CN105948785A - Porous ceramic composite thermal insulation material and preparation method thereof - Google Patents
Porous ceramic composite thermal insulation material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a porous ceramic composite thermal insulation material and a preparation method thereof. The porous ceramic composite thermal insulation material is prepared from the following components: polycrystalline mullite fiber, nano silica, beta-cyclodextrin, methyl p-hydroxybenzoate, boron carbide, silicon carbide, polyacrylamide, rosin, water glass, polyvinyl chloride, ethylene bis stearamide, silica sol, sodium carboxymethylcellulose, hydrochloric acid, isopropanol and water. The preparation method includes: firstly cutting polycrystalline mullite fiber into a length of 1-3mm, then mixing the cut polycrystalline mullite fiber with hydrochloric acid, and performing rinsing with clean water, repeating the operation three times to wash off fiber balls in the fiber, then adding the remaining components and performing stirring, pouring the mixture into a mold, conducting pressing to drain water so as to obtain a wet blank; and drying the wet blank in an oven, then sintering the blank in a muffle furnace. The porous ceramic composite thermal insulation material provided by the invention has a density range of 0.77-0.81g/cm<3>, compressive strength up to 7.28MPa, and strong rigidity, and also has very good thermal insulation effect.
Description
Technical field
The present invention relates to Material Field, be specifically related to a kind of porous ceramics composite heat-insulated material and preparation method thereof.
Background technology
In recent years, along with developing rapidly of science and technology, the research and development of new material are more popular, and performance also becomes increasingly complex and superior, and ceramic porous material is exactly the functional type material that one of which is the most emerging.Its preparation technology mainly has foam impregnation, adds pore creating material, foaming and vacuum filtration etc..Foam impregnation is suitable for preparing the material that the porosity is high and percent opening is big, and its shortcoming is uncontrollable shape and density and pore opening.Adding pore creating material to can be used for preparing the different and adjustable material of the porosity, its shortcoming is that gas cell distribution is poor, it is impossible to prepare macroporosity material.Foaming rule is easier to control the net shape of material, and composition and density, its shortcoming is that ingredient requirement is higher, and process conditions are difficult to control to.And prepare porous material by ceramic fibre, owing to process equipment is the most relatively simple, and the material porosity of preparation is high and developed widely and study, and also is further being studied and applying.
Summary of the invention
Solve the technical problem that:It is an object of the invention to provide a kind of porous ceramics composite heat-insulated material, density range is at 0.77-0.81g/cm3Between, compressive strength is the highest can be to 7.28MPa, and rigidity is strong, has good effect of heat insulation simultaneously.
Technical scheme:A kind of porous ceramics composite heat-insulated material, is prepared from weight portion by following component: polycrystalline mullite fibre 15-30 part, nano silicon 5-10 part, cycloheptaamylose 4-7 part, methyl parahydroxybenzoate 0.1-0.3 part, boron carbide 6-10 part, carborundum 6-10 part, polyacrylamide 0.2-0.5 part, Colophonium 0.2-0.4 part, waterglass 1-2 part, polrvinyl chloride 0.5-1 part, vinyl bis-stearamides 0.1-0.2 part, Ludox 1-2 part, sodium carboxymethyl cellulose 0.5-1 part, hydrochloric acid 10-20 part, isopropanol 10-30 part, water 60-90 part.
Further preferred, described a kind of porous ceramics composite heat-insulated material, it is prepared from weight portion by following component: polycrystalline mullite fibre 20-25 part, nano silicon 6-9 part, cycloheptaamylose 5-6 part, methyl parahydroxybenzoate 0.15-0.25 part, boron carbide 7-9 part, carborundum 7-9 part, polyacrylamide 0.3-0.4 part, Colophonium 0.25-0.35 part, waterglass 1.2-1.8 part, polrvinyl chloride 0.6-0.9 part, vinyl bis-stearamides 0.11-0.17 part, Ludox 1.3-1.7 part, sodium carboxymethyl cellulose 0.6-0.9 part, hydrochloric acid 13-18 part, isopropanol 15-25 part, water 70-80 part.
The preparation method of above-mentioned porous ceramics composite heat-insulated material comprises the following steps:
Step 1: polycrystalline mullite fibre is cut into 1-3 mm length；
Step 2: by the polycrystalline mullite fibre cut and mixed in hydrochloric acid, rinse with clear water after stirring 3-5 minute with blender；
Step 3: 3 steps 2 of repetitive operation, washes away the fibrous nodules in fiber；
Step 4: add remaining ingredient, stir 2-3 hour under rotating speed 300-500r/min with blender；
Step 5: slurry is poured into and carries out 2-3 hour discharge moisture of compacting in mould under pressure 80-110KPa, obtain wet base；
Step 6: put in baking oven by wet base, is dried 10-12 hour at temperature 70-80 DEG C；
Step 7: put in Muffle furnace and be sintered, heating rate is that 2 DEG C/min is warming up to 500-600 DEG C, is incubated 2-3 hour, then rises to 1150-1300 DEG C with 5 DEG C/min of speed, is incubated 2-3 hour, cools down and get final product.
It is further preferred that a length of 2 millimeters of polycrystalline mullite fibre in step 1.
It is further preferred that mixing time is 4 minutes in step 2.
It is further preferred that step 4 medium speed is 350-450r/min, the time is 2.5 hours.
It is further preferred that pressure is 90-100KPa in step 5, the press time is 2.5 hours.
It is further preferred that temperature is 75 DEG C in step 6, drying time is 10.5-11.5 hour.
It is further preferred that be warming up to 550 DEG C for the first time in step 7, being incubated 2.5 hours, second time is warming up to 1200-1250 DEG C, and temperature retention time is 2.5 hours.
Beneficial effect:The density range of the porous ceramics composite heat-insulated material of the present invention is at 0.77-0.81g/cm3Between, compressive strength is the highest can be to 7.28MPa, and rigidity is strong, and density has with compressive strength and necessarily contacts, and density is the biggest, and compressive strength is the biggest.The present invention has good effect of heat insulation simultaneously, and after carrying out the calcination of 300 seconds, its surface temperature is about 1590 DEG C, and minimum only 74 DEG C of back temperature.
Detailed description of the invention
Embodiment 1
A kind of porous ceramics composite heat-insulated material, is prepared from weight portion by following component: polycrystalline mullite fibre 15 parts, nano silicon 5 parts, cycloheptaamylose 4 parts, methyl parahydroxybenzoate 0.1 part, boron carbide 6 parts, carborundum 6 parts, polyacrylamide 0.2 part, Colophonium 0.2 part, waterglass 1 part, polrvinyl chloride 0.5 part, vinyl bis-stearamides 0.1 part, Ludox 1 part, sodium carboxymethyl cellulose 0.5 part, hydrochloric acid 10 parts, isopropanol 10 parts, 60 parts of water.
The preparation method of above-mentioned porous ceramics composite heat-insulated material is: polycrystalline mullite fibre is first cut into 1 mm length, again and mixed in hydrochloric acid, rinse with clear water after stirring 3 minutes with blender, repetitive operation 3 times, wash away the fibrous nodules in fiber, be subsequently adding remaining ingredient, stir 2 hours under rotating speed 300r/min with blender, pour into mould to be carried out under pressure 80KPa suppress 2 hours and discharge moisture, obtain wet base；Putting in baking oven by wet base, put in Muffle furnace and be sintered under temperature 70 C after being dried 10 hours, heating rate is that 2 DEG C/min is warming up to 500 DEG C, is incubated 2 hours, then rises to 1150 DEG C with 5 DEG C/min of speed, is incubated 2 hours, cools down and get final product.
Embodiment 2
A kind of porous ceramics composite heat-insulated material, is prepared from weight portion by following component: polycrystalline mullite fibre 22 parts, nano silicon 7.5 parts, cycloheptaamylose 5.5 parts, methyl parahydroxybenzoate 0.2 part, boron carbide 8 parts, carborundum 8 parts, polyacrylamide 0.35 part, Colophonium 0.3 part, waterglass 1.5 parts, polrvinyl chloride 0.75 part, vinyl bis-stearamides 0.15 part, Ludox 1.5 parts, sodium carboxymethyl cellulose 0.75 part, hydrochloric acid 15 parts, isopropanol 20 parts, 75 parts of water.
The preparation method of above-mentioned porous ceramics composite heat-insulated material is: polycrystalline mullite fibre is first cut into 2 mm lengths, again and mixed in hydrochloric acid, rinse with clear water after stirring 4 minutes with blender, repetitive operation 3 times, wash away the fibrous nodules in fiber, be subsequently adding remaining ingredient, stir 2.5 hours under rotating speed 400r/min with blender, pour into mould to be carried out under pressure 95KPa suppress 2.5 hours and discharge moisture, obtain wet base；Putting in baking oven by wet base, put in Muffle furnace and be sintered at temperature 75 DEG C after being dried 11 hours, heating rate is that 2 DEG C/min is warming up to 550 DEG C, is incubated 2.5 hours, then rises to 1230 DEG C with 5 DEG C/min of speed, is incubated 2.5 hours, cools down and get final product.
Embodiment 3
A kind of porous ceramics composite heat-insulated material, is prepared from weight portion by following component: polycrystalline mullite fibre 30 parts, nano silicon 10 parts, cycloheptaamylose 7 parts, methyl parahydroxybenzoate 0.3 part, boron carbide 10 parts, carborundum 10 parts, polyacrylamide 0.5 part, Colophonium 0.4 part, waterglass 2 parts, polrvinyl chloride 1 part, vinyl bis-stearamides 0.2 part, Ludox 2 parts, sodium carboxymethyl cellulose 1 part, hydrochloric acid 20 parts, isopropanol 30 parts, 90 parts of water.
The preparation method of above-mentioned porous ceramics composite heat-insulated material is: polycrystalline mullite fibre is first cut into 3 mm lengths, again and mixed in hydrochloric acid, rinse with clear water after stirring 5 minutes with blender, repetitive operation 3 times, wash away the fibrous nodules in fiber, be subsequently adding remaining ingredient, stir 3 hours under rotating speed 500r/min with blender, pour into mould to be carried out under pressure 110KPa suppress 3 hours and discharge moisture, obtain wet base；Putting in baking oven by wet base, put in Muffle furnace and be sintered at temperature 80 DEG C after being dried 12 hours, heating rate is that 2 DEG C/min is warming up to 600 DEG C, is incubated 3 hours, then rises to 1300 DEG C with 5 DEG C/min of speed, is incubated 3 hours, cools down and get final product.
Embodiment 4
A kind of porous ceramics composite heat-insulated material, is prepared from weight portion by following component: polycrystalline mullite fibre 20 parts, nano silicon 6 parts, cycloheptaamylose 5 parts, methyl parahydroxybenzoate 0.15 part, boron carbide 7 parts, carborundum 7 parts, polyacrylamide 0.3 part, Colophonium 0.25 part, waterglass 1.2 parts, polrvinyl chloride 0.6 part, vinyl bis-stearamides 0.11 part, Ludox 1.3 parts, sodium carboxymethyl cellulose 0.6 part, hydrochloric acid 13 parts, isopropanol 15 parts, 70 parts of water.
The preparation method of above-mentioned porous ceramics composite heat-insulated material is: polycrystalline mullite fibre is first cut into 2 mm lengths, again and mixed in hydrochloric acid, rinse with clear water after stirring 4 minutes with blender, repetitive operation 3 times, wash away the fibrous nodules in fiber, be subsequently adding remaining ingredient, stir 2.5 hours under rotating speed 350r/min with blender, pour into mould to be carried out under pressure 90KPa suppress 2.5 hours and discharge moisture, obtain wet base；Putting in baking oven by wet base, put in Muffle furnace and be sintered at temperature 75 DEG C after being dried 10.5 hours, heating rate is that 2 DEG C/min is warming up to 550 DEG C, is incubated 2.5 hours, then rises to 1200 DEG C with 5 DEG C/min of speed, is incubated 2.5 hours, cools down and get final product.
Embodiment 5
A kind of porous ceramics composite heat-insulated material, is prepared from weight portion by following component: polycrystalline mullite fibre 25 parts, nano silicon 9 parts, cycloheptaamylose 6 parts, methyl parahydroxybenzoate 0.25 part, boron carbide 9 parts, carborundum 9 parts, polyacrylamide 0.4 part, Colophonium 0.35 part, waterglass 1.8 parts, polrvinyl chloride 0.9 part, vinyl bis-stearamides 0.17 part, Ludox 1.7 parts, sodium carboxymethyl cellulose 0.9 part, hydrochloric acid 18 parts, isopropanol 25 parts, 80 parts of water.
The preparation method of above-mentioned porous ceramics composite heat-insulated material is: polycrystalline mullite fibre is first cut into 2 mm lengths, again and mixed in hydrochloric acid, rinse with clear water after stirring 4 minutes with blender, repetitive operation 3 times, wash away the fibrous nodules in fiber, be subsequently adding remaining ingredient, stir 2.5 hours under rotating speed 450r/min with blender, pour into mould to be carried out under pressure 100KPa suppress 2.5 hours and discharge moisture, obtain wet base；Putting in baking oven by wet base, put in Muffle furnace and be sintered at temperature 75 DEG C after being dried 11.5 hours, heating rate is that 2 DEG C/min is warming up to 550 DEG C, is incubated 2.5 hours, then rises to 1250 DEG C with 5 DEG C/min of speed, is incubated 2.5 hours, cools down and get final product.
Comparative example 1
The present embodiment is not contain cycloheptaamylose with the difference of embodiment 5.Specifically:
A kind of porous ceramics composite heat-insulated material, is prepared from weight portion by following component: polycrystalline mullite fibre 25 parts, nano silicon 9 parts, methyl parahydroxybenzoate 0.25 part, boron carbide 9 parts, carborundum 9 parts, polyacrylamide 0.4 part, Colophonium 0.35 part, waterglass 1.8 parts, polrvinyl chloride 0.9 part, vinyl bis-stearamides 0.17 part, Ludox 1.7 parts, sodium carboxymethyl cellulose 0.9 part, hydrochloric acid 18 parts, isopropanol 25 parts, 80 parts of water.
The preparation method of above-mentioned porous ceramics composite heat-insulated material is: polycrystalline mullite fibre is first cut into 2 mm lengths, again and mixed in hydrochloric acid, rinse with clear water after stirring 4 minutes with blender, repetitive operation 3 times, wash away the fibrous nodules in fiber, be subsequently adding remaining ingredient, stir 2.5 hours under rotating speed 450r/min with blender, pour into mould to be carried out under pressure 100KPa suppress 2.5 hours and discharge moisture, obtain wet base；Putting in baking oven by wet base, put in Muffle furnace and be sintered at temperature 75 DEG C after being dried 11.5 hours, heating rate is that 2 DEG C/min is warming up to 550 DEG C, is incubated 2.5 hours, then rises to 1250 DEG C with 5 DEG C/min of speed, is incubated 2.5 hours, cools down and get final product.
Comparative example 2
The present embodiment is not contain polyacrylamide and waterglass with the difference of embodiment 5.Specifically:
A kind of porous ceramics composite heat-insulated material, is prepared from weight portion by following component: polycrystalline mullite fibre 25 parts, nano silicon 9 parts, cycloheptaamylose 6 parts, methyl parahydroxybenzoate 0.25 part, boron carbide 9 parts, carborundum 9 parts, Colophonium 0.35 part, polrvinyl chloride 0.9 part, vinyl bis-stearamides 0.17 part, Ludox 1.7 parts, sodium carboxymethyl cellulose 0.9 part, hydrochloric acid 18 parts, isopropanol 25 parts, 80 parts of water.
The preparation method of above-mentioned porous ceramics composite heat-insulated material is: polycrystalline mullite fibre is first cut into 2 mm lengths, again and mixed in hydrochloric acid, rinse with clear water after stirring 4 minutes with blender, repetitive operation 3 times, wash away the fibrous nodules in fiber, be subsequently adding remaining ingredient, stir 2.5 hours under rotating speed 450r/min with blender, pour into mould to be carried out under pressure 100KPa suppress 2.5 hours and discharge moisture, obtain wet base；Putting in baking oven by wet base, put in Muffle furnace and be sintered at temperature 75 DEG C after being dried 11.5 hours, heating rate is that 2 DEG C/min is warming up to 550 DEG C, is incubated 2.5 hours, then rises to 1250 DEG C with 5 DEG C/min of speed, is incubated 2.5 hours, cools down and get final product.
Each embodiment being compared with comparative example, comparing result see table, it may be seen that the density range of the embodiment of the present invention is at 0.77-0.81g/cm3Between, compressive strength is the highest can be to 7.28MPa, and rigidity is strong, and density has with compressive strength and necessarily contacts, and density is the biggest, and compressive strength is the biggest.The present invention has good effect of heat insulation simultaneously, and after carrying out the calcination of 300 seconds, its surface temperature is 1591 DEG C, and back temperature is minimum is only 74 DEG C.
The performance indications of table 1 porous ceramics composite heat-insulated material
Note: in ignition test, specimen size is 50mm*25mm, quality is 25g.
Claims (9)
1. a porous ceramics composite heat-insulated material, it is characterized in that: be prepared from weight portion by following component: polycrystalline mullite fibre 15-30 part, nano silicon 5-10 part, cycloheptaamylose 4-7 part, methyl parahydroxybenzoate 0.1-0.3 part, boron carbide 6-10 part, carborundum 6-10 part, polyacrylamide 0.2-0.5 part, Colophonium 0.2-0.4 part, waterglass 1-2 part, polrvinyl chloride 0.5-1 part, vinyl bis-stearamides 0.1-0.2 part, Ludox 1-2 part, sodium carboxymethyl cellulose 0.5-1 part, hydrochloric acid 10-20 part, isopropanol 10-30 part, water 60-90 part.
A kind of porous ceramics composite heat-insulated material the most according to claim 1, it is characterized in that: be prepared from weight portion by following component: polycrystalline mullite fibre 20-25 part, nano silicon 6-9 part, cycloheptaamylose 5-6 part, methyl parahydroxybenzoate 0.15-0.25 part, boron carbide 7-9 part, carborundum 7-9 part, polyacrylamide 0.3-0.4 part, Colophonium 0.25-0.35 part, waterglass 1.2-1.8 part, polrvinyl chloride 0.6-0.9 part, vinyl bis-stearamides 0.11-0.17 part, Ludox 1.3-1.7 part, sodium carboxymethyl cellulose 0.6-0.9 part, hydrochloric acid 13-18 part, isopropanol 15-25 part, water 70-80 part.
3. the preparation method of a kind of porous ceramics composite heat-insulated material described in any one of claim 1 to 2, it is characterised in that: comprise the following steps:
Step 1: polycrystalline mullite fibre is cut into 1-3 mm length；
Step 2: by the polycrystalline mullite fibre cut and mixed in hydrochloric acid, rinse with clear water after stirring 3-5 minute with blender；
Step 3: 3 steps 2 of repetitive operation, washes away the fibrous nodules in fiber；
Step 4: add remaining ingredient, stir 2-3 hour under rotating speed 300-500r/min with blender；
Step 5: slurry is poured into and carries out 2-3 hour discharge moisture of compacting in mould under pressure 80-110KPa, obtain wet base；
Step 6: put in baking oven by wet base, is dried 10-12 hour at temperature 70-80 DEG C；
Step 7: put in Muffle furnace and be sintered, heating rate is that 2 DEG C/min is warming up to 500-600 DEG C, is incubated 2-3 hour, then rises to 1150-1300 DEG C with 5 DEG C/min of speed, is incubated 2-3 hour, cools down and get final product.
The preparation method of a kind of porous ceramics composite heat-insulated material the most according to claim 3, it is characterised in that: a length of 2 millimeters of polycrystalline mullite fibre in described step 1.
The preparation method of a kind of porous ceramics composite heat-insulated material the most according to claim 3, it is characterised in that: in described step 2, mixing time is 4 minutes.
The preparation method of a kind of porous ceramics composite heat-insulated material the most according to claim 3, it is characterised in that: described step 4 medium speed is 350-450r/min, and the time is 2.5 hours.
The preparation method of a kind of porous ceramics composite heat-insulated material the most according to claim 3, it is characterised in that: in described step 5, pressure is 90-100KPa, and the press time is 2.5 hours.
The preparation method of a kind of porous ceramics composite heat-insulated material the most according to claim 3, it is characterised in that: in described step 6, temperature is 75 DEG C, and drying time is 10.5-11.5 hour.
The preparation method of a kind of porous ceramics composite heat-insulated material the most according to claim 3, it is characterised in that: being warming up to 550 DEG C for the first time in described step 7, be incubated 2.5 hours, second time is warming up to 1200-1250 DEG C, and temperature retention time is 2.5 hours.
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