CN109337275A - Adulterate the rufous composite material and preparation method of manganese tungstate modified ASA - Google Patents
Adulterate the rufous composite material and preparation method of manganese tungstate modified ASA Download PDFInfo
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- CN109337275A CN109337275A CN201811046574.7A CN201811046574A CN109337275A CN 109337275 A CN109337275 A CN 109337275A CN 201811046574 A CN201811046574 A CN 201811046574A CN 109337275 A CN109337275 A CN 109337275A
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- rufous
- composite material
- filler
- asa
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L51/00—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
- C08L51/04—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers grafted on to rubbers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The present invention discloses a kind of ASA rufous composite material and preparation method that doping manganese tungstate is modified, the composition and weight percentage of rufous composite material are as follows: ASA resin, 84.05~90.35, rufous filler, 9~15, coupling agent A, 0.05~0.20, coupling agent B, 0.1~0.25, lubricant, 0.5, wherein, the rufous filler is formula M n0.7Zn0.3MoxW1‑xO4Powder, in formula, x=0.0,0.1,0.3 or 0.5.The rufous composite material of doping manganese tungstate modified ASA of the invention, heat aging property is good, environmental-friendly, while assigning ASA plastic product rufous, has widened chromatography.
Description
Technical field
The invention belongs to infrared composite material technical field, especially a kind of heat aging property is good, environmental-friendly mixes
The rufous composite material and preparation method of miscellaneous manganese tungstate modified ASA.
Background technique
Plastics when outdoor is irradiated by sunlight can sharply aging, in addition to air middle-ultraviolet lamp and oxygen cause ageing of plastics
Outside, the near infrared light in sunlight equally influences plastic ageing significantly.Since in entire solar spectrum, near infrared region
(700-2500nm) accounts for the 52% of gross energy, and therefore, the energy accumulation of near infrared region will lead to frosting temperature to frosting
Degree steeply rises, and then accelerated ageing process, this namely plastics aging due to heat.So if plastics can be improved close red
The reflectivity of wave section, it will be able to reduce the surface temperature of the plastic products under sunlight irradiation, this is also advantageous for delaying to mould
The aging of material products.And an effective way for improving plastic products near infrared band reflectivity is exactly, during the preparation process
Near-infrared reflection pigment is added.
Currently, domestic and foreign scholars can be carried out some researchs to the heat-resistant aging of ASA resin.For example, village Yadong will
After ASA resin, ketone-based resins, inorganic additive, styrene-grafted maleic anhydride, antioxidant, light stabilizer mix, twin-screw is used
Extruder is prepared for Heat-resistant ASA plastic alloy, and the plastic alloy is in the base for keeping former ASA resin good weatherability properties and mechanical performance
On plinth, also have good heat resistance and mechanical strength (CN103497474- Heat-resistant ASA plastic alloy and preparation method thereof,
2014).As described above, research institution, generally by addition antioxidant, some organic additives such as light stabilizer improve ASA
The heat aging property of plastic products, and by addition colorant, assign product various colors.
However, problem of the existing technology is: infrared composite material improves the resistance to of plastics by addition heat-proof modifier
Heat aging performance assigns product color by adding colorant, and these additives contain toxic mostly, are not able to satisfy environment
The requirement of protection.
Summary of the invention
The purpose of the present invention is to provide a kind of rufous composite material for adulterating manganese tungstate modified ASA, heat-resistant agings
Can be good, environmental-friendly, while ASA plastic product rufous is assigned, widen chromatography.
Another object of the present invention is to provide a kind of preparation sides of rufous composite material for adulterating manganese tungstate modified ASA
Method.
The technical solution for realizing the aim of the invention is as follows:
A kind of ASA rufous composite material that doping manganese tungstate is modified, composition and weight percentage are as follows:
ASA resin, 84.05~90.35,
Rufous filler, 9~15,
Coupling agent A, 0.05~0.20,
Coupling agent B, 0.1~0.25,
Lubricant, 0.5,
Wherein, the rufous filler is formula M n0.7Zn0.3MoxW1-xO4Powder, in formula, x=0.0,0.1,0.3 or
0.5。
Preferably, the coupling agent A is gamma-aminopropyl-triethoxy-silane.
The coupling agent B is isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate esters.
The lubricant is atoleine.
Realize the technical solution of another object of the present invention are as follows:
A kind of preparation method for adulterating manganese tungstate modified ASA rufous composite material, includes the following steps:
(10) it prepares rufous filler: the raw material of rufous filler being uniformly mixed, hydro-thermal process, washing, drying, obtained
Rufous filler powder, for use；
Described (10) prepare rufous filler step
(11) raw material mixes: first by MnCO3It is added in the dilute hydrochloric acid of pH=3 and stirs evenly；Then Zn is added thereto5
(OH)6(CO3)2, continue stirring and generate a large amount of white chunks precipitatings；To its ultrasonic disperse 5min, it is dispersed into lumpy precipitate tiny
Particle forms uniform MnCO3-Zn5(OH)6(CO3)2- HCl suspension；By Na2WO4·2H2O and Na2MoO4·2H2O dissolution
In deionized water, compound concentration is respectively the mixed solution of 0.02mol/L~0.04mol/L, 0~0.02mol/L, then will
Mixed solution is added to MnCO3-Zn5(OH)6(CO3)2In-HCl suspension, stirring 15min is uniformly mixed it；With pH=1's
Dilute hydrochloric acid adjusts pH to 5, is transferred in reaction kettle；
In (11) the raw material mixing step, MnCO3It is 1 gram of MnCO with dilute hydrochloric acid ratio3/ 300ml dilute hydrochloric acid.
(12) hydro-thermal process: aforesaid reaction vessel is put into baking oven, 150 DEG C of heat preservation 6h；
(13) it washs: taking out reaction kettle natural cooling at room temperature, then successively respectively washed 2 times with deionized water and dehydrated alcohol；
(14) dry: above-mentioned washed powder is placed in oven and dried；Drying temperature is 100 DEG C, and drying time is
2~4h.
(20) it adulterates manganese tungstate: according to the ratio dissolving coupling agent A, B, be added in rufous filler powder, mixing, drying,
It after obtaining rufous filler solid, and is mixed in ASA resin, ethyl acetate is added, mixes, form, dry, it is reddish brown to obtain finished product
Color composite material.
Described (20) adulterate manganese tungstate step
(21) prepared by filler solid: after coupling agent A and B are dissolved in dehydrated alcohol formation mixed solution according to the ratio, being added to
It in rufous filler powder, is uniformly mixed, is placed in baking oven dry, so that dehydrated alcohol sufficiently volatilize and obtain rufous filler and consolidate
Body；
In (21) the filler solid preparation step, the total weight ratio of dehydrated alcohol and coupling agent is 100:1.
(22) resin mixes: rufous filler solid being added in ASA resin and is uniformly mixed；
(23) finished product prepare: be added into above-mentioned uniformly mixed ASA resin, rufous filler solid mixture with profit
The ethyl acetate that lubrication prescription mixes, mixes them thoroughly under grinding condition, forms, dries in a natural environment, obtain into magenta
Brown composite material.
In (23) the finished product preparation step, the weight ratio of ethyl acetate and ASA are 1:1.5.
Compared with prior art, the present invention its remarkable advantage are as follows:
1, heat aging property is good: composite material prepared by the present invention, compared with existing ASA resin, can be improved close red
Outer solar reflectivity is up to 28.31%, with the performance that better trap heat is accumulated in surface of plastic products, to reduce plastics
The surface temperature of product effectively delays the aging of plastic products；
2, composite material is in rufous: the modified ASA resin of doping manganese tungstate can assign ASA plastic product rufous, subtract
The addition of colorant is lacked；
3, environmental-friendly: to be free of heavy metallic oxide and toxic additive, be conducive to environmental protection and human health；
The present invention is described in further detail with reference to the accompanying drawings and detailed description.
Detailed description of the invention
Fig. 1 is the doping manganese tungstate modified ASA rufous composite material and the pure ASA plastic of comparative example of embodiment 1-4 preparation
Near-infrared spectral reflectance figure.
Specific embodiment
For convenient for it is further understood that the present invention, is illustrated with 4 embodiments.
Wherein, Na2MoO4·2H2O, Na2WO4·2H2O, MnCO3, Zn5(OH)6(CO3)2, hydrochloric acid, ASA resin, coupling agent
A: gamma-aminopropyl-triethoxy-silane, coupling agent B: (dioctylphyrophosphoric acid acyloxy) titanate esters of isopropyl three and atoleine
It is marketable material.
Embodiment 1
(1) preparation of rufous filler: by raw material proportioning described in table 1, by MnCO3It is added in the dilute hydrochloric acid of pH=3
Stir evenly (1 gram of MnCO3/ 300ml dilute hydrochloric acid)；Then Zn is added thereto5(OH)6(CO3)2, it is a large amount of white to continue stirring generation
Color lumpy precipitate；Ultrasonic disperse 5min, makes lumpy precipitate be dispersed into fine particle, forms uniform MnCO3-Zn5(OH)6
(CO3)2- HCl suspension；By Na2WO4·2H2O is dissolved in deionized water, and compound concentration is the solution of 0.04mol/L, then
Solution is added to MnCO3-Zn5(OH)6(CO3)2In-HCl suspension, stirring 15min is uniformly mixed it；It is dilute with pH=1
Salt acid for adjusting pH is transferred in reaction kettle to 5；Reaction kettle is put into baking oven, 150 DEG C of heat preservation 6h；Natural cooling at room temperature,
It is successively respectively washed 2 times with deionized water and dehydrated alcohol again；Powder after washing is put into 100 DEG C of baking oven dry 3h.
(2) it adulterates the preparation of manganese tungstate modified ASA rufous composite material: being matched according to 2 rufous composite material of table, it will
Coupling agent A and B are dissolved in dehydrated alcohol (total weight of dehydrated alcohol and coupling agent ratio is 100:1) and form mixed solution；By this
Mixed solution, which is added in rufous filler, is uniformly mixed coupling agent and filler, then places it in dry 2h in 80 DEG C of baking ovens
So that dehydrated alcohol is sufficiently volatilized and obtains brown filler；Processed brown filler is added in ASA resin and is uniformly mixed, Xiang Qi
The ethyl acetate solvent (weight ratio of ethyl acetate and ASA are 1:1.5) that middle addition has been mixed with lubricant, grinding uniformly makes
Its is fully dispersed；Being placed in die for molding is sheet, is dried under natural environment to get the rufous composite material of embodiment 1 is arrived.
Embodiment 2,3,4 presses above-mentioned steps, and required each raw material proportioning is shown in Table shown in 1 and table 2.
1 general formula of table is Mn0.7Zn0.3MoxW1-xO4Rufous filler material with when component list
2 rufous composite material of table proportion
To examine the present invention to adulterate the near-infrared reflection performance of manganese tungstate modified ASA rufous composite material, to assess it
Heat aging property presses the rufous composite material in embodiment described in table 2 and embodiment phase with by commercially available ASA resin
With method made from compared with material (comparative example).Wherein, test reflectivity instrument is ultraviolet-visible-near-infrared point
Light photometer (Shimadzu, Japan, UV-3600), BaSO4For reference substance, 1nm is divided between test wavelength.
Fig. 1 is the Mn of embodiment 1-4 preparation0.7Zn0.3MoxW1-xO4/ ASA rufous composite material and the pure ASA modeling of comparative example
The near-infrared spectral reflectance figure of material.It can be seen from the figure that Mn0.7Zn0.3MoxW1-xO4The reflectivity of/ASA rufous composite material
Pure ASA plastic is above near infrared band (780-2500nm).From table 3 it is observed that the near-infrared sun of embodiment 4
Reflectivity is up to 63.29%, is far longer than the 34.98% of pure ASA plastic (comparative example).This explanation is anti-by rufous near-infrared
Penetrate pigment Mn0.7Zn0.3MoxW1-xO4Modification can greatly improve reflection of the ASA plastic near infrared region solar energy, effectively drop
Accumulation low in calories in surface of plastic products, to slow down the aging of outdoor ASA plastic product.
Wherein, near-infrared solar reflectivity is calculated by standard ASTM G-159-98, and calculation formula is such as
Under:
Wherein, r (λ) is to test the reflectivity measured in af at wavelength lambda, i (λ) (Wm-2·nm-1) it is af at wavelength lambda sunlight
Standard pyranometer (by standard ASTM G-159-98 obtain).
The near-infrared solar reflectivity of the doping manganese tungstate modified ASA rufous composite material of table 3
Test the chromatic value L of composite material*, a*, b*Instrument is the NH310 type color difference meter of three En Chi company of Shenzhen, color
Poor instrument is according to the measuring principle of the CIE colour space, and each color has its specific L*, a*, b*It is worth, wherein L*Represent brightness, range
For 0-100, L*The size of value represents the height of brightness.a*It is worth the green red phase property of (- 128 -+128) expression pigment, negative value indicates
Green phase, positive value indicate red phase.b*Being worth (- 128 -+128) indicates that the yellow phase property of the indigo plant of pigment, negative value indicate that blue phase, positive value indicate
Huang Xiang.Instrument carries out to blackboard correction and blank correction respectively, when test converts test position, is divided into 1- between measurement before test
2s takes the average value of test result three times.
The L of the doping manganese tungstate modified ASA rufous composite material of table 4*, a*, b*Value
| Embodiment | 1 | 2 | 3 | 4 |
| L* | 50.5 | 46.21 | 42.83 | 40.71 |
| a | 5.96 | 11.39 | 16.11 | 18.49 |
| b* | 10.50 | 18.78 | 18.10 | 18.22 |
L*: brightness；a*: green-red index；b*: blue-yellow index；
Table 4 is the L for adulterating manganese tungstate modified ASA rufous composite material*, a*, b*Value.It can be seen from the table, embodiment 1-4
A*Value is positive value, illustrates that composite material exhibits are red phase；b*Value is also positive value, illustrates composite material exhibits for yellow phase；L*
Value is gradually reduced, and illustrates that composite material is gradually dimmed, L*, a*, b*The color that the effect of value is eventually exhibited as composite material is reddish brown
Color.
Doping manganese tungstate modified ASA rufous composite material of the invention can be mentioned significantly by adulterating the modification of manganese tungstate
Heat reflection of the high ASA plastic to the sun reduces the surface temperature of plastic products, effectively slows down the aging of plastic products, assign simultaneously
Plastic products rufous is given, the addition of colorant is reduced.Heavy metallic oxide and toxic addition are free of in raw material and finished product
Agent is conducive to environmental protection and human health, can be widely used in the outer plastic device of make-up room.
Claims (10)
1. a kind of rufous composite material for adulterating manganese tungstate modified ASA, composition and weight percentage are as follows:
ASA resin, 84.05~90.35,
Rufous filler, 9~15,
Coupling agent A, 0.05~0.20,
Coupling agent B, 0.1~0.25,
Lubricant, 0.5,
Wherein, the rufous filler is formula M n0.7Zn0.3MoxW1-xO4Powder, in formula, x=0.0,0.1,0.3 or 0.5.
2. rufous composite material according to claim 1, it is characterised in that:
The coupling agent A is gamma-aminopropyl-triethoxy-silane.
3. rufous composite material according to claim 1, it is characterised in that:
The coupling agent B is isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate esters.
4. rufous composite material according to claim 1, it is characterised in that:
The lubricant is atoleine.
5. a kind of preparation method of the doping manganese tungstate modified ASA rufous composite material as described in Claims 1-4, special
Sign is, includes the following steps:
(10) it prepares rufous filler: the raw material of rufous filler being uniformly mixed, hydro-thermal process, washing, drying, obtained reddish brown
Color filler powder, for use；
(20) it adulterates manganese tungstate: according to the ratio dissolving coupling agent A, B, be added in rufous filler powder, mixing, drying obtain
It after rufous filler solid, and is mixed in ASA resin, ethyl acetate is added, mixes, form, dry, it is multiple to obtain finished product rufous
Condensation material.
6. the preparation method of rufous composite material according to claim 5, which is characterized in that (10) prepare reddish brown
Color filler step includes:
(11) raw material mixes: first by MnCO3It is added in the dilute hydrochloric acid of pH=3 and stirs evenly；Then Zn is added thereto5(OH)6
(CO3)2, continue stirring and generate a large amount of white chunks precipitatings；To its ultrasonic disperse 5min, lumpy precipitate is made to be dispersed into fine particle,
Form uniform MnCO3-Zn5(OH)6(CO3)2- HCl suspension；By Na2WO4·2H2O and Na2MoO4·2H2O be dissolved in from
In sub- water, compound concentration is respectively the mixed solution of 0.02mol/L~0.04mol/L, 0~0.02mol/L, then will be mixed molten
Liquid is added to MnCO3-Zn5(OH)6(CO3)2In-HCl suspension, stirring 15min is uniformly mixed it；With the dilute hydrochloric acid of pH=1
PH to 5 is adjusted, is transferred in reaction kettle；
(12) hydro-thermal process: aforesaid reaction vessel is put into baking oven, 150 DEG C of heat preservation 6h；
(13) it washs: taking out reaction kettle natural cooling at room temperature, then successively respectively washed 2 times with deionized water and dehydrated alcohol；
(14) dry: above-mentioned washed powder is placed in oven and dried；Drying temperature be 100 DEG C, drying time be 2~
4h。
7. the preparation method of rufous composite material according to claim 6, which is characterized in that (11) the raw material mixing
In step, MnCO3It is 1 gram of MnCO with dilute hydrochloric acid ratio3/ 300ml dilute hydrochloric acid.
8. the preparation method of rufous composite material according to claim 5, which is characterized in that described (20) adulterate wolframic acid
Manganese step includes:
(21) prepared by filler solid: after coupling agent A and B are dissolved in dehydrated alcohol formation mixed solution according to the ratio, being added to reddish brown
It in color filler powder, is uniformly mixed, is placed in drying in baking oven, so that dehydrated alcohol is sufficiently volatilized and obtain rufous filler solid；
(22) resin mixes: rufous filler solid being added in ASA resin and is uniformly mixed；
(23) finished product prepare: be added into above-mentioned uniformly mixed ASA resin, rufous filler solid mixture with lubricant
The ethyl acetate of mixing mixes them thoroughly under grinding condition, and molding dries in a natural environment, obtains finished product rufous
Composite material.
9. the preparation method of rufous composite material according to claim 8, which is characterized in that (21) the filler solid
In preparation step, the total weight ratio of dehydrated alcohol and coupling agent is 100:1.
10. the preparation method of rufous composite material according to claim 8, which is characterized in that (23) the finished product system
In standby step, the weight ratio of ethyl acetate and ASA are 1:1.5.
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| CN201811046574.7A CN109337275B (en) | 2018-09-08 | 2018-09-08 | Manganese tungstate-doped modified ASA (acrylonitrile styrene acrylate) reddish brown composite material and preparation method thereof |
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| CN201811046574.7A CN109337275B (en) | 2018-09-08 | 2018-09-08 | Manganese tungstate-doped modified ASA (acrylonitrile styrene acrylate) reddish brown composite material and preparation method thereof |
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| WO2009096165A1 (en) * | 2008-01-31 | 2009-08-06 | Panasonic Corporation | Optical information recording medium, method for manufacturing the same, and target thereof |
| CN106963951A (en) * | 2017-02-27 | 2017-07-21 | 上海师范大学 | Graphene oxide/manganese tungstate/polyethylene glycol nano-hybrid material and its preparation |
| CN108083324A (en) * | 2017-12-25 | 2018-05-29 | 畅的新材料科技（上海）有限公司 | A kind of doped stannum oxide material of near-infrared reflection and preparation method thereof |
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2018
- 2018-09-08 CN CN201811046574.7A patent/CN109337275B/en active Active
Patent Citations (4)
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| CN1745149A (en) * | 2003-10-20 | 2006-03-08 | 住友金属矿山株式会社 | Infrared shielding material microparticle dispersion, infrared shield, process for producing infrared shielding material microparticle, and infrared shielding material microparticle |
| WO2009096165A1 (en) * | 2008-01-31 | 2009-08-06 | Panasonic Corporation | Optical information recording medium, method for manufacturing the same, and target thereof |
| CN106963951A (en) * | 2017-02-27 | 2017-07-21 | 上海师范大学 | Graphene oxide/manganese tungstate/polyethylene glycol nano-hybrid material and its preparation |
| CN108083324A (en) * | 2017-12-25 | 2018-05-29 | 畅的新材料科技（上海）有限公司 | A kind of doped stannum oxide material of near-infrared reflection and preparation method thereof |
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