CN116003941A - PMMA composite material and preparation method thereof - Google Patents
PMMA composite material and preparation method thereof Download PDFInfo
- Publication number
- CN116003941A CN116003941A CN202310068353.4A CN202310068353A CN116003941A CN 116003941 A CN116003941 A CN 116003941A CN 202310068353 A CN202310068353 A CN 202310068353A CN 116003941 A CN116003941 A CN 116003941A
- Authority
- CN
- China
- Prior art keywords
- modified
- hydroxyapatite
- pmma
- suspension
- montmorillonite
- 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.)
- Granted
Links
- 229920003229 poly(methyl methacrylate) Polymers 0.000 title claims abstract description 73
- 239000004926 polymethyl methacrylate Substances 0.000 title claims abstract description 73
- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims description 12
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical class [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims abstract description 60
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical class O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000000725 suspension Substances 0.000 claims description 56
- -1 titanate lipid Chemical class 0.000 claims description 36
- 239000007788 liquid Substances 0.000 claims description 32
- 239000000463 material Substances 0.000 claims description 27
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 24
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 18
- 239000006185 dispersion Substances 0.000 claims description 17
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 16
- 239000007822 coupling agent Substances 0.000 claims description 16
- 238000000227 grinding Methods 0.000 claims description 16
- 239000002244 precipitate Substances 0.000 claims description 16
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 16
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 12
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 9
- 239000004094 surface-active agent Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 8
- 238000000576 coating method Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 125000004185 ester group Chemical group 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 8
- 239000006228 supernatant Substances 0.000 claims description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 239000004519 grease Substances 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract description 4
- 239000003063 flame retardant Substances 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 3
- 230000004075 alteration Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229920000891 common polymer Polymers 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002892 organic cations Chemical class 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- HTPGOQRGCUSPGR-UHFFFAOYSA-N phosphoric acid silane Chemical compound [SiH4].OP(O)(O)=O HTPGOQRGCUSPGR-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Images
Landscapes
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention provides a PMMA composite material, which comprises the following components in percentage by mass: 70% -90% of PMMA; 5% -10% of modified hydroxyapatite; 5 to 15 percent of modified montmorillonite. The PMMA composite material has excellent mechanical property and flame retardant property.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a PMMA composite material and a preparation method thereof.
Background
Polymethyl methacrylate (PMMA) is a common polymer material, has special light transmittance, weather resistance, high strength and good comprehensive mechanical properties, and is widely applied to the fields of medical treatment, construction, aerospace and the like, but is not easy to melt and flow when being burnt at high temperature, and can be gasified directly on the surface to be burnt rapidly, thus belonging to inflammable polymers, and the application range is limited by poor heat resistance.
The polymethyl methacrylate is generally modified by adopting an organic or inorganic material so as to widen the application range. However, at present, the modification of polymethyl methacrylate only improves the mechanical property, but the flame retardant property of polymethyl methacrylate is studied.
Therefore, how to improve the mechanical properties of PMMA and the flame retardant properties of PMMA effectively is a technical problem that needs to be solved by those skilled in the art.
Disclosure of Invention
In order to solve the above problems, a first aspect of the present invention provides a PMMA composite comprising, in mass fraction, components of: 70% -90% of PMMA; 5% -10% of modified hydroxyapatite; 5 to 15 percent of modified montmorillonite.
In a first aspect, the modified hydroxyapatite is obtained by: adding hydroxyapatite into titanate grease coupling agent, adding into chloroform solution after reaction to obtain suspension, performing ultrasonic dispersion on the suspension for 1-2h, washing, drying and grinding to obtain modified hydroxyapatite.
In the first aspect, the mass ratio of the titanate lipid coupling agent to the hydroxyapatite is 1:5.
In a first aspect, the modified montmorillonite is a quaternary ammonium salt modified montmorillonite.
In a first aspect, the quaternary ammonium salt modified montmorillonite is obtained by: adding montmorillonite powder into deionized water, fully stirring to obtain a dispersion liquid with the concentration of 30-60g/L, adding an ester group-containing quaternary ammonium salt surfactant into the dispersion liquid, heating to 70-85 ℃, fully stirring, condensing and refluxing for 2-4 hours to obtain a uniform suspension liquid; and carrying out ultrasonic treatment on the suspension liquid to uniformly disperse the suspension liquid, then carrying out centrifugal separation to remove supernatant to obtain a precipitate, and washing, drying and grinding the precipitate to obtain the quaternary ammonium salt modified montmorillonite.
In a second aspect, the present application provides a method for preparing a PMMA composite, the method comprising the steps of: preparing modified hydroxyapatite; preparing modified montmorillonite; according to the material formula, the material comprises the following components in percentage by mass: 70-90% of PMMA, 5-10% of modified hydroxyapatite and 5-15% of modified montmorillonite; weighing the components; and (3) dissolving PMMA in toluene, sequentially adding modified hydroxyapatite and modified montmorillonite, magnetically stirring for 2 hours to obtain a suspension, performing ultrasonic dispersion on the suspension for 1 hour, and then coating, and drying in a vacuum drying oven at 50 ℃ to constant weight to obtain the PMMA composite material.
In a second aspect, the preparing a modified hydroxyapatite comprises: adding hydroxyapatite into titanate grease coupling agent, adding into chloroform solution after reaction to obtain suspension, performing ultrasonic dispersion on the suspension for 1-2h, washing, drying and grinding to obtain modified hydroxyapatite.
In a second aspect, the mass ratio of titanate lipid coupling agent to hydroxyapatite is 1:5.
In a second aspect, the modified montmorillonite is a quaternary ammonium salt modified montmorillonite.
In a second aspect, preparing the quaternary ammonium salt modified montmorillonite comprises: adding montmorillonite powder into deionized water, fully stirring to obtain a dispersion liquid with the concentration of 30-60g/L, adding an ester group-containing quaternary ammonium salt surfactant into the dispersion liquid, heating to 70-85 ℃, fully stirring, condensing and refluxing for 2-4 hours to obtain a uniform suspension liquid; and carrying out ultrasonic treatment on the suspension liquid to uniformly disperse the suspension liquid, then carrying out centrifugal separation to remove supernatant to obtain a precipitate, and washing, drying and grinding the precipitate to obtain the quaternary ammonium salt modified montmorillonite.
The beneficial effects are that: the invention provides a PMMA composite material, which comprises the following components in percentage by mass: 70% -90% of PMMA; 5% -10% of modified hydroxyapatite; 5 to 15 percent of modified montmorillonite. The modified hydroxyapatite and the modified montmorillonite selected by the invention have good compatibility with PMMA base materials; the modified hydroxyapatite can effectively improve the interface performance of the HA inorganic phase and the PMMA organic phase, and effectively improve the mechanical property of the PMMA composite material; the organic modified montmorillonite is a silicate material with a multi-layer structure, has good barrier effect, plays a certain role in heat insulation, and greatly improves the flame retardance of the PMMA composite material.
Drawings
In order to more clearly illustrate the embodiments of the present description or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a method for preparing PMMA composite material in an embodiment of the invention;
Detailed Description
The following description of the embodiments of the present invention will be made more apparent and fully hereinafter with reference to the accompanying drawings, in which some, but not all embodiments of the invention are shown. All other embodiments, which are derived by a person skilled in the art based on the embodiments of the invention, fall within the scope of protection of the invention.
Meanwhile, throughout the specification, unless otherwise specifically indicated, the terms used herein should be construed as meaning as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification will control.
Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or may be prepared by existing methods.
Example 1
The PMMA composite material is obtained by the following method:
(1) Preparing modified hydroxyapatite; preparing modified montmorillonite;
the preparation of the modified hydroxyapatite comprises the following steps: adding hydroxyapatite into a titanate lipid coupling agent, wherein the mass ratio of the titanate lipid coupling agent to the hydroxyapatite is 1:5, adding the mixture into a chloroform solution after reaction to obtain a suspension, performing ultrasonic dispersion on the suspension for 1-2h, and washing, drying and grinding to obtain modified hydroxyapatite; the modified montmorillonite is quaternary ammonium salt modified montmorillonite, and the preparation of the quaternary ammonium salt modified montmorillonite comprises the following steps: adding montmorillonite powder into deionized water, fully stirring to obtain a dispersion liquid with the concentration of 30-60g/L, adding an ester group-containing quaternary ammonium salt surfactant into the dispersion liquid, heating to 70-85 ℃, fully stirring, condensing and refluxing for 2-4 hours to obtain a uniform suspension liquid; carrying out ultrasonic treatment on the suspension to uniformly disperse the suspension, then centrifugally separating to remove supernatant to obtain a precipitate, and washing, drying and grinding the precipitate to obtain quaternary ammonium salt modified montmorillonite;
(2) According to the material formula, the material comprises the following components in percentage by mass: 85% of PMMA, 5% of modified hydroxyapatite and 10% of modified montmorillonite; accurately weighing the components;
(3) And (3) dissolving PMMA in toluene, sequentially adding modified hydroxyapatite and modified montmorillonite, magnetically stirring for 2 hours to obtain a suspension, performing ultrasonic dispersion on the suspension for 1 hour, and then coating, and drying in a vacuum drying oven at 50 ℃ to constant weight to obtain the PMMA composite material.
Example 2
The PMMA composite material is obtained by the following method:
(1) Preparing modified hydroxyapatite; preparing modified montmorillonite;
the preparation of the modified hydroxyapatite comprises the following steps: adding hydroxyapatite into a titanate lipid coupling agent, wherein the mass ratio of the titanate lipid coupling agent to the hydroxyapatite is 1:5, adding the mixture into a chloroform solution after reaction to obtain a suspension, performing ultrasonic dispersion on the suspension for 1-2h, and washing, drying and grinding to obtain modified hydroxyapatite; the modified montmorillonite is quaternary ammonium salt modified montmorillonite, and the preparation of the quaternary ammonium salt modified montmorillonite comprises the following steps: adding montmorillonite powder into deionized water, fully stirring to obtain a dispersion liquid with the concentration of 30-60g/L, adding an ester group-containing quaternary ammonium salt surfactant into the dispersion liquid, heating to 70-85 ℃, fully stirring, condensing and refluxing for 2-4 hours to obtain a uniform suspension liquid; carrying out ultrasonic treatment on the suspension to uniformly disperse the suspension, then centrifugally separating to remove supernatant to obtain a precipitate, and washing, drying and grinding the precipitate to obtain quaternary ammonium salt modified montmorillonite;
(2) According to the material formula, the material comprises the following components in percentage by mass: PMMA 85%, modified hydroxyapatite 7.5%, and modified montmorillonite 7.5%; accurately weighing the components;
(3) And (3) dissolving PMMA in toluene, sequentially adding modified hydroxyapatite and modified montmorillonite, magnetically stirring for 2 hours to obtain a suspension, performing ultrasonic dispersion on the suspension for 1 hour, and then coating, and drying in a vacuum drying oven at 50 ℃ to constant weight to obtain the PMMA composite material.
Example 3
The PMMA composite material is obtained by the following method:
(1) Preparing modified hydroxyapatite; preparing modified montmorillonite;
the preparation of the modified hydroxyapatite comprises the following steps: adding hydroxyapatite into a titanate lipid coupling agent, wherein the mass ratio of the titanate lipid coupling agent to the hydroxyapatite is 1:5, adding the mixture into a chloroform solution after reaction to obtain a suspension, performing ultrasonic dispersion on the suspension for 1-2h, and washing, drying and grinding to obtain modified hydroxyapatite; the modified montmorillonite is quaternary ammonium salt modified montmorillonite, and the preparation of the quaternary ammonium salt modified montmorillonite comprises the following steps: adding montmorillonite powder into deionized water, fully stirring to obtain a dispersion liquid with the concentration of 30-60g/L, adding an ester group-containing quaternary ammonium salt surfactant into the dispersion liquid, heating to 70-85 ℃, fully stirring, condensing and refluxing for 2-4 hours to obtain a uniform suspension liquid; carrying out ultrasonic treatment on the suspension to uniformly disperse the suspension, then centrifugally separating to remove supernatant to obtain a precipitate, and washing, drying and grinding the precipitate to obtain quaternary ammonium salt modified montmorillonite;
(2) According to the material formula, the material comprises the following components in percentage by mass: 85.5% of PMMA, 9.5% of modified hydroxyapatite and 5% of modified montmorillonite; accurately weighing the components;
(3) And (3) dissolving PMMA in toluene, sequentially adding modified hydroxyapatite and modified montmorillonite, magnetically stirring for 2 hours to obtain a suspension, performing ultrasonic dispersion on the suspension for 1 hour, and then coating, and drying in a vacuum drying oven at 50 ℃ to constant weight to obtain the PMMA composite material.
Comparative example 1
The PMMA material is obtained by the following method:
(1) According to the material formula, the material comprises the following components in percentage by mass: 100% of PMMA; accurately weighing PMMA;
(2) And (3) dissolving PMMA in toluene, magnetically stirring for 2 hours to obtain a suspension, performing ultrasonic dispersion on the suspension for 1 hour, and then coating, and drying in a vacuum drying oven at 50 ℃ to constant weight to obtain the PMMA material.
Comparative example 2
The PMMA material is obtained by the following method:
(1) Preparing modified hydroxyapatite;
the preparation of the modified hydroxyapatite comprises the following steps: adding hydroxyapatite into a titanate lipid coupling agent, wherein the mass ratio of the titanate lipid coupling agent to the hydroxyapatite is 1:5, adding the mixture into a chloroform solution after reaction to obtain a suspension, performing ultrasonic dispersion on the suspension for 1-2h, and washing, drying and grinding to obtain modified hydroxyapatite;
(2) According to the material formula, the material comprises the following components in percentage by mass: PMMA 85% and modified hydroxyapatite 15%%; accurately weighing the components;
(3) And (3) dissolving PMMA in toluene, adding modified hydroxyapatite, magnetically stirring for 2 hours to obtain a suspension, performing ultrasonic dispersion on the suspension for 1 hour, and then coating, and drying in a vacuum drying oven at 50 ℃ to constant weight to obtain the PMMA material.
Comparative example 3
The PMMA material is obtained by the following method:
(1) Preparing modified montmorillonite;
the modified montmorillonite is quaternary ammonium salt modified montmorillonite, and the preparation of the quaternary ammonium salt modified montmorillonite comprises the following steps: adding montmorillonite powder into deionized water, fully stirring to obtain a dispersion liquid with the concentration of 30-60g/L, adding an ester group-containing quaternary ammonium salt surfactant into the dispersion liquid, heating to 70-85 ℃, fully stirring, condensing and refluxing for 2-4 hours to obtain a uniform suspension liquid; carrying out ultrasonic treatment on the suspension to uniformly disperse the suspension, then centrifugally separating to remove supernatant to obtain a precipitate, and washing, drying and grinding the precipitate to obtain quaternary ammonium salt modified montmorillonite;
(2) According to the material formula, the material comprises the following components in percentage by mass: PMMA 85% and modified montmorillonite 15%; accurately weighing the components;
(3) And (3) dissolving PMMA in toluene, adding modified montmorillonite, magnetically stirring for 2 hours to obtain a suspension, performing ultrasonic dispersion on the suspension for 1 hour, and then coating, and drying in a vacuum drying oven at 50 ℃ to constant weight to obtain the PMMA material.
Effect examples
The materials prepared in examples 1 to 3 and comparative examples 1 to 3 were subjected to performance test, and the test results are shown in Table 1.
TABLE 1 Material Performance test results for examples 1-3 and comparative examples 1-3
As can be obtained from table 1, the PMMA composite materials developed by compounding PMMA, modified hydroxyapatite and modified montmorillonite in examples 1 to 3 of the present invention. The hydroxyapatite has small particle size and large specific surface area, has larger contact area with a PMMA matrix, and after being modified by the phosphate silane, the active functional group on the surface is increased, so that the interfacial bonding property of the hydroxyapatite and the PMMA matrix is obviously improved, the hydroxyapatite is well dispersed in the PMMA matrix, and can play a good role in stress dispersion and transmission, thereby achieving the purpose of enhancement and effectively improving the mechanical property of the PMMA composite material; organic cations in the quaternary ammonium salt surfactant are replaced by original hydrated cations among montmorillonite layers through ion exchange, so that the montmorillonite has better properties of lipophilicity, organic compatibility, thermal stability and the like, the interlayer spacing of the montmorillonite is effectively opened, the compatibility between the montmorillonite and organic matters is improved, the interlayer spacing of silicate is increased, and when the silicate is subjected to melt extrusion, high polymer chains in a molten state enter between the sheets more easily, and silicate sheets are covered on the surface of the material to play a role of heat insulation, so that the flame retardant property of the PMMA composite material is effectively improved.
Finally, it is also noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (10)
1. A PMMA composite, characterized in that the composition of the PMMA composite comprises, in mass fraction:
70% -90% of PMMA; 5% -10% of modified hydroxyapatite; 5 to 15 percent of modified montmorillonite.
2. PMMA composite according to claim 1, characterized in that the modified hydroxyapatite is obtained by: adding hydroxyapatite into titanate grease coupling agent, adding into chloroform solution after reaction to obtain suspension, performing ultrasonic dispersion on the suspension for 1-2h, washing, drying and grinding to obtain modified hydroxyapatite.
3. PMMA composite according to claim 2, characterized in that the mass ratio of titanate lipid coupling agent to hydroxyapatite is 1:5.
4. A PMMA composite according to claim 3 wherein the modified montmorillonite is a quaternary ammonium salt modified montmorillonite.
5. The PMMA composite of claim 4 wherein the quaternary ammonium salt modified montmorillonite is obtained by: adding montmorillonite powder into deionized water, fully stirring to obtain a dispersion liquid with the concentration of 30-60g/L, adding an ester group-containing quaternary ammonium salt surfactant into the dispersion liquid, heating to 70-85 ℃, fully stirring, condensing and refluxing for 2-4 hours to obtain a uniform suspension liquid; and carrying out ultrasonic treatment on the suspension liquid to uniformly disperse the suspension liquid, then carrying out centrifugal separation to remove supernatant to obtain a precipitate, and washing, drying and grinding the precipitate to obtain the quaternary ammonium salt modified montmorillonite.
6. The preparation method of the PMMA composite material is characterized by comprising the following steps of:
preparing modified hydroxyapatite; preparing modified montmorillonite;
according to the material formula, the material comprises the following components in percentage by mass: 70-90% of PMMA, 5-10% of modified hydroxyapatite and 5-15% of modified montmorillonite; weighing the components;
and (3) dissolving PMMA in toluene, sequentially adding modified hydroxyapatite and modified montmorillonite, magnetically stirring for 2 hours to obtain a suspension, performing ultrasonic dispersion on the suspension for 1 hour, and then coating, and drying in a vacuum drying oven at 50 ℃ to constant weight to obtain the PMMA composite material.
7. The method of preparing a PMMA composite of claim 6 wherein preparing modified hydroxyapatite comprises: adding hydroxyapatite into titanate grease coupling agent, adding into chloroform solution after reaction to obtain suspension, performing ultrasonic dispersion on the suspension for 1-2h, washing, drying and grinding to obtain modified hydroxyapatite.
8. The method for preparing the PMMA composite material according to claim 7, wherein the mass ratio of the titanate lipid coupling agent to the hydroxyapatite is 1:5.
9. The method for preparing PMMA composite material according to claim 8, wherein the modified montmorillonite is quaternary ammonium salt modified montmorillonite.
10. The method of preparing a PMMA composite of claim 9 wherein preparing the quaternary ammonium salt modified montmorillonite comprises: adding montmorillonite powder into deionized water, fully stirring to obtain a dispersion liquid with the concentration of 30-60g/L, adding an ester group-containing quaternary ammonium salt surfactant into the dispersion liquid, heating to 70-85 ℃, fully stirring, condensing and refluxing for 2-4 hours to obtain a uniform suspension liquid; and carrying out ultrasonic treatment on the suspension liquid to uniformly disperse the suspension liquid, then carrying out centrifugal separation to remove supernatant to obtain a precipitate, and washing, drying and grinding the precipitate to obtain the quaternary ammonium salt modified montmorillonite.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310068353.4A CN116003941B (en) | 2023-01-13 | 2023-01-13 | PMMA composite material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310068353.4A CN116003941B (en) | 2023-01-13 | 2023-01-13 | PMMA composite material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116003941A true CN116003941A (en) | 2023-04-25 |
| CN116003941B CN116003941B (en) | 2024-07-19 |
Family
ID=86035482
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310068353.4A Active CN116003941B (en) | 2023-01-13 | 2023-01-13 | PMMA composite material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116003941B (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101700416A (en) * | 2009-10-28 | 2010-05-05 | 山东轻工业学院 | Method for preparing hydroxyapatite composite |
| KR20120040327A (en) * | 2010-10-19 | 2012-04-27 | 류수착 | Hap / pmma composite and manufacture method |
| CN104530774A (en) * | 2014-12-17 | 2015-04-22 | 武汉工程大学 | Ester-containing quaternary ammonium salt modified montmorillonite and preparation method thereof |
| CN107585750A (en) * | 2017-08-30 | 2018-01-16 | 浙江美加华医疗技术有限公司 | A kind of hydroxyapatite material of surface modification and preparation method thereof |
| CN110693726A (en) * | 2019-11-07 | 2020-01-17 | 慧生医学科技(徐州)有限公司 | Dental caries repair material and preparation method thereof |
| CN111592730A (en) * | 2020-06-17 | 2020-08-28 | 湖北合聚高分子材料有限公司 | High-gloss heat-resistant scratch-resistant weather-resistant PMMA/ASA alloy resin material and preparation method thereof |
| US20210322296A1 (en) * | 2018-08-15 | 2021-10-21 | Dow Toray Co., Ltd. | Aqueous dispersion composition and use thereof |
-
2023
- 2023-01-13 CN CN202310068353.4A patent/CN116003941B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101700416A (en) * | 2009-10-28 | 2010-05-05 | 山东轻工业学院 | Method for preparing hydroxyapatite composite |
| KR20120040327A (en) * | 2010-10-19 | 2012-04-27 | 류수착 | Hap / pmma composite and manufacture method |
| CN104530774A (en) * | 2014-12-17 | 2015-04-22 | 武汉工程大学 | Ester-containing quaternary ammonium salt modified montmorillonite and preparation method thereof |
| CN107585750A (en) * | 2017-08-30 | 2018-01-16 | 浙江美加华医疗技术有限公司 | A kind of hydroxyapatite material of surface modification and preparation method thereof |
| US20210322296A1 (en) * | 2018-08-15 | 2021-10-21 | Dow Toray Co., Ltd. | Aqueous dispersion composition and use thereof |
| CN110693726A (en) * | 2019-11-07 | 2020-01-17 | 慧生医学科技(徐州)有限公司 | Dental caries repair material and preparation method thereof |
| CN111592730A (en) * | 2020-06-17 | 2020-08-28 | 湖北合聚高分子材料有限公司 | High-gloss heat-resistant scratch-resistant weather-resistant PMMA/ASA alloy resin material and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| SS KIM, 等: "Polymethyl methacrylate/montmorillonite nanocomposite beads through a suspension polymerization-derived process", 《JOURNAL OF APPLIED POLYMER SCIENCE》, vol. 97, no. 6, pages 2340 - 2349 * |
| 黎宴良，等: "ＰＭＭＡ／ＯＭＭＴ纳米复合材料炭层结构对阻燃性能的影响", 《现代塑料加工应用》, vol. 25, no. 6, pages 1 - 4 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116003941B (en) | 2024-07-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109778335B (en) | Modified polypropylene fiber and preparation method thereof | |
| CN110093680B (en) | Graphene/cage type polysilsesquioxane modified polyester fiber and preparation method thereof | |
| Dong et al. | Synergistic effect of DOPO immobilized silica nanoparticles in the intumescent flame retarded polypropylene composites | |
| CN113337230B (en) | High-thermal-conductivity semi-cured adhesive film for metal substrate and preparation method thereof | |
| CN110452389B (en) | Low-temperature-resistant low-permeability silicone resin coating composition and preparation method thereof | |
| Chen et al. | Epoxy hybrid composites cured with octaaminophenyl polyhedral oligomeric silsesquioxane | |
| CN116003941B (en) | PMMA composite material and preparation method thereof | |
| Yao et al. | Preparation of a novel flame retardant based on diatomite/polyethyleneimine modified MWCNT for applications in silicone rubber composites | |
| Zhu et al. | Study on the modified fiber with nacre layer structure based on bionic coating and molybdenum disulfide co‐construction incorporated asphalt | |
| CN116135931A (en) | Self-repairing graphene-polymer coating and preparation method thereof | |
| CN102382439B (en) | Modified polycarbonate and preparation method thereof | |
| CN113667309A (en) | Organic-inorganic hybrid crosslinked heat-conducting silica gel and preparation method thereof | |
| CN112251139A (en) | Fire-resistant flame-retardant liquid polyorganosiloxane composition | |
| CN112080041B (en) | Preparation method of POSS grafted tannin modified diatomite flame-retardant modified composite material | |
| CN111205579B (en) | High-efficiency high-temperature-resistant aluminum nitride/polymer composite material and preparation method thereof | |
| Zhang et al. | Synthesis of novel copolymer hybrid modifiers (MMA‐MAH‐MAPOSS and ST‐MAH‐MAPOSS) based on POSS nanoplatform and study on its thermal properties | |
| CN112940457A (en) | Flame-retardant epoxy electromagnetic shielding material and preparation method thereof | |
| CN116285330A (en) | Carbon fiber reinforced PA6T/10T flame retardant material and preparation method thereof | |
| CN114685937A (en) | Flame-retardant epoxy resin composite material and preparation method thereof | |
| CN106009166A (en) | Multi-silane modified heat-resisting optical cable material and preparation method thereof | |
| CN114773707B (en) | Beta-cyclodextrin microcapsule ammonium polyphosphate intumescent flame-retardant low-density polyethylene and preparation method thereof | |
| He et al. | High orientation structure in UHMWPE/BN composites continuously obtained by elongational flow field leading to superior thermal conductivity | |
| CN110591325B (en) | Special halogen-free flame-retardant synergistic functional master batch for modifying polycarbonate resin and preparation method thereof | |
| CN113354906B (en) | High-temperature-resistant composite wood-plastic material and preparation method and application thereof | |
| CN112080147B (en) | Preparation method of sulfydryl organic silicon nanospheres and sulfydryl-alkene polymer flame-retardant system 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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |