just obtained the matrix material of polymethyl methacryate microsphere coating zinc oxide.Fig. 2 is the XRD figure spectrum of this product, and this collection of illustrative plates and zinc oxide standard x RD data (JCPDS No 36-1451) are coincide, and illustrate that the crystallization phases material in the product is a zinc oxide.Fig. 4 is the SEM photo of this product, PMMA microballoon in the comparison diagram 3, the obvious evengranular PMMA microsphere surface that is coated on of ZnO as can be seen, about 10 microns of sphere diameter.
Embodiment 2:
It is in the 880 grams per liter ammoniacal liquor that the methyl methacrylate microballoon of 10～20 microns of 0.5000g diameters is dissolved in 10mL concentration, stirs it is dispersed in the solution; The 5.9495g zinc nitrate hexahydrate is dissolved in the 40mL deionized water, stirs and obtain homogeneous solution, the zine ion total concn is 0.5 mol; Above-mentioned two kinds of solution are mixed; It is 10 that mixing solutions is regulated the pH value with sodium hydroxide; This mixed serum is carried out water-bath, and the water-bath temperature is controlled at 100 ℃, and stir speed (S.S.) is 1000 rev/mins, 2 hours reaction times; With solution centrifugal, the drying of handling well, just obtained the matrix material of poly (methyl methacrylate) micro-sphere coated with zinc oxide.Fig. 5 is the SEM photo of this product, PMMA microballoon in the comparison diagram 3, the obvious evengranular PMMA microsphere surface that is coated on of ZnO as can be seen, about 15 microns of sphere diameter.
Embodiment 3:
It is in the 200 grams per liter ammoniacal liquor that the methyl methacrylate microballoon of 1～5 micron of 0.3000g diameter is dissolved in 10mL concentration, stirs it is dispersed in the solution; The 1.0904g Zinc Chloride Anhydrous is dissolved in the 40mL deionized water, stirs and obtain homogeneous solution, the zine ion total concn is 0.2 mol; Above-mentioned two kinds of solution are mixed; It is 8.5 that mixing solutions is regulated the pH value with ammoniacal liquor; This mixed serum is carried out water-bath, and the water-bath temperature is controlled at 80 ℃, and stir speed (S.S.) is 300 rev/mins, 24 hours reaction times; With solution centrifugal, the drying of handling well, just obtained the matrix material of poly (methyl methacrylate) micro-sphere coated with zinc oxide.
Claims (3)
1. the preparation method of a polymethyl methacryate microsphere coating zinc oxide composite material, this matrix material is a nucleocapsid structure, kernel is a poly (methyl methacrylate) micro-sphere, and shell is a zinc oxide coated layer, and the diameter of poly (methyl methacrylate) micro-sphere is 1 micron～20 microns; The step that it is characterized in that this method is as follows:
1) poly (methyl methacrylate) micro-sphere is added in the ammonia soln, stirring is dispersed in the solution it, and the concentration of poly (methyl methacrylate) micro-sphere is 1～50 grams per liter, and ammonia concn is 20～880 grams per liters;
2) soluble zinc salt is dissolved in the deionized water, stirs and obtain homogeneous solution, zinc ion concentration is 0.01～0.5 mol;
3) two kinds of above-mentioned solution are mixed; Mixing solutions is regulated pH value to 7.5～10 with alkaline solution;
4) above-mentioned mixed serum is carried out water-bath, the water-bath temperature is controlled at 60 ℃～100 ℃, and stir speed (S.S.) is 0～1000 rev/min; 30 minutes～24 hours reaction times;
5), just obtained the matrix material of polymethyl methacryate microsphere coating zinc oxide with solution centrifugal, the drying handled well.
2. the preparation method of a kind of polymethyl methacryate microsphere coating zinc oxide composite material according to claim 1, it is characterized in that: described soluble zinc salt is the nitrate or the chlorate of zinc.
3. the preparation method of a kind of polymethyl methacryate microsphere coating zinc oxide composite material according to claim 1, it is characterized in that: described alkaline solution is ammoniacal liquor or sodium hydroxide solution.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100954150A CN101475726B (en) | 2009-01-12 | 2009-01-12 | Polymethyl methacryate microsphere coating zinc oxide composite material and preparation thereof |
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|---|---|---|---|
| CN2009100954150A CN101475726B (en) | 2009-01-12 | 2009-01-12 | Polymethyl methacryate microsphere coating zinc oxide composite material and preparation thereof |
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|---|---|
| CN101475726A CN101475726A (en) | 2009-07-08 |
| CN101475726B true CN101475726B (en) | 2010-08-18 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102786077B (en) * | 2012-07-30 | 2014-02-19 | 西安理工大学 | Preparation method for submicron cup-shaped zinc oxide crystals |
| CN104059245B (en) * | 2014-06-21 | 2016-08-17 | 江苏爱特恩东台新材料科技有限公司 | Seed deposition method prepares rubber vulcanization activating agent |
| CN113057896B (en) * | 2021-04-03 | 2022-12-16 | 江西永通科技股份有限公司 | Preparation method of sunscreen lotion |
| CN113069381B (en) * | 2021-04-03 | 2022-12-27 | 百特威(上海)化妆品有限公司 | High-efficiency sunscreen liquid |
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