CN115196982A - Boiler lining heat-insulating material and preparation method thereof - Google Patents
Boiler lining heat-insulating material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a boiler lining heat-insulating material and a preparation method thereof, wherein the boiler lining heat-insulating material is prepared from the following raw materials in parts by weight: 35-55 parts of refractory clay tailings, 3-5 parts of nano boron fibers, 1-2 parts of glass fibers, 10-15 parts of aluminate cement, 2-4 parts of nano boron carbide, 1-3 parts of nano silicon nitride, 4-6 parts of fly ash floating beads, 5-7 parts of zirconium oxide, 3-5 parts of sodium silicate, 2-4 parts of a foaming agent, 10-15 parts of epoxy hyperbranched polysiloxane, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane/1, 4,5, 8-naphthalene tetracarboxylic anhydride polycondensate, 2-3 parts of benzidine disulfonic acid, 1-2 parts of phosphorus pentoxide, 0.1-0.3 part of polyphosphoric acid, 3-5 parts of a coupling agent, 1-2 parts of a non-ionic surfactant and 15-25 parts of water. The boiler lining thermal insulation material disclosed by the invention has the advantages of good performance stability and mechanical properties, good thermal insulation property, heat resistance and durability, and long service life.
Description
Technical Field
The invention relates to the technical field of chemical equipment materials, in particular to a boiler lining heat-insulating material and a preparation method thereof.
Background
In recent years, with the rapid development of economy and the progress of global industrialization, energy shortage and environmental problems are still serious. Energy conservation, emission reduction and sustainable development are still the common recognition in the industry. As a common energy conversion device, the operation of the boiler involves energy conversion, storage and transportation, and in these processes, the insulation problem is inevitably faced, and effective insulation of the boiler is performed, so that energy loss is reduced, and the necessary measures for improving the operation safety and economy are provided.
At present, common boiler heat-insulating materials comprise three types, namely inorganic heat-insulating materials, organic heat-insulating materials and composite heat-insulating materials, wherein the inorganic heat-insulating materials are seriously deformed when heated, have no good heat buffering effect and are poor in heat-insulating effect, and the organic heat-insulating materials have good heat-insulating effect but are poor in temperature resistance and are easy to age in the long-term use process. The existing composite heat-insulating material has poor performance stability due to the compatibility problem between inorganic components and organic components, and is easy to cause an external seepage phenomenon in the long-term use process, thereby seriously affecting the service life of the material. The boiler heat-insulating material on the market also has the technical problems of large heat conductivity coefficient, poor heat-insulating effect, harm to human health, further improvement of heat resistance and anti-aging capability and further prolongation of service life.
In order to solve the problems, patent CN104261746B discloses a boiler lining thermal insulation material and a preparation method thereof, wherein the thermal insulation material comprises the following components: phenolic resin, graphite, acrylamide, alumina, silicon dioxide, phthalic anhydride, aluminum chloride, calcium carbonate, cement powder, nitrile rubber, 2-acrylamido ethyl dimethyl ammonium chloride and water. The preparation method comprises the steps of stirring and mixing phenolic resin, acrylamide, aluminum chloride, calcium carbonate and nitrile rubber in a mixer, then adding the mixture into a reaction kettle, heating the mixture, adding 2-acrylamido ethyl dimethyl ammonium chloride, stirring the mixture for reaction under the protection of inert gas, and then naturally cooling the mixture to room temperature; then adding graphite, alumina, silicon dioxide, phthalic anhydride and cement powder into the mixture, crushing the mixture in a crusher, discharging the crushed mixture, adding water into the crushed mixture, stirring and mixing the mixture uniformly in a mixer at room temperature, and finally curing the mixture at 300-400 ℃ to obtain the boiler lining heat-insulating material. However, due to compatibility and matching problems between the components, the performance stability and mechanical properties of the insulation material are to be further improved, and the durability thereof is also to be further improved.
Therefore, the development of the boiler thermal insulation material with good performance stability, mechanical property, thermal insulation, heat resistance and durability and long service life and the preparation method thereof meet market demands, have wide market value and application prospect, and have very important significance for improving the operation safety and the economical efficiency of the boiler.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a boiler lining thermal insulation material with good performance stability and mechanical properties, good thermal insulation, heat resistance and durability, and long service life, and a preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: the boiler lining heat-insulating material comprises the following raw materials in parts by weight: 35-55 parts of refractory clay tailings, 3-5 parts of nano boron fibers, 1-2 parts of glass fibers, 10-15 parts of aluminate cement, 2-4 parts of nano boron carbide, 1-3 parts of nano silicon nitride, 4-6 parts of fly ash floating beads, 5-7 parts of zirconium oxide, 3-5 parts of sodium silicate, 2-4 parts of a foaming agent, 10-15 parts of epoxy hyperbranched polysiloxane, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane/1, 4,5, 8-naphthalene tetracarboxylic anhydride polycondensate, 2-3 parts of benzidine disulfonic acid, 1-2 parts of phosphorus pentoxide, 0.1-0.3 part of polyphosphoric acid, 3-5 parts of a coupling agent, 1-2 parts of a non-ionic surfactant and 15-25 parts of water.
Preferably, the nonionic surfactant is any one of nonylphenol polyoxyethylene ether and triton X-100.
Preferably, the coupling agent is at least one of a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH570.
Preferably, the method for producing the 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane/1, 4,5, 8-naphthalene tetracarboxylic anhydride polycondensate comprises the steps of: dissolving 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane in a high boiling point solvent to form a solution, cooling in an ice bath, slowly dripping a mixed solution of 1,4,5, 8-naphthalene tetracarboxylic anhydride and N-methylpyrrolidone in a constant pressure dropping funnel within 2-3h, reacting at normal temperature for 1-2h after finishing dripping, then dripping isoquinoline, reacting at 115-125 ℃ for 4-6h, then reacting at 185-195 ℃ for 15-20h, cooling to room temperature, precipitating in water, washing the precipitated polymer for 3-5 times with ethanol, and finally drying in a vacuum drying oven at 85-95 ℃ to constant weight.
Preferably, the high boiling point solvent is at least one of dimethyl sulfoxide and N, N-dimethylformamide; the inert gas is any one of nitrogen, helium, neon and argon.
Preferably, the molar ratio of the 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane, high boiling solvent, 1,4,5, 8-naphthalene tetracarboxylic anhydride, N-methylpyrrolidone, isoquinoline is 1 (3-5): 1 (4) (0.3-0.5).
Preferably, the source of the epoxy hyperbranched polyborosiloxane is not particularly required, and in one embodiment of the present invention, the epoxy hyperbranched polyborosiloxane is prepared according to the method of example 1 in patent CN 107868252B.
Preferably, the fly ash floating bead is a commercially available fly ash floating bead for a heat-insulating refractory material, and is coal-fired waste residue of a coal-fired thermal power plant; the fly ash floating bead comprises main chemical components of oxides of silicon and aluminum, wherein the silicon dioxide is 50-65%, the aluminum oxide is 25-35%, the diameter is 0.01-0.1mm, the inner core is in hollow vacuum, and the density is 420-720kg/m 3 。
Preferably, the blowing agent is at least one of a FA-1 blowing agent and a KC-20 blowing agent.
Preferably, the particle size of the nano boron carbide is 300-500nm; the granularity of the nano silicon nitride is 100-400nm; the granularity of the zirconia is 800-1200 meshes.
Preferably, the aluminate cement is pure calcium aluminate cement.
Preferably, the glass fiber has an average diameter of 3-9 μm and an aspect ratio (15-25): 1; the average diameter of the nano boron fiber is 200-500nm, and the length-diameter ratio is (10-20): 1.
Preferably, the refractory clay tailings are one or a combination of two or more of high alumina bauxite, flint clay, kaolinite, andalusite, kyanite or sillimanite.
Preferably, the particle size composition of the refractory clay tailings is as follows: 30-50 wt% for 3-10 meshes, 10-20 wt% for 10-15 meshes, 10-30 wt% for 18-150 meshes, and the balance being not less than 200 meshes.
The invention also aims to provide a preparation method of the boiler lining thermal insulation material, which comprises the following steps: mixing epoxy hyperbranched polyborosiloxane, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane/1, 4,5, 8-naphthalene tetracarboxylic anhydride polycondensate, benzidine disulfonic acid, phosphorus pentoxide and polyphosphoric acid, crushing, sieving by a 50-200-mesh sieve, uniformly mixing with other raw materials, adding into a mold, and curing and molding to obtain the boiler lining heat-insulating material.
Preferably, the curing and forming are carried out in two steps, wherein the temperature of the first step is 175-190 ℃, and the time is 1-2h; the second step is carried out at 250-335 deg.C for 150-200min.
Compared with the prior art, the invention has the beneficial effects that:
(1) The preparation method of the boiler lining heat-insulating material disclosed by the invention can be used after uniformly mixing all the raw materials and then curing at low temperature, does not need special equipment, can be used after curing and forming, and can be automatically sintered into a material with higher strength along with the rise of the boiler temperature; low energy consumption, high preparation efficiency and finished product qualification rate, convenient operation and control, safe and reliable construction engineering quality, simple construction operation and suitability for industrial production.
(2) The invention discloses a boiler lining heat-insulating material which is prepared from the following raw materials in parts by weight: 35-55 parts of refractory clay tailings, 3-5 parts of nano boron fibers, 1-2 parts of glass fibers, 10-15 parts of aluminate cement, 2-4 parts of nano boron carbide, 1-3 parts of nano silicon nitride, 4-6 parts of fly ash floating beads, 5-7 parts of zirconium oxide, 3-5 parts of sodium silicate, 2-4 parts of a foaming agent, 10-15 parts of epoxy hyperbranched polysiloxane, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane/1, 4,5, 8-naphthalene tetracarboxylic anhydride polycondensate, 2-3 parts of benzidine disulfonic acid, 1-2 parts of phosphorus pentoxide, 0.1-0.3 part of polyphosphoric acid, 3-5 parts of a coupling agent, 1-2 parts of a non-ionic surfactant and 15-25 parts of water; through the mutual cooperation and combined action of the raw materials, the prepared heat-insulating material is tightly combined with the base material, and has the advantages of good performance stability, good mechanical property, good heat-insulating property, heat resistance and durability and long service life.
(3) The boiler lining heat-insulating material disclosed by the invention has the advantages that the heat-insulating effect of a material product is remarkable, the internal structure density of the material is higher, and the mechanical strength and the heat resistance are more sufficient through the synergistic effect of inorganic raw materials such as refractory clay tailings, nano boron fibers, glass fibers, aluminate cement, nano boron carbide, nano silicon nitride, fly ash floating beads and zirconia. The fly ash floating beads belong to the recycling of solid wastes, the waste is changed into valuable, the resources are saved, the environmental protection problem is solved, meanwhile, the preparation cost of the material can be effectively reduced, and the material is endowed with better heat preservation and heat insulation performance.
(4) In the curing process of the boiler lining heat-insulating material disclosed by the invention, epoxy groups on epoxy hyperbranched polyborosiloxane can perform an epoxy ring-opening reaction with amino groups on benzidine disulfonic acid, sulfonic groups on the benzidine disulfonic acid can perform a chemical reaction with benzene rings on 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane/1, 4,5, 8-naphthalene tetracarboxylic anhydride polycondensate under the catalytic action of phosphorus pentoxide and polyphosphoric acid to form an interpenetrating network structure, other inorganic components can be better wrapped in the interpenetrating network, so that the connection among the components is tighter, and epoxy groups, amino groups and hydroxyl groups generated by the reaction on the organic raw materials can enhance the compatibility among the raw materials and the combination with the base materials.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the following detailed description will be made on the products of the present invention with reference to the examples.
The epoxy hyperbranched polyborosiloxane in each embodiment of the invention is prepared by the method of embodiment 1 in patent CN 107868252B; the fly ash floating bead is a commercially available fly ash floating bead for a heat-insulating refractory material and is coal-fired waste residue of a coal-fired thermal power plant; the fly ash floating bead comprises main chemical components of oxides of silicon and aluminum, wherein the silicon dioxide is 50-65%, the aluminum oxide is 25-35%, the diameter is 0.01-0.1mm, the inner core is in hollow vacuum,the density is 420-720kg/m 3 。
Example 1
The boiler lining thermal insulation material is prepared from the following raw materials in parts by weight: 35 parts of refractory clay tailings, 3 parts of nano boron fibers, 1 part of glass fibers, 10 parts of aluminate cement, 2 parts of nano boron carbide, 1 part of nano silicon nitride, 4 parts of fly ash floating beads, 5 parts of zirconia, 3 parts of sodium silicate, 2 parts of a foaming agent, 10 parts of epoxy hyperbranched polyborosiloxane, 1, 3-hexafluoropropane/1, 4,5, 8-naphthalene tetracarboxylic anhydride polycondensate, 3 parts of benzidine disulfonic acid, 1 part of phosphorus pentoxide, 0.1 part of polyphosphoric acid, 3 parts of a coupling agent, 1 part of a nonionic surfactant and 15 parts of water; the nonionic surfactant is nonylphenol polyoxyethylene ether; the coupling agent is a silane coupling agent KH550.
The 2, 2-bis [4- (4-aminophenoxy) phenyl group]-1, 3-hexafluoropropane/1, 4,5, 8-naphthalenetetracarboxylic anhydride polycondensate, comprising the steps of: 2, 2-bis [4- (4-aminophenoxy) phenyl]Dissolving 1, 3-hexafluoropropane in a high boiling point solvent to form a solution, cooling in an ice bath, slowly dripping a mixed solution of 1,4,5, 8-naphthalene tetracarboxylic anhydride and N-methylpyrrolidone into the mixed solution within 2 hours by using a constant pressure dropping funnel under the protection of inert gas, reacting for 1 hour at normal temperature after finishing dripping, dripping isoquinoline, reacting for 4 hours at 115 ℃, reacting for 15 hours at 185 ℃, cooling to room temperature, precipitating in water, washing the precipitated polymer for 3 times by using ethanol, and finally drying in a vacuum drying oven at 85 ℃ to constant weight; the high boiling point solvent is dimethyl sulfoxide; the inert gas is nitrogen; the 2, 2-bis [4- (4-aminophenoxy) phenyl group]-1, 3-hexafluoropropane, high boiling solvent, 1,4,5, 8-naphthalenetetracarboxylic anhydride, N-methylpyrrolidone, isoquinoline in a molar ratio of 1; m of the polycondensate was determined by GPC measurement n ＝18560g/mol，M W /M n ＝1.415；
The foaming agent is FA-1 foaming agent; the granularity of the nanometer boron carbide is 300nm; the granularity of the nano silicon nitride is 100nm; the granularity of the zirconia is 800 meshes; the aluminate cement is pure calcium aluminate cement; the glass fiber has an average diameter of 3 μm and an aspect ratio of 15; the average diameter of the nano boron fiber is 200nm, and the length-diameter ratio is 10; the refractory clay tailings are high bauxite; the particle size composition of the refractory clay tailings is as follows: 30wt% for 3-10 meshes, 10wt% for 10-15 meshes, 10wt% for 18-150 meshes, and the balance being not less than 200 meshes.
A preparation method of the boiler lining thermal insulation material comprises the following steps: mixing epoxy hyperbranched polyborosiloxane, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane/1, 4,5, 8-naphthalene tetracarboxylic anhydride polycondensate, benzidine disulfonic acid, phosphorus pentoxide and polyphosphoric acid, crushing and sieving by a 50-mesh sieve, then adding the mixture into a mould after uniformly mixing with other raw materials, and curing and molding to obtain the boiler lining heat-insulating material; the curing and molding are divided into two steps, wherein the temperature of the first step is 175 ℃, and the time is 1h; the temperature of the second step is 250 ℃ and the time is 150min.
Example 2
The boiler lining heat-insulating material comprises the following raw materials in parts by weight: 40 parts of refractory clay tailings, 3.5 parts of nano boron fibers, 1.2 parts of glass fibers, 11 parts of aluminate cement, 2.5 parts of nano boron carbide, 1.5 parts of nano silicon nitride, 4.5 parts of fly ash floating beads, 5.5 parts of zirconia, 3.5 parts of sodium silicate, 2.5 parts of a foaming agent, 11 parts of epoxy hyperbranched polyborosiloxane, 3.5 parts of 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane/1, 4,5, 8-naphthalene tetracarboxylic anhydride polycondensate, 2.2 parts of benzidine disulfonic acid, 1.2 parts of phosphorus pentoxide, 0.15 part of polyphosphoric acid, 3.5 parts of a coupling agent, 1.2 parts of a nonionic surfactant and 17 parts of water; the nonionic surfactant is triton X-100; the coupling agent is a silane coupling agent KH560.
The method for producing the 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane/1, 4,5, 8-naphthalenetetracarboxylic anhydride polycondensate, comprises the steps of: dissolving 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane in a high boiling point solvent to form a solution, cooling in an ice bath, slowly dripping a mixed solution of 1,4,5, 8-naphthalene tetracarboxylic anhydride and N-methylpyrrolidone in a constant pressure dropping funnel within 2.3h, reacting at normal temperature for 1.2h after finishing dripping, then dripping isoquinoline, reacting at 118 ℃ for 4.5h, then reacting at 187 ℃ for 17h, precipitating in water after cooling to room temperature, washing the precipitated polymer for 4 times with ethanol, and finally drying in a vacuum drying oven at 87 ℃ to constant weight.
The high boiling point solvent is N, N-dimethylformamide; the inert gas is helium; the molar ratio of the 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane, high boiling solvent, 1,4,5, 8-naphthalene tetracarboxylic anhydride, N-methylpyrrolidone, isoquinoline is 1; the foaming agent is KC-20 foaming agent.
The granularity of the nanometer boron carbide is 350nm; the granularity of the nano silicon nitride is 200nm; the granularity of the zirconia is 900 meshes; the aluminate cement is pure calcium aluminate cement; the glass fiber has an average diameter of 5 μm and an aspect ratio of 17; the average diameter of the nano boron fiber is 300nm, and the length-diameter ratio is 13; the refractory clay tailings are flint clay; the particle size composition of the refractory clay tailings is as follows: 35wt% for 3-10 meshes, 13wt% for 10-15 meshes, 15wt% for 18-150 meshes, and the balance being not less than 200 meshes.
A preparation method of the boiler lining thermal insulation material comprises the following steps: mixing epoxy hyperbranched polyborosiloxane, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane/1, 4,5, 8-naphthalene tetracarboxylic anhydride polycondensate, benzidine disulfonic acid, phosphorus pentoxide and polyphosphoric acid, crushing and sieving by a 100-mesh sieve, then adding the mixture into a mould after uniformly mixing with other raw materials, and curing and molding to obtain the boiler lining heat-insulating material; the curing and forming are divided into two steps, wherein the temperature of the first step is 180 ℃, and the time is 1.2h; the temperature of the second step was 275 ℃ for 165min.
Example 3
The boiler lining heat-insulating material comprises the following raw materials in parts by weight: 45 parts of refractory clay tailings, 4 parts of nano boron fibers, 1.5 parts of glass fibers, 13 parts of aluminate cement, 3 parts of nano boron carbide, 2 parts of nano silicon nitride, 5 parts of fly ash floating beads, 6 parts of zirconium oxide, 4 parts of sodium silicate, 3 parts of a foaming agent, 13 parts of epoxy hyperbranched polyborosiloxane, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane/1, 4,5, 8-naphthalene tetracarboxylic anhydride, 4 parts of a benzidine disulfonic acid polycondensate, 2.5 parts of phosphorus pentoxide, 0.2 part of polyphosphoric acid, 4 parts of a coupling agent, 1.5 parts of a nonionic surfactant and 20 parts of water; the nonionic surfactant is nonylphenol polyoxyethylene ether; the coupling agent is a silane coupling agent KH570.
A method for producing the 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane/1, 4,5, 8-naphthalene tetracarboxylic anhydride polycondensate, comprising the steps of: dissolving 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane in a high boiling point solvent to form a solution, cooling in an ice bath, slowly dripping a mixed solution of 1,4,5, 8-naphthalene tetracarboxylic anhydride and N-methylpyrrolidone in a constant pressure dropping funnel within 2.5h, reacting at normal temperature for 1.5h after finishing dripping, then dripping isoquinoline, reacting at 120 ℃ for 5h, then reacting at 190 ℃ for 18h, cooling to room temperature, precipitating in water, washing the precipitated polymer for 4 times with ethanol, and finally drying in a vacuum drying oven at 90 ℃ to constant weight.
The high boiling point solvent is dimethyl sulfoxide; the inert gas is neon; the molar ratio of the 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane, high boiling solvent, 1,4,5, 8-naphthalenetetracarboxylic anhydride, N-methylpyrrolidone, isoquinoline was 1.
The foaming agent is FA-1 foaming agent; the granularity of the nanometer boron carbide is 400nm; the granularity of the nano silicon nitride is 250nm; the granularity of the zirconia is 1000 meshes; the aluminate cement is pure calcium aluminate cement; the average diameter of the glass fiber is 6 μm, and the length-diameter ratio is 20; the average diameter of the nano boron fiber is 350nm, and the length-diameter ratio is 15; the refractory clay tailings are kaolinite; the particle size composition of the refractory clay tailings is as follows: 40wt% for 3-10 meshes, 15wt% for 10-15 meshes, 20wt% for 18-150 meshes, and the balance being not less than 200 meshes.
A preparation method of the boiler lining thermal insulation material comprises the following steps: mixing epoxy hyperbranched polyborosiloxane, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane/1, 4,5, 8-naphthalene tetracarboxylic anhydride polycondensate, benzidine disulfonic acid, phosphorus pentoxide and polyphosphoric acid, crushing and sieving by a 130-mesh sieve, then adding the mixture into a mould after uniformly mixing with other raw materials, and curing and molding to obtain the boiler lining heat-insulating material; the curing and forming are divided into two steps, the temperature of the first step is 183 ℃, and the time is 1.5h; the temperature of the second step is 305 ℃, and the time is 180min.
Example 4
The boiler lining thermal insulation material is prepared from the following raw materials in parts by weight: 52 parts of refractory clay tailings, 4.5 parts of nano boron fibers, 1.8 parts of glass fibers, 14 parts of aluminate cement, 3.5 parts of nano boron carbide, 2.5 parts of nano silicon nitride, 5.5 parts of fly ash floating beads, 6.5 parts of zirconium oxide, 4.5 parts of sodium silicate, 3.5 parts of a foaming agent, 14 parts of epoxy hyperbranched polyborosiloxane, 4.5 parts of 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane/1, 4,5, 8-naphthalene tetracarboxylic anhydride polycondensate, 2.8 parts of benzidine disulfonic acid, 1.8 parts of phosphorus pentoxide, 0.25 part of polyphosphoric acid, 4.5 parts of a coupling agent, 1.8 parts of a nonionic surfactant and 23 parts of water.
The nonionic surfactant is a mixture formed by mixing nonylphenol polyoxyethylene ether and triton X-100 according to a mass ratio of 3; the coupling agent is a mixture formed by mixing a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH570 in a mass ratio of 1.
The method for producing the 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane/1, 4,5, 8-naphthalenetetracarboxylic anhydride polycondensate, comprises the steps of: dissolving 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane in a high boiling point solvent to form a solution, cooling in an ice bath, slowly dripping a mixed solution of 1,4,5, 8-naphthalene tetracarboxylic anhydride and N-methylpyrrolidone in a constant pressure dropping funnel within 2.8h, reacting at normal temperature for 1.9h after finishing dripping, then dripping isoquinoline, reacting at 123 ℃ for 5.5h, then reacting at 193 ℃ for 19h, precipitating in water after cooling to room temperature, washing the precipitated polymer for 5 times with ethanol, and finally drying in a vacuum drying oven at 93 ℃ to constant weight.
The high boiling point solvent is a mixture formed by mixing dimethyl sulfoxide and N, N-dimethylformamide according to a mass ratio of 1; the inert gas is argon; the molar ratio of the 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane, high boiling solvent, 1,4,5, 8-naphthalene tetracarboxylic anhydride, N-methylpyrrolidone, isoquinoline was 1.
The foaming agent is a mixture formed by mixing FA-1 foaming agent and KC-20 foaming agent according to the mass ratio of 1; the granularity of the nanometer boron carbide is 480nm; the granularity of the nanometer silicon nitride is 350nm; the granularity of the zirconia is 1100 meshes; the aluminate cement is pure calcium aluminate cement.
The glass fiber has an average diameter of 8 μm and an aspect ratio of 23; the average diameter of the nano boron fiber is 450nm, and the length-diameter ratio is 18; the refractory clay tailings are a mixture formed by mixing high bauxite, flint clay, kaolinite, andalusite and kyanite according to a mass ratio of 3; the particle size composition of the refractory clay tailings is as follows: 45wt% of 3-10 meshes, 18wt% of 10-15 meshes, 25wt% of 18-150 meshes, and the balance being not less than 200 meshes.
A preparation method of the boiler lining thermal insulation material comprises the following steps: mixing epoxy hyperbranched polyborosiloxane, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane/1, 4,5, 8-naphthalene tetracarboxylic anhydride polycondensate, benzidine disulfonic acid, phosphorus pentoxide and polyphosphoric acid, crushing and sieving by a 180-mesh sieve, then adding the mixture into a mould after uniformly mixing with other raw materials, and curing and molding to obtain the boiler lining heat-insulating material; the curing and forming are divided into two steps, wherein the temperature of the first step is 187 ℃, and the time is 1.8h; the temperature of the second step is 325 ℃, and the time is 190min.
Example 5
The boiler lining heat-insulating material comprises the following raw materials in parts by weight: 55 parts of refractory clay tailings, 5 parts of nano boron fibers, 2 parts of glass fibers, 15 parts of aluminate cement, 4 parts of nano boron carbide, 3 parts of nano silicon nitride, 6 parts of fly ash floating beads, 7 parts of zirconia, 5 parts of sodium silicate, 4 parts of a foaming agent, 15 parts of epoxy hyperbranched polyborosiloxane, 1, 3-hexafluoropropane/1, 4,5, 8-naphthalene tetracarboxylic anhydride polycondensate, 5 parts of benzidine disulfonic acid, 2 parts of phosphorus pentoxide, 0.3 part of polyphosphoric acid, 5 parts of a coupling agent, 2 parts of a nonionic surfactant and 25 parts of water; the nonionic surfactant is nonylphenol polyoxyethylene ether; the coupling agent is a silane coupling agent KH560.
A method for producing the 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane/1, 4,5, 8-naphthalene tetracarboxylic anhydride polycondensate, comprising the steps of: dissolving 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane in a high boiling point solvent to form a solution, cooling in an ice bath, slowly dripping a mixed solution of 1,4,5, 8-naphthalene tetracarboxylic anhydride and N-methylpyrrolidone in a constant pressure dropping funnel within 3h, reacting at normal temperature for 2h after finishing dripping, dripping isoquinoline, reacting at 125 ℃ for 6h, reacting at 195 ℃ for 20h, cooling to room temperature, precipitating in water, washing the precipitated polymer for 5 times with ethanol, and finally drying in a vacuum drying oven at 95 ℃ to constant weight.
The high boiling point solvent is dimethyl sulfoxide; the inert gas is nitrogen; the molar ratio of the 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane, high boiling solvent, 1,4,5, 8-naphthalene tetracarboxylic anhydride, N-methylpyrrolidone, isoquinoline was 1.
The foaming agent is an FA-1 foaming agent; the granularity of the nano boron carbide is 500nm; the granularity of the nano silicon nitride is 400nm; the granularity of the zirconia is 1200 meshes; the aluminate cement is pure calcium aluminate cement; the glass fiber has an average diameter of 9 μm and an aspect ratio of 25; the average diameter of the nano boron fiber is 500nm, and the length-diameter ratio is 20; the refractory clay tailings are high bauxite; the particle size composition of the refractory clay tailings is as follows: 50wt% of 3-10 meshes, 20wt% of 10-15 meshes, 30wt% of 18-150 meshes and the balance of more than or equal to 200 meshes.
A preparation method of the boiler lining thermal insulation material comprises the following steps: mixing epoxy hyperbranched polyborosiloxane, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane/1, 4,5, 8-naphthalene tetracarboxylic anhydride polycondensate, benzidine disulfonic acid, phosphorus pentoxide and polyphosphoric acid, crushing, sieving with a 200-mesh sieve, uniformly mixing with other raw materials, adding into a mold, and curing and molding to obtain the boiler lining heat-insulating material; the curing and forming are divided into two steps, wherein the temperature of the first step is 190 ℃, and the time is 2 hours; the temperature of the second step is 335 ℃ and the time is 200min.
Comparative example 1
A boiler lining thermal insulation material, the formulation and preparation method of which are substantially the same as those of example 1, except that 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane/1, 4,5, 8-naphthalene tetracarboxylic anhydride polycondensate, nano boron carbide and fly ash floating beads are not added.
Comparative example 2
The formula and the preparation method of the boiler lining thermal insulation material are basically the same as those of the example 1, except that benzidine disulfonic acid, nano silicon nitride and a foaming agent are not added.
In order to further illustrate the unexpected positive technical effects obtained by the products of the embodiments of the invention, the boiler lining thermal insulation material prepared by the embodiments is subjected to related performance tests according to the current national standard or conventional method in China, and the test results are shown in Table 1.
As can be seen from Table 1, the boiler lining thermal insulation material disclosed in the embodiment of the invention has more excellent thermal insulation, neutral salt spray resistance and thermal shock stability compared with the comparative product; and the linear change rate is small, and the combined addition of 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane/1, 4,5, 8-naphthalene tetracarboxylic anhydride polycondensate, nano boron carbide, fly ash floating beads, benzidine disulfonic acid, nano silicon nitride and foaming agent is beneficial to improving the performances.
TABLE 1
The foregoing is illustrative of the preferred embodiments of the present invention, and is not to be construed as limiting the invention in any way; one of ordinary skill in the art can readily practice the present invention as described above; however, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention without departing from the scope of the invention; meanwhile, any changes, modifications, and evolutions of the equivalent changes of the above embodiments according to the actual techniques of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (10)
1. The boiler lining heat insulation material is characterized by comprising the following raw materials in parts by weight: 35-55 parts of refractory clay tailings, 3-5 parts of nano boron fibers, 1-2 parts of glass fibers, 10-15 parts of aluminate cement, 2-4 parts of nano boron carbide, 1-3 parts of nano silicon nitride, 4-6 parts of fly ash floating beads, 5-7 parts of zirconium oxide, 3-5 parts of sodium silicate, 2-4 parts of a foaming agent, 10-15 parts of epoxy hyperbranched polysiloxane, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane/1, 4,5, 8-naphthalene tetracarboxylic anhydride polycondensate, 2-3 parts of benzidine disulfonic acid, 1-2 parts of phosphorus pentoxide, 0.1-0.3 part of polyphosphoric acid, 3-5 parts of a coupling agent, 1-2 parts of a non-ionic surfactant and 15-25 parts of water.
2. The boiler lining thermal insulation material of claim 1, wherein the non-ionic surfactant is any one of nonylphenol polyoxyethylene ether and triton X-100; the coupling agent is at least one of a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH570.
3. The boiler lining insulation of claim 1, wherein said 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane/1, 4,5, 8-naphthalene tetracarboxylic anhydride polycondensate is prepared by a method comprising the steps of: dissolving 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane in a high boiling point solvent to form a solution, cooling in an ice bath, slowly dripping a mixed solution of 1,4,5, 8-naphthalene tetracarboxylic anhydride and N-methylpyrrolidone in a constant pressure dropping funnel within 2-3h, reacting at normal temperature for 1-2h after finishing dripping, then dripping isoquinoline, reacting at 115-125 ℃ for 4-6h, then reacting at 185-195 ℃ for 15-20h, cooling to room temperature, precipitating in water, washing the precipitated polymer for 3-5 times with ethanol, and finally drying in a vacuum drying oven at 85-95 ℃ to constant weight.
4. The boiler lining insulation of claim 3, wherein said high boiling point solvent is at least one of dimethylsulfoxide, N-dimethylformamide; the inert gas is any one of nitrogen, helium, neon and argon.
5. The boiler lining insulation material of claim 3, wherein the molar ratio of 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane, high boiling point solvent, 1,4,5, 8-naphthalene tetracarboxylic anhydride, N-methylpyrrolidone, and isoquinoline is 1 (3-5) to 1 (4) (0.3-0.5).
6. The boiler lining insulation of claim 1, wherein said blowing agent is at least one of FA-1 blowing agent, KC-20 blowing agent; the granularity of the nanometer boron carbide is 300-500nm; the granularity of the nano silicon nitride is 100-400nm; the granularity of the zirconia is 800-1200 meshes.
7. The boiler lining insulation of claim 1, wherein said aluminate cement is a pure calcium aluminate cement; the average diameter of the glass fiber is 3-9 μm, and the length-diameter ratio is (15-25): 1; the average diameter of the nano boron fiber is 200-500nm, and the length-diameter ratio is (10-20): 1.
8. The boiler lining insulation material of claim 1, wherein the refractory clay tailings are any one or a combination of two or more of bauxite, flint clay, kaolinite, andalusite, kyanite or sillimanite; the particle size composition of the refractory clay tailings is as follows: 30-50 wt% for 3-10 meshes, 10-20 wt% for 10-15 meshes, 10-30 wt% for 18-150 meshes, and the balance being not less than 200 meshes.
9. The method for preparing the boiler lining thermal insulation material according to any one of claims 1 to 8, comprising the steps of: mixing epoxy hyperbranched polyborosiloxane, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane/1, 4,5, 8-naphthalene tetracarboxylic anhydride polycondensate, benzidine disulfonic acid, phosphorus pentoxide and polyphosphoric acid, crushing, sieving by a 50-200-mesh sieve, uniformly mixing with other raw materials, adding into a mold, and curing and molding to obtain the boiler lining heat-insulating material.
10. The method for preparing the boiler lining thermal insulation material according to claim 9, wherein the curing and forming are carried out in two steps, the temperature in the first step is 175-190 ℃, and the time is 1-2 hours; the second step is carried out at 250-335 deg.C for 150-200min.
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