CN101671197B - Preparation method of carbon foam heat insulation material added with hollow ceramic balls - Google Patents
Preparation method of carbon foam heat insulation material added with hollow ceramic balls Download PDFInfo
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- CN101671197B CN101671197B CN2009100939574A CN200910093957A CN101671197B CN 101671197 B CN101671197 B CN 101671197B CN 2009100939574 A CN2009100939574 A CN 2009100939574A CN 200910093957 A CN200910093957 A CN 200910093957A CN 101671197 B CN101671197 B CN 101671197B
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Abstract
The invention relates to a preparation method of carbon foam heat insulation material added with hollow ceramic balls. The method includes the following steps: (1) uniform mixing of raw materials: the foaming formula of phenolic foam comprises the steps: adding 3-5 parts of surfactant, 1-3 parts of foaming agent and 0-2wt% of hollow ceramic microballs to 100 parts of phenolic resin sequentially and uniformly dispersing the mixture by means of combining mechanical stirring and ultrasonic oscillation; (2) adding 5-9 parts of curing agent to the uniformly dispersed mixture of step (1) and after stirring, casting the mixture to a mold to be foamed and solidified, thus obtaining phenolic foam; and (3) carbonized heat treatment: after shelling treatment, putting the phenolic foam in a vacuum carbonization furnace to be heated to the temperature of 800 DEG C at the average rate of 0.5 DEG C/min under vacuum condition, thus obtaining the carbon foam heat insulation material. The high temperature heat insulation material has the advantages of light weight, high strength, low thermal conductivity, low coefficient of heat expansion, low cost, designability and the like.
Description
Technical field
The present invention provides a kind of preparation method who adds the carbon foam heat insulating material of hollow ceramic ball, belongs to the carbon material technical field.
Background technology
Along with progress of science and technology and development, modern material has been proposed harsh more requirement, such as high temperature resistant, corrosion-resistant, density is little, certain physical strength, good heat-insulation effect etc. are arranged.But there are problems such as density is big, intensity is low, heat-proof quality is poor, use temperature is low in the high temperature insulating material of China at present.
Carbon foam is as heat preserving and insulating material of new generation; Be well positioned to meet the requirement of development of modern scientific technology; Have numerous advantages such as light weight, fire-retardant, shock resistance, corrosion resistance and good, high specific strength, it has the mechanical property of low thermal conductivity He each homogeny its undefined structure decision.The aerial use temperature of carbon foam reaches 300 ℃; And under the condition of anaerobic, be heated to 3000 ℃ and still have height heatproof acute degeneration and spatial stability; Its intensity can not reduce with the rising of temperature yet, and this makes it have tempting application potential in high temperature insulating fields such as aerospace.
Summary of the invention
The object of the present invention is to provide a kind of preparation method who adds the carbon foam heat insulating material of hollow ceramic ball, so that the carbon foam that a kind of density is low, intensity is high, thermal conductivity is low, cost is low, have designability to be provided.
A kind of preparation method who adds the carbon foam heat insulating material of hollow ceramic ball of the present invention, this preparation methods may further comprise the steps: (1) raw-material uniform mixing; (2) foaming of polymkeric substance; (3) heat of carbonization is handled.As shown in Figure 1.
(1) raw-material uniform mixing:
The foaming formulation of phenol formaldehyde foam is following:
100 parts in resol
3～5 parts in tensio-active agent
1～3 part of whipping agent
5～9 parts in solidifying agent
Hollow ceramic microballoon 0～2wt%
In liquid phenolic resin, add tensio-active agent, whipping agent and hollow ceramic microballoon in order, with mechanical stirring mixture is disperseed earlier, note reducing destruction, with ultra-sonic oscillation each component is disperseed more equably then microballoon.
(2) foaming of polymkeric substance
Add solidifying agent in the liquid mixture after step (1) is uniformly dispersed, be poured into foaming and curing in the mould after the stirring, obtain phenol formaldehyde foam.Through the addition of increase whipping agent and tensio-active agent, the aperture of the phenol formaldehyde foam that obtains bigger (100～1000 μ m), the content of increase solidifying agent can shorten the foamed solidification time.
(3) heat of carbonization is handled
The phenol formaldehyde foam that step (2) is obtained is put into the vacuum carburization stove, according to heating curve (Fig. 2) after shelling and handling; Speed with average 0.5 ℃/min under vacuum condition is heated to 800 ℃; Cool to room temperature then with the furnace, obtain carbon foam heat insulating material, density is 0.1～0.3g/cm
3
Wherein, the used resol of preparation phenol formaldehyde foam is liquid resole;
Wherein, the used tensio-active agent of preparation phenol formaldehyde foam is a tween-80;
Wherein, the used whipping agent of preparation phenol formaldehyde foam is a Skellysolve A;
Wherein, the used solidifying agent of preparation phenol formaldehyde foam is a hydrochloric acid;
Wherein, described hollow ceramic microballoon, staple is SiO
2And Al
2O
3, the external diameter size is 20 μ m.
The invention has the beneficial effects as follows: the introducing even, the hollow ceramic microballoon of the carbon foam abscess with the present invention makes has improved mechanical property and heat-proof quality; In the preparation process, Working environment is reliable, and is safe.
Principle of the present invention is: the mode that combines through mechanical dispersion and ultrasonic dispersing; The hollow ceramic microballoon is evenly distributed in the liquid resinous mixture; Pass through the foamed solidification process then; The hollow ceramic microballoon is fixed in the phenol formaldehyde foam, handles through the heat of carbonization at last, obtains performance enhanced carbon foam.Because the introducing of toughener hollow ceramic microballoon, the mechanical property and the heat-proof quality of carbon foam are improved.A kind of aerospace field of the present invention is used high temperature insulating material, and its advantage is: density is low, and intensity is high, and thermal conductivity is low, and is corrosion-resistant, and thermal expansivity is low, and cost performance is high, well designability.
Description of drawings
Fig. 1. the preparation technology of carbon foam heat insulating material of the present invention
Fig. 2. carbon foamy carbonization curve
Fig. 3. carbon foamy micro-structure diagram
Fig. 4. carbon foamy micro-structure diagram
Nomenclature:
The wt% mass percent, ℃/min degree centigrade/PM, ℃ degree centigrade, μ m micron, g/cm
3Gram/cubic centimetre
Embodiment
(1) raw-material uniform mixing:
In liquid phenolic resin, add load weighted tensio-active agent, whipping agent and hollow ceramic microballoon in order, with mechanical stirring mixture is disperseed earlier, reduce destruction as far as possible, with ultra-sonic oscillation each component is disperseed more equably then microballoon.
(2) foaming of polymkeric substance
In finely dispersed liquid mixture, add solidifying agent, be poured into after the stirring in the mould, foaming at normal temperatures and pressures and curing obtain phenol formaldehyde foam.Through changing the add-on of whipping agent and tensio-active agent, can obtain different pore size (100～1000 μ m), the content of control solidifying agent can change set time.
(3) heat of carbonization is handled
With phenol formaldehyde foam shell handle after, put into the vacuum carburization stove, according to heating curve (Fig. 2), the speed with average 0.5 ℃/min under vacuum condition is heated to 800 ℃, cools to room temperature then with the furnace, obtains carbon foam article, density is 0.1～0.3g/cm
3
Embodiment one:
Each component raw material of foaming formulation weighing according to 100 parts in resol, 4 parts in tensio-active agent, 2 parts of whipping agents, 7 parts in solidifying agent; In resol, add tensio-active agent, whipping agent in order; Mechanical stirring 1 hour, ultrasonic dispersing was uniformly dispersed it in 2 hours then.Then at normal temperatures and pressures, behind the adding solidifying agent, obtain phenol formaldehyde foam.With phenol formaldehyde foam shell handle after, put into the vacuum carburization stove, under vacuum condition, be heated to 800 ℃ with the speed of average 0.5 ℃/min, obtain carbon foam heat insulating material.Wherein, resol is liquid A step phenolic resin (viscosity (25 ℃): 100～120mPas); Wherein, tensio-active agent is a tween-80; Wherein, whipping agent is a Skellysolve A; Wherein, solidifying agent is a hydrochloric acid.
This carbon foam heat insulating material is carried out performance test: the density of material is 0.172g/cm
3, compressive strength is 4.11MPa, the thermal conductivity in the time of 25 ℃ is 0.25Wm
-1K
-1
Embodiment two:
Each component raw material of foaming formulation weighing according to 100 parts in resol, 4 parts in tensio-active agent, 2 parts of whipping agents, 7 parts in solidifying agent adds tensio-active agent, whipping agent in order in resol, and in mixture, adds the hollow ceramic microballoon of 1wt%.Mechanical stirring 1 hour, ultrasonic dispersing was uniformly dispersed it in 2 hours then.Then at normal temperatures and pressures, behind the adding solidifying agent, obtain phenol formaldehyde foam.With phenol formaldehyde foam shell handle after, put into the vacuum carburization stove, under vacuum condition, be heated to 800 ℃ with the speed of average 0.5 ℃/min, the carbon foam that is enhanced, its microtexture is as shown in Figure 3.Wherein, resol is liquid A step phenolic resin (viscosity (25 ℃): 100～120mPas); Wherein, tensio-active agent is a tween-80; Wherein, whipping agent is a Skellysolve A; Wherein, solidifying agent is a hydrochloric acid; Wherein, the staple of hollow ceramic microballoon is SiO
2And Al
2O
3, the external diameter size is 20 μ m.
This carbon foam heat insulating material is carried out performance test: the density of material is 0.164g/cm
3, compressive strength is 7.76MPa, the thermal conductivity in the time of 25 ℃ is 0.15Wm
-1K
-1
Embodiment three:
Each component raw material of foaming formulation weighing according to 100 parts in resol, 4 parts in tensio-active agent, 2 parts of whipping agents, 7 parts in solidifying agent; In liquid phenolic resin, add tensio-active agent, whipping agent in order, and in mixture, add the hollow ceramic microballoon of 2wt%.Mechanical stirring 1 hour, ultrasonic dispersing was uniformly dispersed it in 2 hours then.At normal temperatures and pressures, behind the adding solidifying agent, obtain phenol formaldehyde foam.With phenol formaldehyde foam shell handle after, put into the vacuum carburization stove, under vacuum condition, be heated to 800 ℃ with the speed of average 0.5 ℃/min, the carbon foam that is enhanced, its microtexture is as shown in Figure 4.Wherein, resol is liquid A step phenolic resin (viscosity (25 ℃): 100～120mPas); Wherein, tensio-active agent is a tween-80; Wherein, whipping agent is a Skellysolve A; Wherein, solidifying agent is a hydrochloric acid; Wherein, the staple of hollow ceramic microballoon is SiO
2And Al
2O
3, the external diameter size is 20 μ m.
This carbon foam heat insulating material is carried out performance test: the density of material is 0.120g/cm
3, compressive strength is 3.53MPa, the thermal conductivity in the time of 25 ℃ is 0.11Wm
-1K
-1
Claims (6)
1. preparation method who adds the carbon foam heat insulating material of hollow ceramic ball, it is characterized in that: this preparation method comprises following step:
(1) raw-material uniform mixing:
The foaming formulation of phenol formaldehyde foam is following:
100 parts in resol
3～5 parts in tensio-active agent
1～3 part of whipping agent
5～9 parts in solidifying agent
Hollow ceramic microballoon 1～2wt%
In resol, add tensio-active agent, whipping agent and hollow ceramic microballoon in order, mixture is carried out homodisperse with the mode that mechanical stirring and ultra-sonic oscillation combine;
(2) foaming of polymkeric substance
Add solidifying agent in the mixture after step (1) is uniformly dispersed, be poured into foaming and curing in the mould after the stirring, obtain phenol formaldehyde foam;
(3) heat of carbonization is handled
With phenol formaldehyde foam shell handle after, put into the vacuum carburization stove, the speed with average 0.5 ℃/min under vacuum condition is heated to 800 ℃, obtains carbon foam heat insulating material.
2. the preparation method of the carbon foam heat insulating material of interpolation hollow ceramic ball according to claim 1 is characterized in that: this resol is liquid resole.
3. the preparation method of the carbon foam heat insulating material of interpolation hollow ceramic ball according to claim 1 is characterized in that: this tensio-active agent is a tween-80.
4. the preparation method of the carbon foam heat insulating material of interpolation hollow ceramic ball according to claim 1 is characterized in that: this whipping agent is a Skellysolve A.
5. the preparation method of the carbon foam heat insulating material of interpolation hollow ceramic ball according to claim 1 is characterized in that: this solidifying agent is a hydrochloric acid.
6. the preparation method of the carbon foam heat insulating material of interpolation hollow ceramic ball according to claim 1 is characterized in that: this hollow ceramic microballoon, staple is SiO
2And Al
2O
3, the external diameter size is 20 μ m.
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| CN2009100939574A CN101671197B (en) | 2009-09-23 | 2009-09-23 | Preparation method of carbon foam heat insulation material added with hollow ceramic balls |
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| CN101671197B true CN101671197B (en) | 2012-11-21 |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103059503B (en) * | 2013-01-11 | 2014-10-01 | 陕西煤业化工技术研究院有限责任公司 | Phenolic foam plastics and preparation method thereof and preparation method of foam carbon |
| CN105984863A (en) * | 2015-02-26 | 2016-10-05 | 上海宝钢化工有限公司 | Preparing method and application of foam carbon |
| CN104909754A (en) * | 2015-06-04 | 2015-09-16 | 合肥和安机械制造有限公司 | Composite modified sepiolite fabric-carbonized foamed phenolic resin based heat insulating material for exhaust pipe of fork truck engine and preparation method of composite modified sepiolite fabric-carbonized foamed phenolic resin based heat insulating material |
| CN104909753A (en) * | 2015-06-04 | 2015-09-16 | 合肥和安机械制造有限公司 | Composite modified colloidal graphite-carbonized foam phenolic resin base insulation material for forklift truck engine exhaust pipe and preparation method of composite modified colloidal graphite-carbonized foam phenolic resin base insulation material |
| CN105967736B (en) * | 2016-05-04 | 2018-06-29 | 山东理工大学 | A kind of preparation method of light porous aluminum phosphate-silicon nitride ceramic ball |
| CN105924215B (en) * | 2016-05-04 | 2018-03-30 | 山东理工大学 | A kind of preparation method of light porous aluminum phosphate sillimanite Ceramic Balls |
| CN105924216B (en) * | 2016-05-04 | 2018-03-30 | 山东理工大学 | A kind of preparation method of light porous aluminum phosphate-Zirconium silicate ceramic ball |
| CN105924217B (en) * | 2016-05-04 | 2018-03-30 | 山东理工大学 | A kind of preparation method of light porous magnesium phosphate-aluminum phosphate Ceramic Balls |
| JP6869328B2 (en) | 2017-03-13 | 2021-05-12 | 旭化成株式会社 | Carbon foam and its manufacturing method |
| CN116621581A (en) * | 2023-04-24 | 2023-08-22 | 西南林业大学 | Thermosetting resin foam carbon and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1057448A (en) * | 1990-04-25 | 1992-01-01 | 株式会社竹中工务店 | Fireproof coating material |
| CN1566207A (en) * | 2003-06-27 | 2005-01-19 | 上海尖端工程材料有限公司 | Process for producing phenol formaldehyde foam products |
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2009
- 2009-09-23 CN CN2009100939574A patent/CN101671197B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1057448A (en) * | 1990-04-25 | 1992-01-01 | 株式会社竹中工务店 | Fireproof coating material |
| CN1566207A (en) * | 2003-06-27 | 2005-01-19 | 上海尖端工程材料有限公司 | Process for producing phenol formaldehyde foam products |
Non-Patent Citations (2)
| Title |
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| 刘明贤 等.酚醛树脂为前驱体制备多孔碳泡沫材料.《功能材料》.2008,第39卷(第1期),引言第1段，第2.2,3.1部分. * |
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