CN105523542A - Preparation method for closed-cell carbosphere foam material - Google Patents
Preparation method for closed-cell carbosphere foam material Download PDFInfo
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- CN105523542A CN105523542A CN201510763744.3A CN201510763744A CN105523542A CN 105523542 A CN105523542 A CN 105523542A CN 201510763744 A CN201510763744 A CN 201510763744A CN 105523542 A CN105523542 A CN 105523542A
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Abstract
The invention provides a preparation method for a closed-cell carbosphere foam material, which belongs to the field of preparation of heat insulation materials. According to the invention, the method can avoid preparation defects in a spray-drying process, and a heat insulation material prepared by using the method has a low heat conduction coefficient. The method comprises the following steps: with an ester compound as a core material, thermosetting phenolic resin as a wall material and an aqueous solution of anionic surfactant as a dispersion system, preparing a thermosetting phenolic resin microcapsule; carrying out heating and volatilization so as to remove the capsule core of the ester compound so as to obtain phenolic resin closed-cell microspheres; and with the phenolic resin closed-cell microspheres as precursors, carrying out carbonization and graphitization so as to prepare the closed-cell carbosphere foam material. The preparation method avoids defects occurred in the spray-drying process; and the prepared closed-cell carbosphere foam material has a heat conduction coefficient of about 5 W/m.K, much lower than the heat conduction coefficient of a traditional C/C composite material and is an ideal high-temperature-resistant heat insulation foam material.
Description
Technical field
The invention belongs to lagging material preparation field.
Background technology
One of foam materials that closed-cell foam material is mechanical property, heat insulation performance is excellent.Closed pore carbosphere foam materials is a kind of type material with the advantage such as ultralight, hollow, water resistant, insulation, is widely used in the fields such as aerospace, building materials, chemical industry, shipbuilding and explosive wastewater.Closed pore carbosphere is generally with after heat-reactive phenolic resin microballoon, obtains through carbonization and greying.Spray-drying process is one of basic skills of heat-reactive phenolic resin microballoon, but spraying dry still and inner-walls of duct often produce the very strong material of a kind of adhesivity, cause material obstructed; Temperature control is improper also may cause the carbonization of product lump and damage equipment, and product yield reduces greatly.
Summary of the invention
The object of this invention is to provide one and avoid above-mentioned defect, the closed pore carbosphere foam materials preparation method that the lagging material thermal conductivity of preparation is low.
The present invention is achieved by the following technical programs: a kind of closed pore carbosphere foam materials preparation method, comprises the synthesis of thermoset lacquer resins, the preparation of resol closed pore microballoon and preparation three step of closed pore carbosphere foam materials;
The synthesis step of described thermoset lacquer resins is, formaldehyde solution and the phenol of 34% is added in flask, the mol ratio keeping formaldehyde and phenol is 1.2 ~ 1.5, NaOH solution with 40% regulates and keeps the pH of reaction system to be 9, in 90 DEG C of heating in water bath for reaction 3h, obtain thermoset lacquer resins red-brown thick liquid;
The preparation process of described resol closed pore microballoon is, 500ml water is added successively in 1000ml there-necked flask, 30ml tetraethoxy, 60ml polyacrylic acid, stir with the speed of 800r/min, form stable " oil-in-water " type emulsion dispersion system, by reaction system heating in water bath to 90 DEG C, slowly add 100ml thermoset lacquer resins, add 5g vulkacit H solidifying agent, regulate with the HCl solution of 6mol/L and keep the pH of reaction system to be 2, in 94 DEG C of heating in water bath solidification 3h, elimination solution, obtain orange-yellow small suspended particle, i.e. resol microcapsule, orange-yellow resol closed pore microballoon can be obtained after being heated to 70 DEG C of removings tetraethoxy (capsule-core),
The preparation process of described closed pore carbosphere foam materials is, resol closed pore microballoon is pressed certain workpiece shapes casting with after suitable binding agent bonding, becomes resol closed pore microballoon foam materials, with it as the body that pioneers, at N after the demoulding
2carry out the carbonizing treatment of 900 ~ 1100 DEG C under protection, obtain the closed pore carbosphere with agraphitic carbon structure, and then under Ar gas shielded, carry out the graphitization processing of 2100 ~ 2600 DEG C, obtain the closed pore carbosphere foam materials with graphite-structure.
The present invention has following beneficial effect:
Preparation method of the present invention avoids the defect that spray-drying process occurs, the closed pore carbosphere foam materials of preparation, its thermal conductivity is 5W/mK, is a kind of desirable high temperature insulation foam materials.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described.
Specific embodiment: preparation process of the present invention comprises preparation three step of the synthesis of thermoset lacquer resins, the preparation of resol closed pore microballoon and closed pore carbosphere foam materials;
The synthesis step of described thermoset lacquer resins is, formaldehyde solution and the phenol of 34% is added in flask, the mol ratio keeping formaldehyde and phenol is 1.2 ~ 1.5, NaOH solution with 40% regulates and keeps the pH of reaction system to be 9, in 90 DEG C of heating in water bath for reaction 3h, obtain thermoset lacquer resins red-brown thick liquid;
The preparation process of described resol closed pore microballoon is, 500ml water is added successively in 1000ml there-necked flask, 30ml tetraethoxy, 60ml polyacrylic acid, stir with the speed of 800r/min, form stable " oil-in-water " type emulsion dispersion system, by reaction system heating in water bath to 90 DEG C, slowly add 100ml thermoset lacquer resins, add 5g vulkacit H solidifying agent, regulate with the HCl solution of 6mol/L and keep the pH of reaction system to be 2, in 94 DEG C of heating in water bath solidification 3h, elimination solution, obtain orange-yellow small suspended particle, i.e. resol microcapsule, orange-yellow resol closed pore microballoon can be obtained after being heated to 70 DEG C of removings tetraethoxy (capsule-core),
The preparation process of described closed pore carbosphere foam materials is, resol closed pore microballoon is pressed certain workpiece shapes casting with after suitable binding agent bonding, becomes resol closed pore microballoon foam materials, with it as the body that pioneers, at N after the demoulding
2carry out the carbonizing treatment of 900 ~ 1100 DEG C under protection, obtain the closed pore carbosphere with agraphitic carbon structure, and then under Ar gas shielded, carry out the graphitization processing of 2100 ~ 2600 DEG C, obtain the closed pore carbosphere foam materials with graphite-structure.
Preparation method of the present invention avoids the defect that spray-drying process occurs, the closed pore carbosphere foam materials of preparation, its thermal conductivity is about 5W/mK, far below traditional C/C matrix material, is a kind of desirable high temperature insulation foam materials.
Above content is the further description done the present invention in conjunction with concrete embodiment, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, some simple deduction or replace can also be made, all should be considered as belonging to protection scope of the present invention.
Claims (1)
1. a closed pore carbosphere foam materials preparation method, is characterized in that: comprise the synthesis of thermoset lacquer resins, the preparation of resol closed pore microballoon and preparation three step of closed pore carbosphere foam materials;
The synthesis step of described thermoset lacquer resins is, formaldehyde solution and the phenol of 34% is added in flask, the mol ratio keeping formaldehyde and phenol is 1.2 ~ 1.5, NaOH solution with 40% regulates and keeps the pH of reaction system to be 9, in 90 DEG C of heating in water bath for reaction 3h, obtain thermoset lacquer resins red-brown thick liquid;
The preparation process of described resol closed pore microballoon is, 500ml water is added successively in 1000ml there-necked flask, 30ml tetraethoxy, 60ml polyacrylic acid, stir with the speed of 800r/min, form stable " oil-in-water " type emulsion dispersion system, by reaction system heating in water bath to 90 DEG C, slowly add 100ml thermoset lacquer resins, add 5g vulkacit H solidifying agent, regulate with the HCl solution of 6mol/L and keep the pH of reaction system to be 2, in 94 DEG C of heating in water bath solidification 3h, elimination solution, obtain orange-yellow small suspended particle, orange-yellow resol closed pore microballoon is obtained after being heated to 70 DEG C,
The preparation process of described closed pore carbosphere foam materials is, resol closed pore microballoon is pressed certain workpiece shapes casting with after suitable binding agent bonding, becomes resol closed pore microballoon foam materials, with it as the body that pioneers, at N after the demoulding
2carry out the carbonizing treatment of 900 ~ 1100 DEG C under protection, obtain the closed pore carbosphere with agraphitic carbon structure, and then under Ar gas shielded, carry out the graphitization processing of 2100 ~ 2600 DEG C, obtain the closed pore carbosphere foam materials with graphite-structure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510763744.3A CN105523542A (en) | 2015-11-11 | 2015-11-11 | Preparation method for closed-cell carbosphere foam material |
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| CN201510763744.3A CN105523542A (en) | 2015-11-11 | 2015-11-11 | Preparation method for closed-cell carbosphere foam material |
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| CN105523542A true CN105523542A (en) | 2016-04-27 |
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| CN201510763744.3A Pending CN105523542A (en) | 2015-11-11 | 2015-11-11 | Preparation method for closed-cell carbosphere foam material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106654278A (en) * | 2016-11-29 | 2017-05-10 | 南方科技大学 | Novel carbon spheres and preparation method and application thereof |
| CN108483931A (en) * | 2018-06-05 | 2018-09-04 | 孙祎 | A kind of preparation method of high intensity even porous foam glass |
-
2015
- 2015-11-11 CN CN201510763744.3A patent/CN105523542A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106654278A (en) * | 2016-11-29 | 2017-05-10 | 南方科技大学 | Novel carbon spheres and preparation method and application thereof |
| CN106654278B (en) * | 2016-11-29 | 2019-03-05 | 南方科技大学 | A kind of novel carbon ball and the preparation method and application thereof |
| CN108483931A (en) * | 2018-06-05 | 2018-09-04 | 孙祎 | A kind of preparation method of high intensity even porous foam glass |
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Application publication date: 20160427 |
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| WD01 | Invention patent application deemed withdrawn after publication |