CN118459963A - Silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material and preparation method thereof - Google Patents
Silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material and preparation method thereof Download PDFInfo
- Publication number
- CN118459963A CN118459963A CN202410563592.1A CN202410563592A CN118459963A CN 118459963 A CN118459963 A CN 118459963A CN 202410563592 A CN202410563592 A CN 202410563592A CN 118459963 A CN118459963 A CN 118459963A
- Authority
- CN
- China
- Prior art keywords
- ionic liquid
- silicon
- graphene
- modified graphene
- phosphorus
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000002608 ionic liquid Substances 0.000 title claims abstract description 92
- 229920007019 PC/ABS Polymers 0.000 title claims abstract description 63
- HIVGXUNKSAJJDN-UHFFFAOYSA-N [Si].[P] Chemical compound [Si].[P] HIVGXUNKSAJJDN-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 239000002131 composite material Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 58
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 33
- 239000011347 resin Substances 0.000 claims abstract description 17
- 229920005989 resin Polymers 0.000 claims abstract description 17
- MCTWTZJPVLRJOU-UHFFFAOYSA-N 1-methyl-1H-imidazole Chemical compound CN1C=CN=C1 MCTWTZJPVLRJOU-UHFFFAOYSA-N 0.000 claims abstract description 10
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims abstract description 10
- OOCUOKHIVGWCTJ-UHFFFAOYSA-N chloromethyl(trimethyl)silane Chemical compound C[Si](C)(C)CCl OOCUOKHIVGWCTJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims abstract description 10
- 230000004048 modification Effects 0.000 claims abstract description 3
- 238000012986 modification Methods 0.000 claims abstract description 3
- 238000000498 ball milling Methods 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- -1 1-methyl-3-trimethylsilylmethyl imidazole chloride salt Chemical compound 0.000 claims description 14
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 12
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- YZPNFYQRPJKWFJ-UHFFFAOYSA-N 2-methyl-1h-imidazol-1-ium;chloride Chemical compound Cl.CC1=NC=CN1 YZPNFYQRPJKWFJ-UHFFFAOYSA-N 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims description 3
- XLSZMDLNRCVEIJ-UHFFFAOYSA-N methylimidazole Natural products CC1=CNC=N1 XLSZMDLNRCVEIJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- GSNUFIFRDBKVIE-UHFFFAOYSA-N DMF Natural products CC1=CC=C(C)O1 GSNUFIFRDBKVIE-UHFFFAOYSA-N 0.000 claims description 2
- 239000000155 melt Substances 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 239000007810 chemical reaction solvent Substances 0.000 claims 1
- OELUWWUHVLEKRT-UHFFFAOYSA-N trimethyl-(3-methyl-2h-imidazol-1-yl)silane Chemical compound CN1CN([Si](C)(C)C)C=C1 OELUWWUHVLEKRT-UHFFFAOYSA-N 0.000 claims 1
- 230000017525 heat dissipation Effects 0.000 abstract description 2
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 9
- 229920000642 polymer Polymers 0.000 description 9
- 230000003993 interaction Effects 0.000 description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- XECAHXYUAAWDEL-UHFFFAOYSA-N acrylonitrile butadiene styrene Chemical compound C=CC=C.C=CC#N.C=CC1=CC=CC=C1 XECAHXYUAAWDEL-UHFFFAOYSA-N 0.000 description 2
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 2
- 239000004676 acrylonitrile butadiene styrene Substances 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000005160 1H NMR spectroscopy Methods 0.000 description 1
- 238000005481 NMR spectroscopy Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000005418 spin wave Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material and a preparation method thereof, relating to the technical field of heat conduction/heat dissipation, wherein the silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material consists of silicon-phosphorus ionic liquid modified graphene and PC/ABS, the silicon-phosphorus ionic liquid modified graphene is prepared by modifying graphene by ionic liquid, and the ionic liquid is prepared by reacting chloromethyl trimethylsilane, 1-methylimidazole and sodium hypophosphite. The ionic liquid modification improves the dispersibility of graphene in PC/ABS resin, and effectively improves the heat conduction performance and mechanical property of PC/ABS composite material.
Description
Technical Field
The invention relates to the technical field of heat conduction/heat dissipation, in particular to a silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material and a preparation method thereof.
Background
PC/ABS is an engineering plastic with good toughness and processability, and consists of Polycarbonate (PC) and acrylonitrile-butadiene-styrene copolymer (ABS). PC/ABS has excellent comprehensive performance and is widely applied to the fields of automobiles, electronics, buildings, medical treatment and the like. However, the poor thermal conductivity of PC/ABS reduces their competitiveness in some areas where high thermal conductivity is required, limiting the range of PC/ABS applications. The thermal conductivity of the polymer matrix can be enhanced by adding fillers having high thermal conductivity, such as metals, carbon-based materials, and ceramics. It is well known that graphene is one of the most effective additives, and is widely used to improve the overall properties of polymer composites, such as mechanical properties, electrical properties and thermal properties, due to its excellent physical properties. Graphene is widely applied to the field of heat-conducting composite materials due to the high heat-conducting property (the heat conductivity coefficient 5300 W.m -1·k-1) of the graphene, and the graphene polymer composite material is considered as a heat-dissipating material with extremely development prospect.
However, as with polymer composites containing other fillers, the thermal resistance of the graphene-polymer matrix interface greatly impedes heat conduction. Therefore, functionalization thereof improves dispersibility in the polymer, and thereby moderately improves the heat conduction ability of the polymer composite. Ionic Liquids (ILs) are a class of room temperature liquid organic salts with high thermal stability, consisting of ion pairs, which can exist under a wide range of chemical and physical conditions. ILs are widely used in a variety of fields due to their own characteristics. In recent years ILs have been used to modify carbon-based nanomaterials to improve their dispersibility in polymer matrices, thereby further improving the mechanical, electrical and thermal properties of the polymer composites.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material and a preparation method thereof.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
The silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material consists of silicon-phosphorus ionic liquid modified graphene and PC/ABS, wherein the silicon-phosphorus ionic liquid modified graphene is prepared by modifying graphene by ionic liquid, and the ionic liquid is prepared by reacting chloromethyl trimethylsilane, 1-methylimidazole and sodium hypophosphite.
The preparation method of the silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material comprises the following three steps:
The first step: chloromethyl trimethylsilane reacts with 1-methylimidazole to obtain 1-methyl-3-trimethylsilylmethyl imidazole chloride salt, and the 1-methyl-3-trimethylsilylmethyl imidazole chloride salt reacts with sodium hypophosphite in a solvent to generate 1-methyl-3-trimethylsilylmethyl imidazole hypophosphite ionic liquid;
And a second step of: carrying out modification treatment on graphene by adopting the ionic liquid prepared in the first step to obtain silicon-phosphorus ionic liquid modified graphene;
And a third step of: and carrying out melt blending on the silicon-phosphorus ionic liquid modified graphene and PC/ABS resin to obtain the silicon-phosphorus ionic liquid modified graphene-PC/ABS heat conduction composite material.
The process flow of the 1-methyl-3-trimethylsilylmethyl imidazole hypophosphite ionic liquid prepared according to the method is as follows:
In the first step, chloromethyl trimethylsilane and 1-methylimidazole are subjected to reflux reaction at 100-120 ℃ for 24-36 hours to obtain 1-methyl-3-trimethylsilylmethyl imidazole chloride; dissolving 1-methyl-3-trimethylsilicon methylimidazole chloride and sodium hypophosphite in distilled water, carrying out reflux reaction at 80-100 ℃ for 24-36h, and carrying out reduced pressure distillation to remove distilled water; soaking the product in a solvent for 24-48h, removing solids by suction filtration, and removing the solvent by reduced pressure distillation to obtain 1-methyl-3-trimethylsilomethyl imidazole hypophosphite;
preferably, the molar ratio of chloromethyl trimethylsilane to 1-methylimidazole is 1:1-1:2;
Preferably, the molar ratio of the 1-methyl-3-trimethylsilylmethyl imidazole chloride salt to the sodium hypophosphite is 1:1-1:2; the solvent is one of dichloromethane, ethanol, methanol and acetone.
According to the preparation method of the silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material, in the second step, a solvent is added into the ionic liquid prepared in the first step, so that a mixed liquid is obtained; adding graphene into a ball milling tank containing grinding balls, adding the mixed solution into the ball milling tank for ball milling, and then washing, suction filtering and drying to obtain a product;
preferably, the ball milling rotating speed is 100-200rpm/min; ball milling time is 6-10h;
Preferably, the dosage ratio of the graphene to the mixed solution is as follows: (10-20) g (200-250) ml. The solvent is a mixture of water and one of methanol, ethanol, DMF and THF, and the mass concentration of the organic solvent in the mixture is 2%;
preferably, the graphene is one of reduced graphene oxide, expanded graphite and electrochemical exfoliated graphene;
preferably, the mass ratio of the ionic liquid to the graphene is 0.01:1-0.05:1.
In the third step, the silicon-phosphorus ionic liquid modified graphene and PC/ABS resin are subjected to melt blending to obtain the silicon-phosphorus ionic liquid modified graphene-PC/ABS heat conduction composite material;
Preferably, the melt blending temperature is 200-240 ℃;
preferably, the mass ratio of the ionic liquid modified graphene to the PC/ABS resin is 5:100-15:100. The PC/ABS resin is one of AC3100, AC3108, AC2300, AC2500 and PC-550K.
The silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material prepared by the method has the following interaction mechanism of silicon-phosphorus ionic liquid, graphene and PC/ABS:
The silicon phosphorus ionic liquid modified graphene-PC/ABS composite material is characterized in that imidazole in 1-methyl-3-trimethylsilicon methylimidazole hypophosphite ionic liquid can generate cation-pi interaction with graphene so as to be modified by ionic liquid; the imidazole of the ionic liquid belongs to a conjugated structure and can form pi-pi interaction with benzene rings in PC/ABS, so that the interface interaction between graphene and PC/ABS matrix resin is improved, the dispersibility of the ionic liquid is improved, and the heat conduction performance and the mechanical property of the PC/ABS composite material are improved (figure 1).
The invention has the advantages and effects that:
1. the invention provides a novel preparation method of a silicon-phosphorus ionic liquid, which has wide application range.
2. The ionic liquid and PC/ABS have pi-pi interaction, and the ionic liquid is used for modifying the graphene, so that the dispersibility of the graphene in PC/ABS resin can be improved, and the problem of agglomeration in PC/ABS resin is solved.
3. The silicon-phosphorus ionic liquid modified graphene-PC/ABS heat conduction composite material prepared by the invention has excellent heat conduction and mechanical properties.
Drawings
FIG. 1 silicon phosphorus ionic liquid, graphene and PC/ABS interaction mechanism;
FIG. 2 1-methyl-3-trimethylsilylmethylimidazole hypophosphite ionic liquid structural characterization, (a) IR spectrum, (b) 1HNMR,(c)13 C NMR, (d) Mass Spectrometry.
Detailed Description
The present invention will be described in detail with reference to examples.
Example 1
A preparation method of a silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material comprises the following specific operation steps:
The first step: 0.1mol of 1-methylimidazole and 0.1mol of chloromethyl trimethylsilane were introduced into a 250ml three-necked flask equipped with a reflux condenser, thermometer and magnon under the protection of nitrogen atmosphere, and reacted at 100℃for 24 hours under reflux. After the reaction is finished, ethyl acetate and petroleum ether are used for alternately washing, unreacted raw materials are removed, petroleum ether is distilled off under reduced pressure, and 1-methyl-3-trimethylsilicon methylimidazole chloride is obtained. Dissolving 0.1mol of 1-methyl-3-trimethylsilicon methylimidazole chloride and 0.1mol of sodium hypophosphite in 100ml of distilled water, reacting for 24 hours at 80 ℃, distilling off distilled water, soaking the product in methylene dichloride for 48 hours, removing solids by suction filtration, and distilling off the solvent under reduced pressure to obtain the 1-methyl-3-trimethylsilicon methylimidazole hypophosphite. The structural characterization of the 1-methyl-3-trimethylsilylmethyl imidazole hypophosphite ionic liquid in figure 2 shows that the ionic liquid is successfully prepared.
And a second step of: 20g of electrochemical stripping graphene is added into a ball milling tank, 0.4g of the ionic liquid prepared in the first step is dispersed in 200ml of ethanol water solution with the mass concentration of 2%, then the ionic liquid is added into the ball milling tank, 300g of grinding balls are added into the ball milling tank, after the addition is completed, the ball milling tank is arranged on a planetary ball mill, and ball milling is carried out for 6 hours at 120 rpm. And then washing with water, suction filtering, and putting the product into an oven at 80 ℃ for drying to obtain black powder which is the silicon-phosphorus ionic liquid functionalized graphene (Si-G).
And a third step of: 12.6G of silicon-phosphorus ionic liquid modified graphene (Si-G) and 167.4G of PC/ABS resin (PC-550K) are melted and mixed at 220 ℃ to obtain the silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material.
Example 2
The first step: as in example 1.
And a second step of: as in example 1.
And a third step of: 16.2G of silicon-phosphorus ionic liquid modified graphene (Si-G) and 163.8G of PC/ABS resin (PC-550K) are melted and mixed at 220 ℃ to obtain the silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material.
Example 3
The first step: as in example 1.
And a second step of: as in example 1.
And a third step of: 19.8G of silicon-phosphorus ionic liquid modified graphene (Si-G) and 160.2G of PC/ABS resin (PC-550K) are melted and mixed at 220 ℃ to obtain the silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material.
Example 4
The first step: as in example 1.
And a second step of: 20g of expanded graphite was charged into a ball-milling pot, 0.4g of the ionic liquid prepared in example 1 was dispersed in 200ml of an aqueous ethanol solution having a mass concentration of 2%, then charged into the ball-milling pot, 300g of grinding balls were charged into the ball-milling pot, and after the charging was completed, the ball-milling pot was mounted on a planetary ball mill and ball-milled at 120rpm for 6 hours. And then washing with water, suction filtering, and putting the product into an oven at 80 ℃ for drying to obtain black powder which is the silicon-phosphorus ionic liquid functionalized graphene (Si-TSG).
And a third step of: 12.6g of silicon-phosphorus ionic liquid modified graphene (Si-TSG) and 167.4g of PC/ABS resin (PC-550K) are melted and mixed at 220 ℃ to obtain the silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material.
Example 5
The first step: as in example 1.
And a second step of: same as in example 4.
And a third step of: 16.2g of silicon-phosphorus ionic liquid modified graphene (Si-TSG) and 163.8g of PC/ABS resin (PC-550K) are melted and mixed at 220 ℃ to obtain the silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material.
Example 6
The first step: as in example 1.
And a second step of: same as in example 4.
And a third step of: 19.8g of silicon-phosphorus ionic liquid modified graphene (Si-TSG) and 160.2g of PC/ABS resin (PC-550K) are melted and mixed at 220 ℃ to obtain the silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material.
The samples of examples 1-6 were tested for performance, wherein tensile strength was tested according to GB 1040-79, flexural modulus was tested according to GB/T9341-2008, impact strength was tested according to GB/T1843-2008, thermal conductivity was tested according to GB/T32064-2015, and the test results are shown in Table 1:
TABLE 1 Performance test of silicon phosphorus ionic liquid modified graphene-PC/ABS composite material
The preparation method has the main raw materials of electrochemical stripping graphene and expanded graphite, and is low in cost; the compatibility with PC/ABS composite materials can be improved after the ionic liquid is modified.
According to the invention, the ball milling process is adopted to modify the graphene, so that mass industrialized production can be realized.
The silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material disclosed by the invention has excellent heat conduction performance, improved mechanical properties and can be applied to an automobile radiator.
Claims (8)
1. The silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material is characterized by comprising silicon-phosphorus ionic liquid modified graphene and PC/ABS, wherein the silicon-phosphorus ionic liquid modified graphene is prepared by modifying graphene by ionic liquid, and the ionic liquid is prepared by reacting chloromethyl trimethylsilane, 1-methylimidazole and sodium hypophosphite.
2. The preparation method of the silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material is characterized by comprising the following steps of:
The first step: chloromethyl trimethylsilane reacts with 1-methylimidazole to obtain 1-methyl-3-trimethylsilylmethyl imidazole chloride salt, and the 1-methyl-3-trimethylsilylmethyl imidazole chloride salt reacts with sodium hypophosphite in a solvent to generate 1-methyl-3-trimethylsilylmethyl imidazole hypophosphite ionic liquid;
And a second step of: carrying out modification treatment on graphene by adopting the ionic liquid prepared in the first step to obtain silicon-phosphorus ionic liquid modified graphene;
And a third step of: carrying out melt blending on the silicon-phosphorus ionic liquid modified graphene and PC/ABS resin to obtain a silicon-phosphorus ionic liquid modified graphene-PC/ABS heat conduction composite material;
The synthetic route of the 1-methyl-3-trimethylsilylmethyl imidazole phosphite ionic liquid is as follows:
3. the preparation method of the silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material according to claim 2, which is characterized in that in the first step, chloromethyl trimethylsilane and 1-methylimidazole are subjected to reflux reaction at 100-120 ℃ to obtain 1-methyl-3-trimethylsilicon methylimidazole chloride; dissolving 1-methyl-3-trimethylsilicon methylimidazole chloride and sodium hypophosphite in distilled water, carrying out reflux reaction at 80-100 ℃, and carrying out reduced pressure distillation to remove distilled water; the product is soaked in a solvent, the solid is removed by suction filtration, the solvent is removed by reduced pressure distillation, and the 1-methyl-3-trimethylsilicon methylimidazole hypophosphite is obtained.
4. The method for preparing the silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material according to claim 2, wherein in the first step, the molar ratio of chloromethyl trimethylsilane to 1-methylimidazole is 1:1-1:2; the molar ratio of the 1-methyl-3-trimethylsilyl imidazole chloride salt to the sodium hypophosphite is 1:1-1:2; the reaction solvent adopts one of dichloromethane, ethanol, methanol and acetone.
5. The preparation method of the silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material according to claim 2, wherein in the second step, a solvent is added into the ionic liquid prepared in the first step to obtain a mixed solution; and adding graphene into a ball milling tank containing grinding balls, adding the mixed solution into the ball milling tank for ball milling, and then washing, suction filtering and drying to obtain a product.
6. The preparation method of the silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material, which is disclosed in claim 5, is characterized in that the ball milling rotation speed is 100-200rpm/min; ball milling time is 6-10h; the dosage ratio of the graphene to the mixed solution is as follows: (10-20) g (200-250) ml; the solvent is a mixture of water and one of methanol, ethanol, DMF and THF, and the mass concentration of the organic solvent in the mixture is 2%; the graphene is one of reduced graphene oxide, expanded graphite and electrochemical exfoliated graphene; the mass ratio of the ionic liquid to the graphene is 0.01:1-0.05:1.
7. The preparation method of the silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material according to claim 2, wherein in the third step, silicon-phosphorus ionic liquid modified graphene and PC/ABS resin are subjected to melt blending to obtain the silicon-phosphorus ionic liquid modified graphene-PC/ABS heat conduction composite material; the melt blending temperature is 200-240 ℃; the mass ratio of the silicon-phosphorus ionic liquid modified graphene to the PC/ABS resin is 5:100-15:100.
8. A 1-methyl-3-trimethylsilylimidazole hypophosphite ionic liquid, which is characterized by being prepared by the preparation method according to any one of claims 2-7, and having the structural formula:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410563592.1A CN118459963A (en) | 2024-05-08 | 2024-05-08 | Silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410563592.1A CN118459963A (en) | 2024-05-08 | 2024-05-08 | Silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN118459963A true CN118459963A (en) | 2024-08-09 |
Family
ID=92151075
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202410563592.1A Pending CN118459963A (en) | 2024-05-08 | 2024-05-08 | Silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN118459963A (en) |
-
2024
- 2024-05-08 CN CN202410563592.1A patent/CN118459963A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| WO2021023226A1 (en) | Nitrogen-rich group functionalized graphene, preparation method, and application | |
| CN109467574B (en) | Reactive flame retardant based on vanillin as well as preparation and application thereof | |
| CN110283284B (en) | High-thermal-conductivity modified epoxy resin and preparation method thereof | |
| CN109135189B (en) | P/N/Si-containing multi-element polyphosphazene silazane flame retardant for epoxy resin and preparation method thereof | |
| CN116285318B (en) | Light heat conduction engineering plastic and preparation method thereof | |
| CN107129493B (en) | Diamine type dibenzoxazine containing alicyclic hydrocarbon imide group and preparation method thereof | |
| CN115010993A (en) | Preparation method and application of graphene oxide hybrid flame retardant | |
| CN111253437A (en) | P/N/Si-containing multi-element reactive epoxy resin flame retardant and preparation method thereof | |
| CN112940257A (en) | Eugenol epoxy group double-splint type cage-like silsesquioxane as well as preparation method and application thereof | |
| CN113462024A (en) | Polydopamine and metal ion modified montmorillonite flame retardant and preparation method thereof | |
| CN101659677B (en) | Triphosphazene epoxy resin and preparation method thereof | |
| Selvaraj et al. | Development of high-performance hybrid sustainable bio-composites from biobased carbon reinforcement and cardanol-benzoxazine matrix | |
| CN101891936B (en) | Preparation method of composite material based on epoxy resin and phosphazene nanotubes | |
| WO2022156832A2 (en) | Preparation method for high-insulativity low-temperature electronic packaging material | |
| CN111253739A (en) | DOPO derivative/carbon nanotube synergistic flame-retardant glass fiber nylon composite material | |
| CN112876685B (en) | Tetraepoxy group liquid cage type silsesquioxane as well as preparation method and application thereof | |
| CN112194822B (en) | Phosphorus-containing flame retardant, preparation method and modified epoxy resin | |
| CN117050523B (en) | Wear-resistant polyphenylene sulfide material and preparation method thereof | |
| CN118459963A (en) | Silicon-phosphorus ionic liquid modified graphene-PC/ABS composite material and preparation method thereof | |
| CN116355133B (en) | Modified silicon dioxide-bismaleimide composite material and synthesis process thereof | |
| CN115716936B (en) | Phosphaphenanthrene siloxane bio-based flame-retardant branched macromolecule and preparation method and application thereof | |
| CN113651846B (en) | Method for modifying rubber by cardanol derivative | |
| CN113929717A (en) | 2-aminopyrimidine-based compound, flame-retardant epoxy resin material, and preparation method and application thereof | |
| KR102515280B1 (en) | Polyphenylene sulfide composite material and manufacturing method thereof | |
| CN118421052B (en) | High-insulation flame-retardant epoxy resin composition and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |