Summary of the invention
The technical problem that the present invention mainly solves: the high temperature insulation product strength made for current expanded vermiculite is low, yielding and fire performance is poor, because expanded vermiculite has larger structure hole, be mainly micron order, this makes its high temperature insulating, the problem that fire performance is also undesirable, provide the method that the modified expanded vermiculite of a kind of gel obtains high temperature insulation matrix material, the present invention carries out nanometer by the micron order hole of method to expanded vermiculite preparing gel modification, stable micropore and structure is formed between vermiculite layers, give vermiculite better thermostability, modified expanded vermiculite is to the refractoriness of matrix material, heat-proof quality and mechanical property are all improved, thus reach save energy, reduce the object of product cost.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
(1) vermiculite of 400 ~ 500g is got, putting it into mass concentration by solid-to-liquid ratio 1:2 is in the nitric acid of 0.6 ~ 0.8mol/L, immersion 2 ~ 3h is carried out at 60 ~ 70 DEG C, taking-up is filtered after immersion, put into retort furnace again, calcining 20 ~ 30min is carried out at the temperature of 500 ~ 550 DEG C, afterwards vermiculite is cooled to room temperature to take out, again the ethanolic soln that vermiculite puts into massfraction 80% by solid-to-liquid ratio 1:3 is soaked 2 ~ 3h, solid is filtered to obtain after immersion, put it into dry 2 ~ 3h in the baking oven of 60 ~ 70 DEG C, put into sand mill after drying and carry out sand milling, with 350 ~ 400 object screen cloth screenings, obtain vermiculite powder,
(2) according to the mass fraction, choose 20 ~ 25 parts of Resorcinols respectively, 40 ~ 50 parts of formaldehyde, 10 ~ 15 parts of propylene oxide, 15 ~ 20 parts of water join in there-necked flask, put into the water-bath of 60 ~ 70 DEG C, dissolve completely to solid by magnetic stirrer, put into afterwards in glass test tube, leave standstill 20 ~ 24h at normal temperatures, can colloidal sol be obtained;
(3) get 100 ~ 120g step (1) to obtain vermiculite powder and join in above-mentioned colloidal sol by solid-to-liquid ratio 1.1, put it into after mixing in water-bath, 22 ~ 24h is incubated under 50 ~ 55 DEG C of bath temperatures, make the aging one-tenth gel of colloidal sol, afterwards bath temperature is heated up 90 ~ 95 DEG C, continue aging 2 ~ 3 days, obtain the expanded vermiculite of gel modification;
(4) expanded vermiculite of above-mentioned obtained gel modification is first pressed the alcohol solution dipping 10 ~ 20h of solid-to-liquid ratio 1:3 massfraction 85%, take out afterwards and at 55 ~ 60 DEG C, soak 30 ~ 36h with the ethanolic soln of the tetraethoxy of solid-to-liquid ratio 1:4 again, soak and filter, filter residue is cleaned 1 ~ 3 time with distilled water and acetone respectively, after cleaning, puts into the dry 20 ~ 22h of thermostat container of 65 ~ 70 DEG C;
(5) above-mentioned dried solid is put in charring furnace, first it is vacuumized, be filled with nitrogen wherein again, in a nitrogen atmosphere, 250 ~ 300 DEG C are warming up to the heat-up rate of 2 ~ 4 DEG C/min, be incubated 1 ~ 2h at this temperature, naturally cool to room temperature afterwards, from charring furnace, take out solid;
(6) above-mentioned obtained solid is added water glass bonding agent by solid-to-liquid ratio 6:1, after abundant mixing, fast compound is poured in stainless mould, put into hydropress, in the pressure compression moulding of 0.2 ~ 0.3Mpa, then the sample suppressed is put into the dry 3 ~ 5h of loft drier of 100 ~ 110 DEG C, high temperature insulation matrix material can be obtained.
Application method of the present invention: high temperature insulation matrix material the present invention obtained can be applied in pipeline, stove and other Thermal Equipment, be applied in building material industry, can as a kind of New Building Materials, traditional mineral wool can be substituted, make house not only heat insulation but also warming, use it for Highrise buildings, then can replace general cladding glass, greatly alleviate buildings deadweight, and can fireproofing function be played, high temperature insulation matrix material of the present invention substitutes traditional lagging material, heat-energy losses can be greatly reduced, improve heat utilization rate, the high temperature of this goods ability 2000 DEG C, thermal conductivity under normal temperature is 0.01 ~ 0.03W/mk, thermal conductivity at 800 DEG C is 0.04 ~ 0.05W/mk, density is 380 ~ 420kg/m
3.
The invention has the beneficial effects as follows:
(1) the present invention carries out nanometer by the micron order hole of method to expanded vermiculite preparing gel modification, forms stable micropore and structure between vermiculite layers, gives vermiculite better thermostability;
(2) expanded vermiculite that the present invention is modified is all improved the refractoriness of matrix material, heat-proof quality and mechanical property, thus reaches save energy, reduces the object of product cost.
Embodiment
First the vermiculite of 400 ~ 500g is got, putting it into mass concentration by solid-to-liquid ratio 1:2 is in the nitric acid of 0.6 ~ 0.8mol/L, immersion 2 ~ 3h is carried out at 60 ~ 70 DEG C, taking-up is filtered after immersion, put into retort furnace again, calcining 20 ~ 30min is carried out at the temperature of 500 ~ 550 DEG C, afterwards vermiculite is cooled to room temperature to take out, again the ethanolic soln that vermiculite puts into massfraction 80% by solid-to-liquid ratio 1:3 is soaked 2 ~ 3h, solid is filtered to obtain after immersion, put it into dry 2 ~ 3h in the baking oven of 60 ~ 70 DEG C, put into sand mill after drying and carry out sand milling, with 350 ~ 400 object screen cloth screenings, obtain vermiculite powder, according to the mass fraction, choose 20 ~ 25 parts of Resorcinols respectively, 40 ~ 50 parts of formaldehyde, 10 ~ 15 parts of propylene oxide, 15 ~ 20 parts of water join in there-necked flask, put into the water-bath of 60 ~ 70 DEG C, dissolve completely to solid by magnetic stirrer, put into afterwards in glass test tube, leave standstill 20 ~ 24h at normal temperatures, can colloidal sol be obtained, get 100 ~ 120g to obtain vermiculite powder and join in above-mentioned colloidal sol by solid-to-liquid ratio 1.1, put it into after mixing in water-bath, 22 ~ 24h is incubated under 50 ~ 55 DEG C of bath temperatures, make the aging one-tenth gel of colloidal sol, afterwards bath temperature is heated up 90 ~ 95 DEG C, continue aging 2 ~ 3 days, obtain the expanded vermiculite of gel modification, by the expanded vermiculite of obtained gel modification first by the alcohol solution dipping 10 ~ 20h of solid-to-liquid ratio 1:3 with massfraction 85%, take out afterwards and at 55 ~ 60 DEG C, soak 30 ~ 36h with the ethanolic soln of the tetraethoxy of solid-to-liquid ratio 1:4 again, soak and filter, filter residue is cleaned 1 ~ 3 time with distilled water and acetone respectively, after cleaning, puts into the dry 20 ~ 22h of thermostat container of 65 ~ 70 DEG C, dried solid is put in charring furnace, first it is vacuumized, then be filled with nitrogen wherein, in a nitrogen atmosphere, be warming up to 250 ~ 300 DEG C with the heat-up rate of 2 ~ 4 DEG C/min, be incubated 1 ~ 2h at this temperature, naturally cool to room temperature afterwards, from charring furnace, take out solid, obtained solid is added water glass bonding agent by solid-to-liquid ratio 6:1, after abundant mixing, fast compound is poured in stainless mould, put into hydropress, in the pressure compression moulding of 0.2 ~ 0.3Mpa, then the sample suppressed is put into the dry 3 ~ 5h of loft drier of 100 ~ 110 DEG C, high temperature insulation matrix material can be obtained.
Example 1
First the vermiculite of 400g is got, putting it into mass concentration by solid-to-liquid ratio 1:2 is in the nitric acid of 0.6mol/L, immersion 2h is carried out at 60 DEG C, taking-up is filtered after immersion, put into retort furnace again, calcining 20min is carried out at the temperature of 500 DEG C, afterwards vermiculite is cooled to room temperature to take out, again the ethanolic soln that vermiculite puts into massfraction 80% by solid-to-liquid ratio 1:3 is soaked 2h, filter to obtain solid after immersion, put it into dry 2h in the baking oven of 60 DEG C, put into sand mill after drying and carry out sand milling, with 350 object screen cloth screenings, obtain vermiculite powder; According to the mass fraction, choose 20 parts of Resorcinols respectively, 50 parts of formaldehyde, 10 parts of propylene oxide, 20 parts of water join in there-necked flask, put into the water-bath of 60 DEG C, dissolve completely to solid by magnetic stirrer, put into afterwards in glass test tube, leave standstill 20h at normal temperatures, can colloidal sol be obtained; Get 100g to obtain vermiculite powder and join in above-mentioned colloidal sol by solid-to-liquid ratio 1.1, put it into after mixing in water-bath, under 50 DEG C of bath temperatures, be incubated 22h, make the aging one-tenth gel of colloidal sol, bath temperature is heated up 90 DEG C afterwards, continue aging 2 days, obtain the expanded vermiculite of gel modification; By the expanded vermiculite of obtained gel modification first by the alcohol solution dipping 10h of solid-to-liquid ratio 1:3 with massfraction 85%, take out afterwards and at 55 DEG C, soak 30h with the ethanolic soln of the tetraethoxy of solid-to-liquid ratio 1:4 again, soak and filter, filter residue is cleaned 1 time with distilled water and acetone respectively, after cleaning, puts into the dry 20h of thermostat container of 65 DEG C; Dried solid is put in charring furnace, first it is vacuumized, then be filled with nitrogen wherein, in a nitrogen atmosphere, be warming up to 250 DEG C with the heat-up rate of 2 DEG C/min, be incubated 1h at this temperature, naturally cool to room temperature afterwards, from charring furnace, take out solid; Obtained solid is added water glass bonding agent by solid-to-liquid ratio 6:1, after abundant mixing, fast compound is poured in stainless mould, put into hydropress, in the pressure compression moulding of 0.2Mpa, then the sample suppressed is put into the dry 3h of loft drier of 100 DEG C, high temperature insulation matrix material can be obtained.
High temperature insulation matrix material the present invention obtained can be applied in pipeline, stove and other Thermal Equipment, be applied in building material industry, can as a kind of New Building Materials, traditional mineral wool can be substituted, make house not only heat insulation but also warming, use it for Highrise buildings, then can replace general cladding glass, greatly alleviate buildings deadweight, and can fireproofing function be played, high temperature insulation matrix material of the present invention substitutes traditional lagging material, heat-energy losses can be greatly reduced, improve heat utilization rate, the high temperature of this goods ability 2000 DEG C, thermal conductivity under normal temperature is 0.01W/mk, thermal conductivity at 800 DEG C is 0.04W/mk, density is 380kg/m
3.
Example 2
First the vermiculite of 450g is got, putting it into mass concentration by solid-to-liquid ratio 1:2 is in the nitric acid of 0.7mol/L, immersion 2.5h is carried out at 65 DEG C, taking-up is filtered after immersion, put into retort furnace again, calcining 25min is carried out at the temperature of 525 DEG C, afterwards vermiculite is cooled to room temperature to take out, again the ethanolic soln that vermiculite puts into massfraction 80% by solid-to-liquid ratio 1:3 is soaked 2.5h, filter to obtain solid after immersion, put it into dry 2.5h in the baking oven of 65 DEG C, put into sand mill after drying and carry out sand milling, with 375 object screen cloth screenings, obtain vermiculite powder; According to the mass fraction, choose 23 parts of Resorcinols respectively, 47 parts of formaldehyde, 15 parts of propylene oxide, 15 parts of water join in there-necked flask, put into the water-bath of 65 DEG C, dissolve completely to solid by magnetic stirrer, put into afterwards in glass test tube, leave standstill 22h at normal temperatures, can colloidal sol be obtained; Get 110g to obtain vermiculite powder and join in above-mentioned colloidal sol by solid-to-liquid ratio 1.1, put it into after mixing in water-bath, under 53 DEG C of bath temperatures, be incubated 23h, make the aging one-tenth gel of colloidal sol, bath temperature is heated up 93 DEG C afterwards, continue aging 2.5 days, obtain the expanded vermiculite of gel modification; By the expanded vermiculite of obtained gel modification first by the alcohol solution dipping 15h of solid-to-liquid ratio 1:3 with massfraction 85%, take out afterwards and at 57 DEG C, soak 33h with the ethanolic soln of the tetraethoxy of solid-to-liquid ratio 1:4 again, soak and filter, filter residue is cleaned 2 times with distilled water and acetone respectively, after cleaning, puts into the dry 21h of thermostat container of 67 DEG C; Dried solid is put in charring furnace, first it is vacuumized, then be filled with nitrogen wherein, in a nitrogen atmosphere, be warming up to 275 DEG C with the heat-up rate of 3 DEG C/min, be incubated 1.5h at this temperature, naturally cool to room temperature afterwards, from charring furnace, take out solid; Obtained solid is added water glass bonding agent by solid-to-liquid ratio 6:1, after abundant mixing, fast compound is poured in stainless mould, put into hydropress, in the pressure compression moulding of 0.25Mpa, then the sample suppressed is put into the dry 4h of loft drier of 105 DEG C, high temperature insulation matrix material can be obtained.
High temperature insulation matrix material the present invention obtained can be applied in pipeline, stove and other Thermal Equipment, be applied in building material industry, can as a kind of New Building Materials, traditional mineral wool can be substituted, make house not only heat insulation but also warming, use it for Highrise buildings, then can replace general cladding glass, greatly alleviate buildings deadweight, and can fireproofing function be played, high temperature insulation matrix material of the present invention substitutes traditional lagging material, heat-energy losses can be greatly reduced, improve heat utilization rate, the high temperature of this goods ability 2000 DEG C, thermal conductivity under normal temperature is 0.02W/mk, thermal conductivity at 800 DEG C is 0.045W/mk, density is 400kg/m
3.
Example 3
First the vermiculite of 500g is got, putting it into mass concentration by solid-to-liquid ratio 1:2 is in the nitric acid of 0.8mol/L, immersion 3h is carried out at 70 DEG C, taking-up is filtered after immersion, put into retort furnace again, calcining 30min is carried out at the temperature of 550 DEG C, afterwards vermiculite is cooled to room temperature to take out, again the ethanolic soln that vermiculite puts into massfraction 80% by solid-to-liquid ratio 1:3 is soaked 3h, filter to obtain solid after immersion, put it into dry 3h in the baking oven of 70 DEG C, put into sand mill after drying and carry out sand milling, with 400 object screen cloth screenings, obtain vermiculite powder; According to the mass fraction, choose 25 parts of Resorcinols respectively, 40 parts of formaldehyde, 15 parts of propylene oxide, 20 parts of water join in there-necked flask, put into the water-bath of 70 DEG C, dissolve completely to solid by magnetic stirrer, put into afterwards in glass test tube, leave standstill 24h at normal temperatures, can colloidal sol be obtained; Get 120g to obtain vermiculite powder and join in above-mentioned colloidal sol by solid-to-liquid ratio 1.1, put it into after mixing in water-bath, under 55 DEG C of bath temperatures, be incubated 24h, make the aging one-tenth gel of colloidal sol, bath temperature is heated up 95 DEG C afterwards, continue aging 3 days, obtain the expanded vermiculite of gel modification; By the expanded vermiculite of obtained gel modification first by the alcohol solution dipping 20h of solid-to-liquid ratio 1:3 with massfraction 85%, take out afterwards and at 60 DEG C, soak 36h with the ethanolic soln of the tetraethoxy of solid-to-liquid ratio 1:4 again, soak and filter, filter residue is cleaned 3 times with distilled water and acetone respectively, after cleaning, puts into the dry 22h of thermostat container of 70 DEG C; Dried solid is put in charring furnace, first it is vacuumized, then be filled with nitrogen wherein, in a nitrogen atmosphere, be warming up to 300 DEG C with the heat-up rate of 4 DEG C/min, be incubated 2h at this temperature, naturally cool to room temperature afterwards, from charring furnace, take out solid; Obtained solid is added water glass bonding agent by solid-to-liquid ratio 6:1, after abundant mixing, fast compound is poured in stainless mould, put into hydropress, in the pressure compression moulding of 0.3Mpa, then the sample suppressed is put into the dry 5h of loft drier of 110 DEG C, high temperature insulation matrix material can be obtained.
High temperature insulation matrix material the present invention obtained can be applied in pipeline, stove and other Thermal Equipment, be applied in building material industry, can as a kind of New Building Materials, traditional mineral wool can be substituted, make house not only heat insulation but also warming, use it for Highrise buildings, then can replace general cladding glass, greatly alleviate buildings deadweight, and can fireproofing function be played, high temperature insulation matrix material of the present invention substitutes traditional lagging material, heat-energy losses can be greatly reduced, improve heat utilization rate, the high temperature of this goods ability 2000 DEG C, thermal conductivity under normal temperature is 0.03W/mk, thermal conductivity at 800 DEG C is 0.05W/mk, density is 420kg/m
3.