CN105482336A - Expanded vermiculite modified 3D (three dimensional) printer window glass material and preparation method thereof - Google Patents
Expanded vermiculite modified 3D (three dimensional) printer window glass material and preparation method thereof Download PDFInfo
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- CN105482336A CN105482336A CN201510976009.0A CN201510976009A CN105482336A CN 105482336 A CN105482336 A CN 105482336A CN 201510976009 A CN201510976009 A CN 201510976009A CN 105482336 A CN105482336 A CN 105482336A
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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
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
- C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
- C08L33/10—Homopolymers or copolymers of methacrylic acid esters
- C08L33/12—Homopolymers or copolymers of methyl methacrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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 invention discloses an expanded vermiculite modified 3D (three dimensional) printer window glass material and a preparation method thereof. The preparation method comprises the steps of 1) under the existence of ultraviolet, dissolving nano expanded vermiculite, a complex of a structure shown in the formula (I) and graphene into N,N-dimethyl formamide, performing ultrasonic agitation to form a modified solution; 2) mixing polymethylmethacrylate, 2-Octyl-3(2H)-isothiazolone, dimethylformamide, silicon oxide, sodium gluconate, a rare-earth oxide, Fischer-Tropsch wax with the modified solution, then melting, cooling, pelleting so as to obtain the 3D printer window glass material; Mes is 2'4'6'-trimethylphenyl. The 3D printer window glass material prepared by the method has excellent mechanical property and resistance to elevated temperature. The chemical formula is shown in the description.
Description
Technical field
The present invention relates to sight glass material, particularly, 3D printer sight glass material relating to a kind of expanded vermiculite modification and preparation method thereof.
Background technology
Sight glass material divides from material, can be divided into inorganic glass materials and pmma material.Wherein, the main component of inorganic glass materials is silicate, and this kind of glass material has excellent wear-resistant and heat-resisting performance, but this kind of glass material has frangible defect.And pmma material has the advantage of excellent resistance to fracture, but its surface is to form cut, and thermotolerance is poor.
3D printer sight glass is an important assembly in 3D printer, for the ease of observing the process in printer, requirement sight glass is then needed to have excellent transmittance, tensile strength, thermotolerance and anti abrasive performance, but current glass material is difficult to meet these several requirements, and especially resistance to elevated temperatures is poor simultaneously.
Summary of the invention
3D printer sight glass material that the object of this invention is to provide a kind of expanded vermiculite modification and preparation method thereof, the 3D printer sight glass material obtained by the method has excellent mechanical property and resistance to elevated temperatures.
To achieve these goals, the invention provides a kind of preparation method of 3D printer sight glass material of expanded vermiculite modification, comprising:
1) in the presence of uv light, by nanometer expanded vermiculite, be dissolved in ultrasonic agitation in DMF such as formula the complex compound of structure (I) Suo Shi and Graphene and form modification liquid;
2) polymethyl methacrylate, octylisothiazolinone, dimethyl formamide, silicon oxide, Sunmorl N 60S, rare earth oxide, Fischer-Tropsch wax and modification liquid are mixed, then melting, cooling, granulation are with obtained 3D printer sight glass material;
Wherein, Mes is mesityl.
Present invention also offers a kind of 3D printer sight glass material of expanded vermiculite modification, this 3D printer sight glass material is prepared from by above-mentioned method.
By technique scheme, preparation method provided by the invention first by nanometer expanded vermiculite, be dissolved in ultrasonic agitation in DMF such as formula the complex compound of structure (I) Suo Shi and Graphene and form modification liquid; Then polymethyl methacrylate, octylisothiazolinone, dimethyl formamide, silicon oxide, Sunmorl N 60S, rare earth oxide, Fischer-Tropsch wax and modification liquid are mixed, then melting, cooling, granulation are with obtained 3D printer sight glass material.In the process, by the synergy between each material, make the 3D printer sight glass material obtained not only have excellent mechanical property, also there is excellent abrasion resistance properties simultaneously.In addition, this preparation method's raw material is easy to get, and step is simple.
Other features and advantages of the present invention are described in detail in embodiment part subsequently.
Embodiment
Below the specific embodiment of the present invention is described in detail.Should be understood that, embodiment described herein, only for instruction and explanation of the present invention, is not limited to the present invention.
The invention provides a kind of preparation method of 3D printer sight glass material of expanded vermiculite modification, comprising:
1) in the presence of uv light, by nanometer expanded vermiculite, be dissolved in ultrasonic agitation in DMF such as formula the complex compound of structure (I) Suo Shi and Graphene and form modification liquid;
2) polymethyl methacrylate, octylisothiazolinone, dimethyl formamide, silicon oxide, Sunmorl N 60S, rare earth oxide, Fischer-Tropsch wax and modification liquid are mixed, then melting, cooling, granulation are with obtained 3D printer sight glass material;
Wherein, Mes is mesityl.
In step 1 of the present invention) in, ultraviolet wavelength can be selected in wide scope, but in order to make the 3D printer sight glass material obtained have more excellent mechanical property and abrasion resistance properties, preferably, in step 1) in, ultraviolet wavelength is 150-200nm.
In step 1 of the present invention) in, the condition of ultrasonic agitation can be selected in wide scope, but in order to make the 3D printer sight glass material obtained, there is more excellent mechanical property and abrasion resistance properties, preferably, in step 1) in, ultrasonic agitation at least meets the following conditions: hyperacoustic frequency is 25-30KHz, and whipping temp is 55-65 DEG C, and churning time is 4-6h.
In step 1 of the present invention) in, the particle diameter of nanometer expanded vermiculite can be selected in wide scope, but in order to make the 3D printer sight glass material obtained, there is more excellent mechanical property and abrasion resistance properties, preferably, in step 1) in, the particle diameter of nanometer expanded vermiculite is 35-40nm.
In step 1 of the present invention) in, the consumption of each material can be selected in wide scope, but in order to make the 3D printer sight glass material obtained, there is more excellent mechanical property and abrasion resistance properties, preferably, in step 1) in, relative to the nanometer expanded vermiculite of 100 weight parts, consumption such as formula the complex compound of structure (I) Suo Shi is 17-26 weight part, the consumption of Graphene is 4-4.5 weight part, and the consumption of DMF is 200-280 weight part.
In step 2 of the present invention) in, the consumption of each material can be selected in wide scope, but in order to make the 3D printer sight glass material obtained, there is more excellent mechanical property and abrasion resistance properties, preferably, in step 2) in, relative to the polymethyl methacrylate of 100 weight parts, the consumption of octylisothiazolinone is 12-23 weight part, the consumption of dimethyl formamide is 8-13 weight part, the consumption of silicon oxide is 3-7 weight part, the consumption of Sunmorl N 60S is 5.5-10 weight part, the consumption of rare earth oxide is 1.2-2 weight part, the consumption of Fischer-Tropsch wax is 40-50 weight part, the consumption of modification liquid is 14-19 weight part.
In step 2 of the present invention) in, the concrete kind of rare earth oxide can be selected in wide scope, but in order to make the 3D printer sight glass material obtained, there is more excellent mechanical property and abrasion resistance properties, preferably, rare earth oxide is selected from one or more in cerous oxide, cerium dioxide, Praseodymium trioxide and rubidium oxide.
In step 2 of the present invention) in, the condition of melting can be selected in wide scope, but in order to make the 3D printer sight glass material obtained, there is more excellent mechanical property and abrasion resistance properties, preferably, in step 2) in, melting at least meets the following conditions: melt temperature is 175-185 DEG C, and the fusion time is 30-50min.
In step 2 of the present invention) in, the temperature of cooling can be selected in wide scope, but in order to make the 3D printer sight glass material obtained have more excellent mechanical property and abrasion resistance properties, preferably, in step 2) in, the temperature of cooling is 5-15 DEG C.
Present invention also offers a kind of 3D printer sight glass material of expanded vermiculite modification, this 3D printer sight glass material is prepared from by above-mentioned method.
Below will be described the present invention by embodiment.
Embodiment 1
1) under the existence of ultraviolet (wavelength is 180nm), by nanometer expanded vermiculite (particle diameter is 38nm), complex compound, Graphene, N such as formula structure (I) Suo Shi, dinethylformamide mixes according to the weight ratio of 100:20:4.7:250, and under the condition of ultrasonic (frequency is 28KHz) of 60 DEG C, stir 5h formation modification liquid;
2) polymethyl methacrylate, octylisothiazolinone, dimethyl formamide, silicon oxide, Sunmorl N 60S, rare earth oxide (cerium dioxide), Fischer-Tropsch wax and modification liquid are mixed according to the weight ratio of 100:20:10:5:8:1.7:45:16, then at 180 DEG C melting 40min, at 10 DEG C cooling, granulation with obtained 3D printer sight glass materials A 1;
Wherein, Mes is mesityl.
Embodiment 2
1) under the existence of ultraviolet (wavelength is 150nm), by nanometer expanded vermiculite (particle diameter is 35nm), complex compound, Graphene, N such as formula structure (I) Suo Shi, dinethylformamide mixes according to the weight ratio of 100:17:4:200, and under the condition of ultrasonic (frequency is 25KHz) of 55 DEG C, stir 4h formation modification liquid;
2) polymethyl methacrylate, octylisothiazolinone, dimethyl formamide, silicon oxide, Sunmorl N 60S, rare earth oxide (Praseodymium trioxide), Fischer-Tropsch wax and modification liquid are mixed according to the weight ratio of 100:12:8:3:5.5:1.2:40:14, then at 175 DEG C melting 30min, at 5 DEG C cooling, granulation with obtained 3D printer sight glass materials A 2;
Wherein, Mes is mesityl.
Embodiment 3
1) under the existence of ultraviolet (wavelength is 200nm), by nanometer expanded vermiculite (particle diameter is 40nm), complex compound, Graphene, N such as formula structure (I) Suo Shi, dinethylformamide mixes according to the weight ratio of 100:26:4.5:280, and under the condition of ultrasonic (frequency is 30KHz) of 65 DEG C, stir 6h formation modification liquid;
2) polymethyl methacrylate, octylisothiazolinone, dimethyl formamide, silicon oxide, Sunmorl N 60S, rare earth oxide (rubidium oxide), Fischer-Tropsch wax and modification liquid are mixed according to the weight ratio of 100:23:13:7:10:2:50:19, then at 185 DEG C melting 50min, at 15 DEG C cooling, granulation with obtained 3D printer sight glass materials A 3;
Wherein, Mes is mesityl.
Comparative example 1
Carry out obtained 3D printer sight glass material B 1 according to the method for embodiment 1, unlike, step 1) in do not use Graphene.
Comparative example 2
Carry out obtained 3D printer sight glass material B 2 according to the method for embodiment 1, unlike, step 1) in do not use complex compound such as formula structure (I) Suo Shi.
Comparative example 3
Carry out obtained 3D printer sight glass material B 3 according to the method for embodiment 1, unlike, step 1) in do not use nanometer expanded vermiculite.
Test example 1
Detect the tensile strength of above-mentioned 3D printer sight glass material, transmittance and softening temperature, concrete outcome is in table 1.
Table 1
Tensile strength/MPa | Transmittance/% | Softening temperature/DEG C | |
A1 | 75 | 96 | 169 |
A2 | 74 | 97 | 172 |
A3 | 72 | 95 | 167 |
B1 | 57 | 94 | 161 |
B2 | 55 | 94 | 153 |
B3 | 53 | 93 | 155 |
Known by above-described embodiment, comparative example and test example, the 3D printer sight glass material of expanded vermiculite modification provided by the invention has excellent tensile strength, transmittance and softening temperature.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode, in order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible array mode.
In addition, also can carry out arbitrary combination between various different embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (10)
1. a preparation method for the 3D printer sight glass material of expanded vermiculite modification, is characterized in that, comprising:
1) in the presence of uv light, by nanometer expanded vermiculite, be dissolved in ultrasonic agitation in DMF such as formula the complex compound of structure (I) Suo Shi and Graphene and form modification liquid;
2) polymethyl methacrylate, octylisothiazolinone, dimethyl formamide, silicon oxide, Sunmorl N 60S, rare earth oxide, Fischer-Tropsch wax and described modification liquid are mixed, then melting, cooling, granulation are with obtained described 3D printer sight glass material;
Wherein, Mes is mesityl.
2. preparation method according to claim 1, wherein, in step 1) in, described ultraviolet wavelength is 150-200nm.
3. preparation method according to claim 1, wherein, in step 1) in, described ultrasonic agitation at least meets the following conditions: hyperacoustic frequency is 25-30KHz, and whipping temp is 55-65 DEG C, and churning time is 4-6h.
4. preparation method according to claim 1, wherein, in step 1) in, the particle diameter of described nanometer expanded vermiculite is 35-40nm.
5. according to the preparation method in claim 1-4 described in any one, wherein, in step 1) in, relative to the described nanometer expanded vermiculite of 100 weight parts, the consumption of the described complex compound such as formula structure (I) Suo Shi is 17-26 weight part, the consumption of described Graphene is 4-4.5 weight part, and the consumption of described DMF is 200-280 weight part.
6. preparation method according to claim 5, wherein, in step 2) in, relative to the described polymethyl methacrylate of 100 weight parts, the consumption of described octylisothiazolinone is 12-23 weight part, the consumption of described dimethyl formamide is 8-13 weight part, the consumption of described silicon oxide is 3-7 weight part, the consumption of described Sunmorl N 60S is 5.5-10 weight part, the consumption of described rare earth oxide is 1.2-2 weight part, the consumption of described Fischer-Tropsch wax is 40-50 weight part, and the consumption of described modification liquid is 14-19 weight part.
7. preparation method according to claim 6, wherein, described rare earth oxide be selected from cerous oxide, cerium dioxide, Praseodymium trioxide and rubidium oxide one or more.
8. preparation method according to claim 6, wherein, in step 2) in, described melting at least meets the following conditions: melt temperature is 175-185 DEG C, and the fusion time is 30-50min.
9. preparation method according to claim 6, wherein, in step 2) in, the temperature of described cooling is 5-15 DEG C.
10. a 3D printer sight glass material for expanded vermiculite modification, is characterized in that, described 3D printer sight glass material is prepared from by the method in claim 1-9 described in any one.
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CN1446850A (en) * | 2002-03-22 | 2003-10-08 | 中国人民解放军海军工程大学 | Compound nano organic glass of protecting against X ray |
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CN102408658A (en) * | 2011-10-21 | 2012-04-11 | 上海交通大学 | Graphene modified poly-methyl methacrylate composite and preparation method thereof |
CN103333449A (en) * | 2013-07-25 | 2013-10-02 | 中国科学院合肥物质科学研究院 | Polymethyl methacrylate-zinc hydroxide nanocomposite and preparation method thereof |
CN103382256A (en) * | 2013-07-01 | 2013-11-06 | 上海交通大学 | Preparation method of polymethyl methacrylate/nano silicon compound membrane |
CN104945815A (en) * | 2015-07-28 | 2015-09-30 | 张家港市德力特新材料有限公司 | Anti-aging organic glass |
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2015
- 2015-12-22 CN CN201510976009.0A patent/CN105482336A/en active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1446850A (en) * | 2002-03-22 | 2003-10-08 | 中国人民解放军海军工程大学 | Compound nano organic glass of protecting against X ray |
US20050143580A1 (en) * | 2003-12-04 | 2005-06-30 | Boehringer Ingelheim International Gmbh | Novel ruthenium catalyst |
CN101633740A (en) * | 2008-07-22 | 2010-01-27 | 上海杰事杰新材料股份有限公司 | Method for preparing transparent heat-resistant polymethyl methacrylate nano-composite membrane |
CN102408658A (en) * | 2011-10-21 | 2012-04-11 | 上海交通大学 | Graphene modified poly-methyl methacrylate composite and preparation method thereof |
CN103382256A (en) * | 2013-07-01 | 2013-11-06 | 上海交通大学 | Preparation method of polymethyl methacrylate/nano silicon compound membrane |
CN103333449A (en) * | 2013-07-25 | 2013-10-02 | 中国科学院合肥物质科学研究院 | Polymethyl methacrylate-zinc hydroxide nanocomposite and preparation method thereof |
CN104945815A (en) * | 2015-07-28 | 2015-09-30 | 张家港市德力特新材料有限公司 | Anti-aging organic glass |
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Application publication date: 20160413 |