CN106256802A - A kind of organosilicon/phenolic resin binder and prepare the application of refractory material - Google Patents
A kind of organosilicon/phenolic resin binder and prepare the application of refractory material Download PDFInfo
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- CN106256802A CN106256802A CN201610648721.2A CN201610648721A CN106256802A CN 106256802 A CN106256802 A CN 106256802A CN 201610648721 A CN201610648721 A CN 201610648721A CN 106256802 A CN106256802 A CN 106256802A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
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- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
- C04B35/573—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by reaction sintering or recrystallisation
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
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- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
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Abstract
The invention belongs to fire resisting material field, relate generally to a kind of organosilicon/phenolic resin binder and prepare the application of refractory material, described composite refractory raw material includes the SiC aggregate of different-grain diameter, crystalline flake graphite, organic siliconresin, phenolic resin, can apply to build the sizing brick of metallurgical furnace liner or the fire-resistant functional device such as mozzle, flow-controlled device by laying bricks or stones.The present invention introduces the organic siliconresin containing Si O Si main chain in phenolic resin, burning till or during high-temperature service, SiC is generated at phenolic resin pyrolysis carbon skeleton situ by Pintsch process, carbon thermal reduction, full-bodied silica glass thin film is generated after SiC oxidation, oxygen is impregnated with inhibition, is conducive to improving the antioxygenic property of refractory material.Organosilicon/phenolic resin binder has higher Residual carbon than currently used commercial phenolic resin or Colophonium bonding agent, and prepared SiC multiple phase refractory material has higher mechanical strength and antioxygenic property.
Description
Technical field
The invention belongs to fire resisting material field, particularly to a kind of organosilicon/phenolic resin binder and prepare fire proofed wood
The application of material.
Technical background
Carbon containing refractory starts to commercially produce at 20 century 70s, has become as now and is applied to BOF stove, steel
Manufacture of iron and steel by melting container or the most important class refractory materials of technology such as bag, electric arc furnace, slide plate, continuous casting installation for casting.Due to similar graphite
The existence of structure carbon element constituent element, they show preferable shock resistance and erosion-resisting characteristics.The performance of carbon containing refractory
Determined by carbon source, bonding agent, antioxidant and oxide aggregate.Compared with sintered refractory, bonding agent is to carbon containing fire proofed wood
Material plays even more important effect.Bonding agent is possible not only to give blank strength so that it is can load and unload, masonry stacking, and burn
After knot presented in carbon skeleton.The organic bond that carbon containing refractory is conventional does not affect its refractoriness, and can carry
For carbon source.Phenolic resin, as bonding agent, is to realize industrialized production the most the earliest, it is possible to meet refractory material produce with
The Environmental security that applied environment is proposed, high Residual carbon, pyrolysis generate the carbon skeleton of three dimensional structure, stable storing, good flowing
Property be combined with aggregate, the requirement such as reasonable price.But, phenolic resin carbonized belongs to typical solid phase carbonization, and the carbon of generation is
Amorphous glass carbon, antioxygenic property is poor, limits the active time of carbon containing refractory to a certain extent.Used for refractory material
The modification of phenolic resin binder focuses primarily upon catalysis pyrolysis and inorganic nano particle modified two aspects.Catalysis pyrolysis is main
By being mixed into transition metal in phenolic resin, improve degree of graphitization or the in-situ preparation CNT of pyrolytic carbon；Inorganic
Nanometer particle-modified mainly mix nano clay in phenolic resin, Graphene, boron carbide improve phenolic resin pyrolysis carbon
Antioxygenic property.The limitation that phenolic resin pyrolysis carbon antioxygenic property is improved by former approach, later approach is deposited
Easily reunite at nanoparticle, be difficult to scattered problem.
Summary of the invention
For defect and the deficiency of prior art, the present invention proposes a kind of organosilicon/phenolic resin binder and preparation thereof
The application of refractory material, bonding agent compares than commercial phenolic resin binder, and carbon yield can improve about 20%, and this method can be
Phenolic resin pyrolysis carbon situ generates SiC, improves its antioxygenic property combining carbon containing refractory；The side that the present invention uses
Method technique is simple, low in raw material price, be easily controlled.
The present invention proposes following technical solution:
A kind of organosilicon/phenolic resin binder, this bonding agent includes organic siliconresin and phenolic resin.
Concrete, organic siliconresin accounts for the 5%～15% of bonding agent mass fraction, and remainder is phenolic resin, both percentages
It is 100% than summation.
More specifically, described phenolic resin is thermosetting-resoles, the moisture of thermosetting-resoles
Content≤4%, remaining carbon >=42% of thermosetting-resoles；Described organic siliconresin is poly-methylsiloxane tree
Fat.
Described organosilicon/phenolic resin binder is for preparing the application of refractory material.
Concrete, using SiC as aggregate and fine powder, graphite is carbon source, and bonding agent is described organosilicon phenolic resin knot
Mixture, above-mentioned raw materials obtains refractory material after pressed compact is fired.
More specifically, the particle size range of described SiC includes: 0～0.068mm, 0.1～0.5mm and 0.5～1mm tri-kinds,
Its purity is that SiC content is more than 90%, and the SiC of 0.1～0.5mm and 0.5～1mm particle diameter is aggregate, 0～0.068mm particle diameter
SiC is fine powder；Graphite is high-purity crystalline flake graphite, and particle diameter is 300 μm, and fixed carbon content is 99.9%.
Further, by mass percentage, aggregate is 60%, and fine powder is 25%, and carbon source is 8%, and bonding agent is 7%.
It addition, the detailed process fired is: the base substrate suppressed is put in atmosphere sintering furnace, vacuum be 5KPa with
Under, it is passed through inert protective gas, is warming up to 1400 DEG C with 5 DEG C/min programming rate, be incubated 2 hours, take out goods after cooling i.e.
Obtain refractory material.
The invention have the advantages that
(1) bonding agent of the present invention is compared than commercial phenolic resin binder, and carbon yield can improve about 20%；
(2) this method can generate SiC at phenolic resin pyrolysis carbon situ, improves it and combines the anti-of carbon containing refractory
Oxidation susceptibility；
(3) the method technique that the present invention uses is simple, low in raw material price, be easily controlled.
Detailed description of the invention
Organosilicon/the phenolic resin binder of the present invention includes organic siliconresin and phenolic resin.Concrete, organosilicon tree
Fat accounts for the 5%～15% of bonding agent mass fraction, and remainder is phenolic resin, and both percentage ratio summations are 100%.More specifically,
Phenolic resin is thermosetting-resoles, moisture≤4% of thermosetting-resoles, thermosetting first rank phenolic aldehyde
Remaining carbon >=42% of resin, mean molecule quantity is 400；Described organic siliconresin is poly-methylsiloxane resin, preferably,
Polymethyl-benzene base organic siliconresin, the mean molecule quantity of polymethyl-benzene base organic siliconresin is 1200.
Preferably, by mass percentage, organic siliconresin accounts for 5% in resinoid bond.
Preferably, by mass percentage, organic siliconresin accounts for 10% in resinoid bond.
Preferably, by mass percentage, organic siliconresin accounts for 15% in resinoid bond.
Organosilicon/phenolic resin binder is for preparing the application of refractory material, and detailed process is: choose different-grain diameter
SiC as aggregate, fine powder and crystalline flake graphite as carbon source；Graininess organic siliconresin and phenolic resin are pressed certain mass mark
It is dissolved in dehydrated alcohol after mixed grinding；Cement mixer batch mixing, by two kinds of resin solution mixing, stirs；Drying, pressure
Burn till at a temperature of 1400 DEG C after base molding, solidification.
The SiC particle size range used includes: 0～0.068mm, 0.1～0.5mm, 0.5～1mm tri-kind, SiC content is more than
90%, 0.1～the SiC of 0.5mm and 0.5～1mm particle diameter is aggregate, and the SiC of 0～0.068mm particle diameter is fine powder；Crystalline flake graphite grain
Footpath 300 μm, additional by mass fraction 7%, at inert atmosphere kiln roasting after solidification, firing temperature is 1400 DEG C.
Concrete, described milling parameters is: resinoid bond is 2:1 with the mass ratio of medium ball, phenolic resin
Being 1:4 with the mass ratio of dehydrated alcohol, Ball-milling Time is 1 hour, and drum's speed of rotation is 400r/min；Firing process parameter: protect
Protecting gas is nitrogen or argon, and flow 500ml/min is warming up to 1400 DEG C with 5 DEG C/min programming rate, is incubated 2 hours.
The following is the embodiment that inventor provides, the invention is not restricted to below example, in the scope that the present invention is given
In, all can prepare satisfactory SiC-C composite refractory.
Embodiment 1:
Bonding agent is pure commercial heatset resol, be dissolved in after grinding in dehydrated alcohol resinoid bond molten
Liquid.
Resinoid bond is 2:1 with the mass ratio of medium ball, and Ball-milling Time is 1 hour, and drum's speed of rotation is 400r/min；
Stir in the SiC (0.5～1mm:45wt%, 0.1～0.5mm:25wt%) of coarse granule and middle granule is poured into cement mixing pond
Mix homogeneously, pours the particulate material of mix homogeneously into by the resin-bonded agent solution prepared according to additional resinoid bond 7wt%
In, continue mixing fully wrapped around to bonding agent, then pour SiC fine powder (0～0.044mm:30wt%) into, be stirred for 0.5 hour extremely
Fine powder, granule, bonding agent mix homogeneously.120 DEG C of solidifications after molding.Burn till concrete technology parameter: protective gas is nitrogen, with 5
DEG C/speed of min is incubated 2 hours after being raised to 1400 DEG C.Take out, the rupture strength of test article, comprcssive strength, bulk density,
It is respectively as follows: 11.37MPa, 49.43MPa, 3.27g/cm3.It is calculated bonding agent Residual carbon according to burning till before and after's product weight difference
It is 46%, characterizes the antioxygenic property of sample, oxidation peak by the temperature that oxidation heat liberation peak value in differential scanning calorimetric curve is corresponding
Value temperature is 546 DEG C.
Embodiment 2:
Polymethyl-benzene base organic siliconresin content in bonding agent is 5wt%, and thermosetting-resoles is 95wt%,
It is dissolved in after mixed grinding in dehydrated alcohol and i.e. obtains resin-bonded agent solution.
Resinoid bond is 2:1 with the mass ratio of medium ball, and Ball-milling Time is 1 hour, and drum's speed of rotation is 400r/min；
Stir in the SiC (0.5～1mm:45wt%, 0.1～0.5mm:25wt%) of coarse granule and middle granule is imported cement mixing pond
Mix homogeneously, pours the particulate material of mix homogeneously into by the resin-bonded agent solution prepared according to additional resinoid bond 7wt%
In, continue mixing fully wrapped around to bonding agent, then pour SiC fine powder (0～0.044mm:30wt%) into, be stirred for 0.5 hour extremely
Fine powder, granule, bonding agent mix homogeneously.120 DEG C of solidifications after molding.Burn till concrete technology parameter: protective gas is nitrogen, with 5
DEG C/speed of min is raised to 1400 DEG C and is incubated 2 hours.Take out, the rupture strength of test article, comprcssive strength, bulk density, point
It is not: 13.41MPa, 54.64MPa, 3.25g/cm3.According to burning till before and after's product weight difference and being calculated bonding agent Residual carbon it is
53%, improve 7% than embodiment 1.The anti-of sample is characterized by the temperature that oxidation heat liberation peak value in differential scanning calorimetric curve is corresponding
Oxidation susceptibility, oxidation peak temperature is 618 DEG C, improves about 72 DEG C than embodiment 1.
Embodiment 3:
Polymethyl-benzene base organic siliconresin content in bonding agent is 10wt%, and thermosetting-resoles is
90wt%, is dissolved in after mixed grinding in dehydrated alcohol and obtains resinoid bond.
Resinoid bond is 2:1 with the mass ratio of medium ball, and Ball-milling Time is 1 hour, and drum's speed of rotation is 400r/min；
Stir in the SiC (0.5～1mm:45wt%, 0.1～0.5mm:25wt%) of coarse granule and middle granule is imported cement mixing pond
Mix homogeneously, pours the particulate material of mix homogeneously into by the resin-bonded agent solution prepared according to additional resinoid bond 7wt%
In, continue mixing fully wrapped around to bonding agent, then pour SiC fine powder (0～0.044mm:30wt%) into, be stirred for 0.5 hour extremely
Fine powder, granule, bonding agent mix homogeneously.Solidify at a temperature of 120 DEG C after molding.Burn till concrete technology parameter: protective gas is
Nitrogen, is raised to 1400 DEG C with the speed of 5 DEG C/min and is incubated 2 hours.Take out, the rupture strength of test article, comprcssive strength, volume
Density, is respectively as follows: 15.36MPa, 52.28MPa, 3.24g/cm3.It is calculated bonding agent according to burning till before and after's product weight difference
Residual carbon is 59%, improves 6% than embodiment 2.The temperature corresponding with oxidation heat liberation peak value in differential scanning calorimetric curve characterizes
The antioxygenic property of sample, oxidation peak temperature is 673 DEG C, improves about 55 DEG C than embodiment 2.
Embodiment 4:
Polymethyl-benzene base organic siliconresin content in bonding agent is 15wt%, thermosetting-resoles 85wt%,
It is dissolved in after mixed grinding in dehydrated alcohol and i.e. obtains resin-bonded agent solution.
Resinoid bond is 2:1 with the mass ratio of medium ball, and Ball-milling Time is 1 hour, and drum's speed of rotation is 400r/min；
Stir in the SiC (0.5～1mm:45wt%, 0.1～0.5mm:25wt%) of coarse granule and middle granule is imported cement mixing pond
Mix homogeneously, pours the particulate material of mix homogeneously into by the resin-bonded agent solution prepared according to additional resinoid bond 7wt%
In, continue mixing fully wrapped around to bonding agent, then pour SiC fine powder (0～0.044mm:30wt%) into, be stirred for 0.5 hour extremely
Fine powder, granule, bonding agent mix homogeneously.120 DEG C of solidifications after molding.Burn till concrete technology parameter: protective gas is nitrogen, with 5
DEG C/speed of min is raised to 1400 DEG C and is incubated 2 hours.Take out, the rupture strength of test article, comprcssive strength, bulk density, point
It is not: 16.29MPa, 56.73MPa, 3.22g/cm3.According to burning till before and after's product weight difference and being calculated bonding agent Residual carbon it is
61%, improve 2% than embodiment 3.The anti-of sample is characterized by the temperature that oxidation heat liberation peak value in differential scanning calorimetric curve is corresponding
Oxidation susceptibility, oxidation peak temperature is 709 DEG C, improves about 36 DEG C than embodiment 3.
Claims (8)
1. organosilicon/phenolic resin binder, it is characterised in that this bonding agent includes organic siliconresin and phenolic resin.
2. organosilicon/phenolic resin binder as claimed in claim 1, it is characterised in that organic siliconresin accounts for bonding agent matter
The 5%～15% of amount mark, remainder is phenolic resin, and both percentage ratio summations are 100%.
3. organosilicon/phenolic resin binder as claimed in claim 1 or 2, it is characterised in that described phenolic resin is heat
Solidity resol, moisture≤4% of thermosetting-resoles, the remaining carbon of thermosetting-resoles
>=42%；Described organic siliconresin is poly-methylsiloxane resin.
4. organosilicon/the phenolic resin binder described in claim 1,2 or 3 is for preparing the application of refractory material.
Applying the most as claimed in claim 4, it is characterised in that using SiC as aggregate and fine powder, graphite is carbon source, bonding agent
For the organosilicon phenolic resin binder described in claim 1,2 or 3, above-mentioned raw materials obtains refractory material after pressed compact is fired.
Apply the most as claimed in claim 5, it is characterised in that the particle size range of described SiC includes: 0～0.068mm, 0.1
～0.5mm and 0.5～1mm tri-kinds, its purity is that SiC content is more than 90%, and the SiC of 0.1～0.5mm and 0.5～1mm particle diameter is
Aggregate, the SiC of 0～0.068mm particle diameter is fine powder；Graphite is high-purity crystalline flake graphite, and particle diameter is 300 μm, and fixed carbon content is
99.9%.
7. the application as described in claim 5 or 6, it is characterised in that by mass percentage, aggregate is 60%, and fine powder is
25%, carbon source is 8%, and bonding agent is 7%.
8. the application as described in claim 5 or 6, it is characterised in that the detailed process fired is: put into by the base substrate suppressed
In atmosphere sintering furnace, vacuum is below 5KPa, is passed through inert protective gas, is warming up to 1400 DEG C with 5 DEG C/min programming rate,
It is incubated 2 hours, takes out goods after cooling and i.e. obtain refractory material.
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| CN110668447A (en) * | 2019-10-31 | 2020-01-10 | 哈尔滨工业大学 | Synthesis method of silicon carbide nanowire |
| CN111777417A (en) * | 2020-07-29 | 2020-10-16 | 攀钢冶金材料有限责任公司 | Silicon carbide-carbon ramming mass for blast furnace slag high-temperature carbonization electric furnace and preparation method thereof |
| CN113461431A (en) * | 2021-05-17 | 2021-10-01 | 江苏苏嘉集团新材料有限公司 | Resin binder with frosted texture for refractory material and preparation process thereof |
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| CN111777417A (en) * | 2020-07-29 | 2020-10-16 | 攀钢冶金材料有限责任公司 | Silicon carbide-carbon ramming mass for blast furnace slag high-temperature carbonization electric furnace and preparation method thereof |
| CN113461431A (en) * | 2021-05-17 | 2021-10-01 | 江苏苏嘉集团新材料有限公司 | Resin binder with frosted texture for refractory material and preparation process thereof |
| CN113461431B (en) * | 2021-05-17 | 2022-07-19 | 江苏苏嘉集团新材料有限公司 | Resin binder with frosted texture for refractory material and preparation process thereof |
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Application publication date: 20161228 |