CN103877933A - Composite material and preparation method thereof - Google Patents
Composite material and preparation method thereof Download PDFInfo
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- CN103877933A CN103877933A CN201410111059.8A CN201410111059A CN103877933A CN 103877933 A CN103877933 A CN 103877933A CN 201410111059 A CN201410111059 A CN 201410111059A CN 103877933 A CN103877933 A CN 103877933A
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Abstract
The invention discloses a composite material and a preparation method thereof. The composite material is a composite material with a grading structure, which integrates different pore diameters of a composite zeolite molecular sieve, foam carbon and cordierite, so as to expand an adsorption range of the composite material and realize the strong adsorption and purification function. The preparation method disclosed by the invention comprises the following steps: dissolving a carbon precursor of the foam carbon into an organic solvent and sufficiently mixing with the composite zeolite molecular sieve to prepare a suspension solution; curing the suspension solution into a foam condensate; grinding and loading the generated foam condensate into pores of a cordierite honeycomb material; carbonizing and generating the foam carbon with the uniform pore diameters by using the uniform pores of the cordierite honeycomb material so as to combine the foam carbon with the cordierite honeycomb material; combining the zeolite molecular sieve with the generated foam carbon. The zeolite molecular sieve does not react in a preparation process and keeps the previous performance so as to prepare the composite material with the grading structure.
Description
Technical field
The present invention relates to field of compound material, relate in particular to zeolite/Carbon foam/cordierite composite of a kind of hierarchy and preparation method thereof.
Background technology
Zeolite molecular sieve, Carbon foam, cellular material are all more adsorption cleaning and catalyst material of application at present.The network structure of zeolite molecular sieve crystal inside has been given the function such as adsorbing separation, ion-exchange of zeolite molecular sieve uniqueness, aspect catalysis, gas separation, is being widely used.Powder-type zeolite molecular sieve is easy to dispersed placement, but can cause dust pollution in application, general by adding binding agent mixing formation section bar or flaky material, but adding of binding agent may change the pore structure of zeolite molecular sieve and lack micropore, reduce the active of zeolite molecular sieve and effect, need to have the material that can support zeolite molecular sieve and do not affect again its performance to carry out combination with it simultaneously.Carbon foam is the cellular carbonaceous functional material with more macroporous three-dimensional order, there is intensity high, thermal coefficient of expansion is low, the excellent specific properties such as anti-ablation, and there is good formability and processability, therefore be also widely used in purification, the every field such as catalytic treatment and electronics, and adopt in the generative process of organic material as carbonaceous presoma, carbonaceous presoma dissolves in organic solvent, the possibility of evenly adhering to other materials in Carbon foam is provided, and in the process with organic material production Carbon foam, temperature, pressure scope is not sufficient to make zeolite molecular sieve recurring structure, performance change, can be used as the Substrates of zeolite molecular sieve, and can form with zeolite molecular sieve the composite of hierarchy, but usually there is the unmanageable problem of aperture homogeneity in generating in Carbon foam, the inhomogeneous skewness that must cause zeolite molecular sieve in Carbon foam aperture, affect the performance of composite.Cordierite honeycomb material is the uniform porous material in a kind of aperture, be usually used in purifying vehicle exhaust, and high strength, high temperature resistant, corrosion-resistant, wear-resisting, be good Substrates, also can be used as confinement template prepared by Carbon foam, be conducive to the generation of Carbon foam uniform pore size.In addition, zeolite molecular sieve, Carbon foam, cordierite honeycomb material have the aperture of different sizes, can adsorb, purify emission molecule or the ion of different sizes, and impact is very little each other, has the potential quality that constitutes grading structure material.
Summary of the invention
The present invention has developed a kind of composite and preparation method thereof, described composite is zeolite/Carbon foam/cordierite composite, wherein, described zeolite is zeolite molecular sieve, described cordierite is cordierite honeycomb material, the different pore size of the comprehensive zeolite molecular sieve of the present invention, Carbon foam and cordierite forms the uniform composite of a kind of hierarchy and aperture, expand the adsorption range of composite, realize stronger adsorption function, and comprehensive Carbon foam and the high-intensity mechanical property of cordierite, be conducive to make more applicable purifying vehicle exhaust material.
Technical scheme provided by the invention is:
A preparation method for composite, concrete steps comprise:
Step 1, powder-type zeolite molecular sieve, novolac resin and hexamethylenetetramine are mixed taking mass ratio as the ratio of 1: 50: 5, add organic solvent and described novolac resin and hexamethylenetetramine are fully dissolved, the mass ratio of described organic solvent and described novolac resin is 12: 1;
Step 2, fully stirs the mixed solution of step 1 gained, obtains the homodisperse suspension of powder-type zeolite molecular sieve, and described mixing time is 5h;
Step 3, the described suspension of step 2 gained is put into high temperature and high pressure kettle, passing into high pure nitrogen to still internal pressure is 1.2～2Mpa, is heated to 200～210 DEG C, and keeps 0.8～1.5h with the programming rate of 0.25 DEG C/point, then keep temperature-resistant, unload and be depressed into normal pressure, release speed is 0.3～0.5Mpa/h, after release, is heated to 260～280 DEG C with the programming rate of 0.25 DEG C/point, and keep 1h, obtain foam curing thing;
Step 4, packs in the hole of cordierite honeycomb material after the described foam curing thing of step 3 gained is ground, and puts into high temperature and high pressure kettle, pass into high pure nitrogen to 10～16Mpa, be heated to 520～550 DEG C with the programming rate of 3～7 DEG C/point, and keep 2～4h, obtain nascent material;
Step 5, puts into retort by the described nascent material of step 4 gained and carries out charing, passes into high pure nitrogen as protection gas, is warming up to 800～900 DEG C, and keeps 30～45min with the programming rate of 1～3 DEG C/min.
Preferably, in described preparation method, described powder-type zeolite molecular sieve is T-shaped zeolite molecular sieve.
Preferably, in described preparation method, described organic solvent is ethanol, methyl alcohol or acetone.
Preferably, in described preparation method, described cordierite honeycomb material aperture is 2～3mm, and porosity is 40～80 hole/cm
2.
A kind of composite prepared according to above-mentioned preparation method also belongs to the scope that the present invention protects, the micropore size average out to 0.3～0.5nm of described composite, Carbon foam macropore diameter average out to 200～300 μ m.
Composite of the present invention, the different pore size of comprehensive zeolite molecular sieve, Carbon foam and cordierite forms the uniform composite of a kind of hierarchy and aperture, expand the adsorption range of composite, realize stronger adsorption function, and comprehensive Carbon foam and the high-intensity mechanical property of cordierite, be conducive to make more applicable purifying vehicle exhaust material.Preparation method provided by the present invention, the carbonaceous presoma of Carbon foam is dissolved in organic solvent and with zeolite molecular sieve and is fully mixed into suspension, first be cured as foam curing thing, make the presoma evenly combination in advance of zeolite molecular sieve and Carbon foam, again the foam curing thing of generation is ground and packed in the hole of cordierite honeycomb material, and through charing, utilize the even hole of cordierite honeycomb material, when generating the Carbon foam of uniform pore size, Carbon foam is combined with cordierite honeycomb material, and make the zeolite molecular sieve that disperses and the Carbon foam of generation further combined with, and zeolite molecular sieve does not react in preparation process, keep original performance, thereby prepare the composite with hierarchy.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, to make those skilled in the art can implement according to this with reference to description word.
The invention provides a kind of composite and preparation method thereof, the micropore size average out to 0.3～0.5nm of described composite, Carbon foam macropore diameter average out to 200～300 μ m.The preparation method of described zeolite/Carbon foam/cordierite composite, concrete steps comprise:
(1) powder-type zeolite molecular sieve, novolac resin and hexamethylenetetramine are mixed taking mass ratio as the ratio of 1: 50: 5, add organic solvent and described novolac resin and hexamethylenetetramine are fully dissolved, the mass ratio of described organic solvent and described novolac resin is 12: 1, described powder-type zeolite molecular sieve is preferably T-shaped zeolite molecular sieve, and described organic solvent is preferably ethanol, methyl alcohol or acetone;
(2) mixed solution of step (1) gained is fully stirred, obtain the homodisperse suspension of powder-type zeolite molecular sieve, described mixing time is 5h;
(3) the described suspension of step (2) gained is put into high temperature and high pressure kettle, passing into high pure nitrogen to still internal pressure is 1.2～2Mpa, be heated to 200～210 DEG C with the programming rate of 0.25 DEG C/point, and keep 0.8～1.5h, and then keep temperature-resistant, unload and be depressed into normal pressure, release speed is 0.3～0.5Mpa/h, after release, be heated to 260～280 DEG C with the programming rate of 0.25 DEG C/point, and keep 1h, obtain foam curing thing;
(4) will after the described foam curing thing grinding of step (3) gained, pack in the hole of cordierite honeycomb material, and put into high temperature and high pressure kettle, pass into high pure nitrogen to 10～16Mpa, be heated to 520～550 DEG C with the programming rate of 3～7 DEG C/point, and keep 2～4h, obtain nascent material, it is that 2～3mm and porosity are 40～80 hole/cm that described cordierite honeycomb material is preferably aperture
2;
(5) the described nascent material of step (4) gained is put into retort and carry out charing; pass into high pure nitrogen as protection gas; be warming up to 800～900 DEG C with the programming rate of 1～3 DEG C/min, and keep 30～45min, obtain described composite.
Embodiment mono-
(1) T-shaped powdery zeolite molecular sieve, novolac resin and hexamethylenetetramine are mixed taking mass ratio as the ratio of 1: 50: 5, add ethanol and described novolac resin and hexamethylenetetramine are fully dissolved, the mass ratio of described organic solvent and described novolac resin is 12: 1;
(2) mixed solution of step (1) gained is fully stirred, obtain the homodisperse suspension of zeolite molecular sieve, described mixing time is 5h;
(3) the described suspension of step (2) gained is put into high temperature and high pressure kettle, passing into high pure nitrogen to still internal pressure is 1.2Mpa, be heated to 200 DEG C with the programming rate of 0.25 DEG C/point, and keep 0.8h, and then keep temperature-resistant, unload and be depressed into normal pressure, release speed is 0.3Mpa/h, after release, be heated to 260 DEG C with the programming rate of 0.25 DEG C/point, and keep 1h, obtain foam curing thing;
(4) will after the described foam curing thing grinding of step (3) gained, pack in the hole of cordierite honeycomb material, and put into high temperature and high pressure kettle, pass into high pure nitrogen to 10Mpa, be heated to 520 DEG C with the programming rate of 3～7 DEG C/point, and keep 2h, obtain nascent material, it is that 2mm and porosity are 40 hole/cm that described cordierite honeycomb material is preferably aperture
2;
(5) the described nascent material of step (4) gained is put into retort and carry out charing, pass into high pure nitrogen as protection gas, be warming up to 800 DEG C with the programming rate of 1 DEG C/min, and keep 30min, obtain described composite.
The micropore size of the described composite obtaining is 0.3～0.5nm, Carbon foam macropore diameter average out to 300 μ m.
Embodiment bis-
(1) T-shaped powdery zeolite molecular sieve, novolac resin and hexamethylenetetramine are mixed taking mass ratio as the ratio of 1: 50: 5, add methyl alcohol and described novolac resin and hexamethylenetetramine are fully dissolved, the mass ratio of described organic solvent and described novolac resin is 12: 1;
(2) mixed solution of step (1) gained is fully stirred, obtain the homodisperse suspension of zeolite molecular sieve, described mixing time is 5h;
(3) the described suspension of step (2) gained is put into high temperature and high pressure kettle, passing into high pure nitrogen to still internal pressure is 2Mpa, be heated to 210 DEG C with the programming rate of 0.25 DEG C/point, and keep 1.5h, and then keep temperature-resistant, unload and be depressed into normal pressure, release speed is 0.5Mpa/h, after release, be heated to 280 DEG C with the programming rate of 0.25 DEG C/point, and keep 1h, obtain foam curing thing;
(4) will after the described foam curing thing grinding of step (3) gained, pack in the hole of cordierite honeycomb material, and put into high temperature and high pressure kettle, pass into high pure nitrogen to 16Mpa, be heated to 550 DEG C with the programming rate of 7 DEG C/point, and keep 4h, obtain nascent material, it is that 3mm and porosity are 80 hole/cm that described cordierite honeycomb material is preferably aperture
2;
(5) the described nascent material of step (4) gained is put into retort and carry out charing, pass into high pure nitrogen as protection gas, be warming up to 900 DEG C with the programming rate of 3 DEG C/min, and keep 45min, obtain described composite.
The micropore size of the described composite obtaining is 0.3～0.5nm, Carbon foam macropore diameter average out to 210 μ m.
Embodiment tri-
(1) T-shaped powdery zeolite molecular sieve, novolac resin and hexamethylenetetramine are mixed taking mass ratio as the ratio of 1: 50: 5, add acetone and described novolac resin and hexamethylenetetramine are fully dissolved, the mass ratio of described organic solvent and described novolac resin is 12: 1;
(2) mixed solution of step (1) gained is fully stirred, obtain the homodisperse suspension of zeolite molecular sieve, described mixing time is 5h;
(3) the described suspension of step (2) gained is put into high temperature and high pressure kettle, passing into high pure nitrogen to still internal pressure is 1.5Mpa, be heated to 205 DEG C with the programming rate of 0.25 DEG C/point, and keep 1h, and then keep temperature-resistant, unload and be depressed into normal pressure, release speed is 0.4Mpa/h, after release, be heated to 270 DEG C with the programming rate of 0.25 DEG C/point, and keep 1h, obtain foam curing thing;
(4) will after the described foam curing thing grinding of step (3) gained, pack in the hole of cordierite honeycomb material, and put into high temperature and high pressure kettle, pass into high pure nitrogen to 12Mpa, be heated to 530 DEG C with the programming rate of 5 DEG C/point, and keep 3h, obtain nascent material, it is that 2.5mm and porosity are 60 hole/cm that described cordierite honeycomb material is preferably aperture
2;
(5) the described nascent material of step (4) gained is put into retort and carry out charing, pass into high pure nitrogen as protection gas, be warming up to 850 DEG C with the programming rate of 2 DEG C/min, and keep 40min, obtain described composite.
The micropore size of the described composite obtaining is 0.3～0.5nm, Carbon foam macropore diameter average out to 200 μ m.
Embodiment tetra-
(1) 3A zeolite molecular sieve, novolac resin and hexamethylenetetramine are mixed taking mass ratio as the ratio of 1: 50: 5, add ethanol and described novolac resin and hexamethylenetetramine are fully dissolved, the mass ratio of described organic solvent and described novolac resin is 12: 1;
(2) mixed solution of step (1) gained is fully stirred, obtain the homodisperse suspension of zeolite molecular sieve, described mixing time is 5h;
(3) the described suspension of step (2) gained is put into high temperature and high pressure kettle, passing into high pure nitrogen to still internal pressure is 1.1Mpa, be heated to 202 DEG C with the programming rate of 0.25 DEG C/point, and keep 1.2h, and then keep temperature-resistant, unload and be depressed into normal pressure, release speed is 0.37Mpa/h, after release, be heated to 265 DEG C with the programming rate of 0.25 DEG C/point, and keep 1h, obtain foam curing thing;
(4) will after the described foam curing thing grinding of step (3) gained, pack in the hole of cordierite honeycomb material, and put into high temperature and high pressure kettle, pass into high pure nitrogen to 15Mpa, be heated to 530 DEG C with the programming rate of 4 DEG C/point, and keep 2.5h, obtain nascent material, it is that 2.3mm and porosity are 50 hole/cm that described cordierite honeycomb material is preferably aperture
2;
(5) the described nascent material of step (4) gained is put into retort and carry out charing, pass into high pure nitrogen as protection gas, be warming up to 880 DEG C with the programming rate of 1.5 DEG C/min, and keep 35min, obtain described composite.
The micropore size average out to 0.3nm of the described composite obtaining, Carbon foam macropore diameter average out to 260 μ m.
Although embodiment of the present invention are open as above, but it is not restricted to listed utilization in description and embodiment, it can be applied to various applicable the field of the invention completely, for those skilled in the art, can easily realize other amendment, therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details and illustrates here and the legend of describing.
Claims (5)
1. a preparation method for composite, is characterized in that, comprising:
Step 1, powder-type zeolite molecular sieve, novolac resin and hexamethylenetetramine are mixed taking mass ratio as the ratio of 1: 50: 5, add organic solvent and described novolac resin and hexamethylenetetramine are fully dissolved, the mass ratio of described organic solvent and described novolac resin is 12: 1;
Step 2, fully stirs the mixed solution of step 1 gained, obtains the homodisperse suspension of powder-type zeolite molecular sieve, and described mixing time is 5h;
Step 3, the described suspension of step 2 gained is put into high temperature and high pressure kettle, passing into high pure nitrogen to still internal pressure is 1.2～2Mpa, is heated to 200～210 DEG C, and keeps 0.8～1.5h with the programming rate of 0.25 DEG C/point, then keep temperature-resistant, unload and be depressed into normal pressure, release speed is 0.3～0.5Mpa/h, after release, is heated to 260～280 DEG C with the programming rate of 0.25 DEG C/point, and keep 1h, obtain foam curing thing;
Step 4, packs in the hole of cordierite honeycomb material after the described foam curing thing of step 3 gained is ground, and puts into high temperature and high pressure kettle, pass into high pure nitrogen to 10～16Mpa, be heated to 520～550 DEG C with the programming rate of 3～7 DEG C/point, and keep 2～4h, obtain nascent material;
Step 5, puts into retort by the described nascent material of step 4 gained and carries out charing, passes into high pure nitrogen as protection gas, is warming up to 800～900 DEG C, and keeps 30～45min with the programming rate of 1～3 DEG C/min.
2. preparation method as claimed in claim 1, is characterized in that, described powder-type zeolite molecular sieve is T-shaped zeolite molecular sieve.
3. preparation method as claimed in claim 1, is characterized in that, described organic solvent is ethanol, methyl alcohol or acetone.
4. preparation method as claimed in claim 1, is characterized in that, described cordierite honeycomb material aperture is 2～3mm, and porosity is 40～80 hole/cm
2.
5. according to the prepared a kind of composite of the arbitrary described preparation method of claim 1 to 4, it is characterized in that, described composite micropore size is 0.3～0.5nm, Carbon foam macropore diameter average out to 200～300 μ m.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6259510A (en) * | 1985-09-06 | 1987-03-16 | Kanebo Ltd | Molecular sieve carbon for air separation |
| CN101928133A (en) * | 2010-07-23 | 2010-12-29 | 华东理工大学 | Carbon composite material with integral structure and preparation method thereof |
| CN103253652A (en) * | 2013-05-22 | 2013-08-21 | 华东理工大学 | Preparation method of foam carbon/cordierite composite material |
-
2014
- 2014-03-24 CN CN201410111059.8A patent/CN103877933B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6259510A (en) * | 1985-09-06 | 1987-03-16 | Kanebo Ltd | Molecular sieve carbon for air separation |
| CN101928133A (en) * | 2010-07-23 | 2010-12-29 | 华东理工大学 | Carbon composite material with integral structure and preparation method thereof |
| CN103253652A (en) * | 2013-05-22 | 2013-08-21 | 华东理工大学 | Preparation method of foam carbon/cordierite composite material |
Non-Patent Citations (1)
| Title |
|---|
| 肖南 等: "分级结构沸石/泡沫炭整体复合材料的制备", 《新型碳材料》 * |
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