CN108675817A - A kind of preparation method and applications of iron oxide red ceramic fibrous composite material - Google Patents

A kind of preparation method and applications of iron oxide red ceramic fibrous composite material Download PDF

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Publication number
CN108675817A
CN108675817A CN201810682453.5A CN201810682453A CN108675817A CN 108675817 A CN108675817 A CN 108675817A CN 201810682453 A CN201810682453 A CN 201810682453A CN 108675817 A CN108675817 A CN 108675817A
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CN
China
Prior art keywords
iron oxide
oxide red
composite material
preparation
ceramic
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Pending
Application number
CN201810682453.5A
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Chinese (zh)
Inventor
宋大为
王北星
曹勇
蔡玉田
田冠宇
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sinopec Energy Management Co Ltd
Guizhou Aerospace Wujiang Electro Mechanical Equipment Co Ltd
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Sinopec Energy Management Co Ltd
Guizhou Aerospace Wujiang Electro Mechanical Equipment Co Ltd
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Application filed by Sinopec Energy Management Co Ltd, Guizhou Aerospace Wujiang Electro Mechanical Equipment Co Ltd filed Critical Sinopec Energy Management Co Ltd
Priority to CN201810682453.5A priority Critical patent/CN108675817A/en
Publication of CN108675817A publication Critical patent/CN108675817A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B30/00Compositions for artificial stone, not containing binders
    • C04B30/02Compositions for artificial stone, not containing binders containing fibrous materials
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20Resistance against chemical, physical or biological attack
    • C04B2111/28Fire resistance, i.e. materials resistant to accidental fires or high temperatures
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/40Porous or lightweight materials
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/20Mortars, concrete or artificial stone characterised by specific physical values for the density
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/30Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
    • C04B2201/32Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Nonwoven Fabrics (AREA)
  • Inorganic Fibers (AREA)
  • Thermal Insulation (AREA)

Abstract

The invention discloses a kind of preparation method and applications of iron oxide red ceramic fibrous composite material, and, mainly using aggressiveness before ceramic fiber blanket saturated absorption and in specified conditions gel, supercritical fluid CO2 dries to form iron oxide red/ceramic fibre advanced composite material (ACM) for it.Iron oxide red prepared by the present invention/ceramic fibre advanced composite material (ACM) has excellent heat-insulating property, mechanical performance, fire prevention and water resistance, easy for construction, and the preparation method of material avoids solvent replacement step, and operation is simple, and process control, production can serialization.

Description

A kind of preparation method and applications of iron oxide red ceramic fibrous composite material
Technical field
The invention belongs to chemical pipeline and equipment soak heat-barrier material technical field more particularly to a kind of iron oxide red/potteries Porcelain fiber advanced composite material (ACM) preparation method and applications.
Technical background
Traditional industry pipeline and insulation of equipment heat-barrier material have rock wool, simple glass cotton blanket, high aluminium silicate wool, polyurethane Deng, wherein rock wool and high aluminium silicate wool poor thermal insulation property, the easy moisture absorption, big installation thickness the shortcomings of, polyurethane non-refractory, easily Combustion.
Iron oxide red/ceramic fibre advanced composite material (ACM) is a kind of light nanoporous amorphous solid-state material of structure-controllable, Its porosity is up to 80%~99.8%, and bore hole size is 1~100nm, high-specific surface area 200-1000m2/g, low-density variation 100~500kg/m3 of range, thermal conductivity is less than 0.018W/mK under normal temperature and pressure, is a kind of resistance that thermal and insulating performance is excellent Combustible material uses it for industrial pipeline and insulation of equipment is heat-insulated is of great significance.
Invention content
The present invention's faces to be to solve to solve traditional industry pipeline and insulation of equipment heat-barrier material heat insulation property Can poor, the easy moisture absorption, non-refractory, it is inflammable, the shortcomings of thickness is big is installed, a kind of iron oxide red/ceramic fibre advanced composite material (ACM) is provided Preparation method and applications.
To achieve the above object, the technical solution adopted in the present invention is:
The present invention is the preparation method of such a iron oxide red ceramic fibrous composite material, and this method is to utilize ceramic fiber blanket Aggressiveness and in specified conditions gel, supercritical fluid CO before saturated absorption2Drying forms iron oxide red/ceramic fibre NEW TYPE OF COMPOSITE material Material;Preparation method avoids solvent replacement step, and operation is simple, and production can serialization.This method comprises the following steps:
1) preparation of aggressiveness before;
2) composite molding of iron oxide red/ceramic fibre advanced composite material (ACM);
3) ageing or ageing of iron oxide red/ceramic fibre advanced composite material (ACM) and surface are modified;
4) drying of iron oxide red/ceramic fibre advanced composite material (ACM).
Wherein, the raw material of the preceding aggressiveness includes silicon source presoma, hydrolyst, additive and solvent.
Further, the silicon source presoma includes one in ethyl orthosilicate, methyl orthosilicate, trim,ethylchlorosilane Kind or two or more mixtures;The hydrolyst includes pure water, hydrochloric acid, nitric acid, sulfuric acid, oxalic acid, acetic acid, ammonium hydroxide, carbon The mixture of one or more of sour ammonium, ammonium hydrogen carbonate;The additive includes iron oxide red, ethyl cellulose, N, N- bis- The mixing of one or more of methylformamide, DMAC N,N' dimethyl acetamide, formamide, acetamide and alkylating reagent Object;The solvent includes the mixture of one or more of straight chain alcohol of 95% or more mass fraction, including methanol, second Alcohol and butanol.
Further, the ceramic fiber blanket is that density made of the ceramic fibre material with a diameter of 2-5 μm is not more than 300kg/m3Homogeneous plate or blanket.
Further, the preceding aggressiveness is formulated by following volume ratio:Ethyl orthosilicate:95% absolute ethyl alcohol:Hydrolysis Catalyst:Additive=10:(40~200):(1~5):(0.1~1.5).
Further, the ageing is that wet gel is put into ethanol solution to impregnate for 24 hours for 35~45 DEG C;The surface Modification is that the wet gel of ageing is put into 50~60 DEG C of progress surface modifications in the ethanol solution added with surface modifier;Institute It includes one kind in pregnancy disilazane, hexamethyldisiloxane to state surface modifier.
Further, the preparation raw material of the preceding aggressiveness includes the component of following volume ratio:Ethyl orthosilicate:95% is anhydrous Ethyl alcohol:Water catalyst:Additive=10:(40~200):(1~5):(0.1~1.5).
In preparation process, the drying is that the iron oxide red of ageing/ceramic fibre advanced composite material (ACM) material is put into super face In boundary's drying equipment, by CO2Fluid injects dry drying kettle, and temperature and pressure is in CO in adjusting drying kettle2The supercritical state of fluid With material under state, the solvent in material is made to be dissolved among supercritical fluid, solvent is collected from separating still discharge gate;With system Standby hydrophilic iron oxide red/ceramic fibre advanced composite material (ACM);Alternatively, the drying is by the modified iron oxide red/ceramic fibre in surface Advanced composite material (ACM) material is put into drying kettle, by CO2Fluid injects drying kettle, and temperature and pressure is in CO in adjusting drying kettle2Stream The supercriticality and material of body, make the solvent in material be dissolved among supercritical fluid, are received from the outlet of separating still Collect solvent;To prepare hydrophobic type iron oxide red/ceramic fibre advanced composite material (ACM).
Wherein, the CO2Fluid controlled at 45~55 DEG C, pressure is 10~18MPa;CO2Fluid flow is 1000 ~3000kg/h, drying time are 3~8h.
The invention also provides application of this iron oxide red ceramic fibrous composite material on making industrial pipeline.
Iron oxide red prepared by the present invention/ceramic fibre advanced composite material (ACM) have high porosity, high-specific surface area, low-density, The excellent performances such as extremely low thermal conductivity are a kind of fire proofings that thermal and insulating performance is splendid.
Compared with prior art, the present invention has substantive distinguishing features and significant progress following prominent:Use above-critical state Under CO2Fluid is recycled as dried medium, the solvent in same system, and solvent consumption is few, and price is cheap, therefore The features such as drying cost is low, non-environmental-pollution.Short preparation period, only 2d, so that it may multiple to prepare a roll of complete ceramic fibre Mould assembly aeroge thermal insulation material, and the prior art needs 6~7d.Ceramic fiber blanket is used as aeroge enhancing base materials, can be well The heat conductivility for reducing ceramic fiber blanket makes aeroge crispness improve, the compound airsetting of ceramic fibre that the present invention produces The thermal coefficient of glue thermal insulation material at normal temperatures is 0.015~0.022W/mK.Present invention process is simple, and continuous production is strong.
Specific implementation mode
The specific implementation mode of the present invention is described further with reference to embodiment.It should be noted that right It is used to help understand the present invention in the explanation of these embodiments, but does not constitute limitation of the invention.In addition, being retouched below Involved technical characteristic can be combined with each other as long as they do not conflict with each other in each embodiment of the present invention stated, The numerical value or ratio being directed to refer both to mass figures or mass ratio such as without explanation.
Embodiment 1:
Iron oxide red/ceramic fibre advanced composite material (ACM) preparation method includes the following steps:Preparation → iron oxide red/ceramics of preceding aggressiveness Composite molding → ageing → drying → detection of fiber advanced composite material (ACM).It is formulated as follows the preceding aggressiveness of volume ratio:Positive silicic acid second Ester:95% absolute ethyl alcohol:Water catalyst:Additive=10:90:2:0.1.Water catalyst be respectively 0.02mol/l hydrochloric acid solutions, 0.01mol/l ammonia spirits, additive are nano-level iron rouge and powder end, reaction time 3h.It is in thickness by reaction glue spray 10mm, density 165kg/m3Ceramic fiber blanket on, make ceramic fiber blanket saturation absorption glue, ceramic fiber blanket without be bubbled, Recess, the equal uniform ground of upper and lower surface are re-fed into 38 DEG C of environment and stand 20min, form iron oxide red/ceramic fibre advanced composite material (ACM) Wet gel.The wet gel of ceramic fibre aeroge is put into 35 DEG C of ethanol solutions and is impregnated for 24 hours.The ceramic fibre gas that will be aged Gel rubber material is put into drying kettle, by CO2Fluid injects drying kettle, and temperature and pressure is in CO in adjusting drying kettle2The super of fluid faces Boundary's state and material make the solvent in material be dissolved among supercritical fluid, and supercritical temperature is 45 DEG C, and pressure is 14MPa;CO2The flow that fluid passes through drying kettle is 2600kg/h, collects solvent from the dry outlet of separating still, shuts down and take out material Material.
Dried is randomly selected into (3 points of performances that can should reflect bulk roll of material as possible) at 3 points, takes 300 × 300mm materials Expect each two pieces, measures density, thermal coefficient, hydrophobicity, mechanical strength.Survey its related data:Material thickness 10mm, density 200kg/m3, room temperature thermal coefficient 0.018W/mK, hydrophobicity 0, S4 grades of combustion rating.
Embodiment 2:
Applied analysis report of the iron oxide red/ceramic fibre advanced composite material (ACM) on industrial pipeline and equipment includes following step Suddenly:Using 40mm thickness iron oxide red/ceramic fibre advanced composite material (ACM) and 200mm thickness Conventional insulations rock wool respectively to 400 DEG C of height Warm steam pipe line carries out insulation, i.e. scheme 1:It is wrapped up, is then used thin along caliber direction with 10mm thickness ceramic nanofibers cottons Iron wire or stainless steel band tie up solid first layer, wrap up the second layer to layer 5 with same way, ceramics are received between paying attention to every layer Rice cellucotton needs the fissure of displacement to wrap up, and ties up solid, finally makees outer protective with color steel or aluminium skin or stainless steel sheet|.Scheme 2:With 50mm thickness asbestos are wrapped up along caliber direction, are tied up solid first layer with thin wire or stainless steel band, are then wrapped up with same way The second layer is to layer 5, and ceramic nanofibers cotton needs the fissure of displacement to wrap up between paying attention to every layer, tie up it is solid, finally use color steel or aluminium Skin or stainless steel sheet| make outer protective.
Under the premise of reaching same heat insulation effect, heat insulation effect and energy consumption to above two material have been carried out to score Analysis, iron oxide red/ceramic fibre advanced composite material (ACM) insulation layer thickness is only Conventional insulation 1/4, save pipeline occupied space and Construction intensity, and energy saving 50%.
The specific application example of the above only present invention, the present invention also has other embodiments, all to use equivalent replacement Or the technical solution that equivalent transformation is formed, it all falls within protection domain of the presently claimed invention.

Claims (10)

1. a kind of preparation method of iron oxide red ceramic fibrous composite material, it is characterised in that:This method is full using ceramic fiber blanket With aggressiveness before absorption and in specified conditions gel, supercritical fluid CO2Drying forms iron oxide red/ceramic fibre advanced composite material (ACM); This method comprises the following steps:
1) preparation of aggressiveness before;
2) composite molding of iron oxide red/ceramic fibre advanced composite material (ACM);
3) ageing or ageing of iron oxide red/ceramic fibre advanced composite material (ACM) and surface are modified;
4) drying of iron oxide red/ceramic fibre advanced composite material (ACM).
2. the preparation method of iron oxide red ceramic fibrous composite material according to claim 1, it is characterised in that:The preceding aggressiveness Raw material include silicon source presoma, hydrolyst, additive and solvent.
3. the preparation method of iron oxide red ceramic fibrous composite material according to claim 2, it is characterised in that:The silicon source Presoma includes the mixture of one or more of ethyl orthosilicate, methyl orthosilicate, trim,ethylchlorosilane;The water It includes one or both of pure water, hydrochloric acid, nitric acid, sulfuric acid, oxalic acid, acetic acid, ammonium hydroxide, ammonium carbonate, ammonium hydrogen carbonate to solve catalyst Above mixture;The additive include iron oxide red, ethyl cellulose, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, The mixture of one or more of formamide, acetamide and alkylating reagent;The solvent includes mass fraction 95% The mixture of one or more of above straight chain alcohol.
4. the preparation method of iron oxide red ceramic fibrous composite material according to claim 1 or 2, it is characterised in that:The pottery Porcelain tapetum fibrosum is that density made of ceramic fibre material with a diameter of 2-5 μm is not more than 300kg/m3Homogeneous plate or Blanket.
5. the preparation method of iron oxide red ceramic fibrous composite material according to claim 2, it is characterised in that:The preceding aggressiveness It is formulated by following volume ratio:Ethyl orthosilicate:95% absolute ethyl alcohol:Hydrolyst:Additive=10:(40~200): (1~5):(0.1~1.5).
6. the preparation method of iron oxide red ceramic fibrous composite material according to claim 1 or 2, it is characterised in that:It is described old Change is that wet gel is put into ethanol solution to impregnate for 24 hours for 35~45 DEG C;It is to put the wet gel of ageing that the surface, which is modified, Enter 50~60 DEG C of progress surface modifications in the ethanol solution added with surface modifier;The surface modifier includes pregnancy two One kind in silazane, hexamethyldisiloxane.
7. the preparation method of iron oxide red ceramic fibrous composite material according to claim 1 or 2, it is characterised in that:Before described The preparation raw material of aggressiveness includes the component of following volume ratio:Ethyl orthosilicate:95% absolute ethyl alcohol:Water catalyst:Additive= 10:(40~200):(1~5):(0.1~1.5).
8. the preparation method of iron oxide red ceramic fibrous composite material according to claim 1 or 2, it is characterised in that:It is described dry Dry is that the iron oxide red of ageing/ceramic fibre advanced composite material (ACM) material is put into supercritical drying equipment, by CO2Fluid injection is dry Dry drying kettle, adjust drying kettle in temperature and pressure in CO2With material under the supercriticality of fluid, make molten in material Agent is dissolved among supercritical fluid, and solvent is collected from separating still discharge gate;It is novel multiple to prepare hydrophilic iron oxide red/ceramic fibre Condensation material;
Alternatively, the drying is that the modified iron oxide red in surface/ceramic fibre advanced composite material (ACM) material is put into drying kettle, it will CO2Fluid injects drying kettle, and temperature and pressure is in CO in adjusting drying kettle2The supercriticality and material of fluid, make material In solvent be dissolved among supercritical fluid, from the outlet of separating still collect solvent;To prepare hydrophobic type iron oxide red/ceramic fibre Advanced composite material (ACM).
9. iron oxide red according to claim 7/ceramic fibre advanced composite material (ACM) drying, it is characterised in that:The CO2Fluid Controlled at 45~55 DEG C, pressure is 10~18MPa;CO2Fluid flow is 1000~3000kg/h, drying time 3 ~8h.
10. a kind of application of iron oxide red ceramic fibrous composite material prepared such as claim 1 on making industrial pipeline.
CN201810682453.5A 2018-06-27 2018-06-27 A kind of preparation method and applications of iron oxide red ceramic fibrous composite material Pending CN108675817A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109851314A (en) * 2018-12-18 2019-06-07 贵州航天乌江机电设备有限责任公司 A kind of preparation method of high-temperature pipe nanoporous aerogel heat-insulating material
CN109853292A (en) * 2018-12-18 2019-06-07 贵州航天乌江机电设备有限责任公司 A kind of preparation method of the compound aerosil sheathing paper of ceramic fiber paper

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CN101081742A (en) * 2006-05-29 2007-12-05 山东鲁阳股份有限公司 Ceramic fiber building fireproof plate
CN101948334A (en) * 2010-09-03 2011-01-19 中山市华山高新陶瓷材料有限公司 Zirconium iron red ceramic pigment and production method thereof
CN107266100A (en) * 2017-07-18 2017-10-20 海城市中兴镁质合成材料有限公司 MgO CaO Fe prepared by a kind of use magnesia-calcium brick fine powder2O3It is electric furnace ramming mass
CN107935540A (en) * 2017-12-19 2018-04-20 贵州航天乌江机电设备有限责任公司 A kind of preparation process of oxidization fiber fiber composite type aerosil insulation blanket
CN108083760A (en) * 2017-12-19 2018-05-29 贵州航天乌江机电设备有限责任公司 A kind of preparation process of the compound aerosil insulation quilt of ceramic fibre

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070272902A1 (en) * 2006-05-25 2007-11-29 Aspen Aerogels, Inc. Aerogel compositions with enhanced performance
CN101081742A (en) * 2006-05-29 2007-12-05 山东鲁阳股份有限公司 Ceramic fiber building fireproof plate
CN101948334A (en) * 2010-09-03 2011-01-19 中山市华山高新陶瓷材料有限公司 Zirconium iron red ceramic pigment and production method thereof
CN107266100A (en) * 2017-07-18 2017-10-20 海城市中兴镁质合成材料有限公司 MgO CaO Fe prepared by a kind of use magnesia-calcium brick fine powder2O3It is electric furnace ramming mass
CN107935540A (en) * 2017-12-19 2018-04-20 贵州航天乌江机电设备有限责任公司 A kind of preparation process of oxidization fiber fiber composite type aerosil insulation blanket
CN108083760A (en) * 2017-12-19 2018-05-29 贵州航天乌江机电设备有限责任公司 A kind of preparation process of the compound aerosil insulation quilt of ceramic fibre

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109851314A (en) * 2018-12-18 2019-06-07 贵州航天乌江机电设备有限责任公司 A kind of preparation method of high-temperature pipe nanoporous aerogel heat-insulating material
CN109853292A (en) * 2018-12-18 2019-06-07 贵州航天乌江机电设备有限责任公司 A kind of preparation method of the compound aerosil sheathing paper of ceramic fiber paper

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