CN108658572B - Preparation method of anti-falling powder aerogel composite heat-preservation felt - Google Patents
Preparation method of anti-falling powder aerogel composite heat-preservation felt Download PDFInfo
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Abstract
The invention belongs to the technical field of energy-saving and environment-friendly materials, and particularly relates to a preparation method of an anti-loose powder aerogel composite heat-insulation felt for building and industrial energy-saving heat insulation, which comprises an aerogel wet gel solution and a fiber framework material, wherein the weight ratio of the aerogel wet gel solution to the fiber framework material is 2-30: 1; the preparation method comprises the following steps of according to the aerogel wet gel solution: and (3) soaking the fiber framework material into the aerogel wet gel solution according to the weight ratio of the fiber framework material = 2-30: 1, so that the fiber framework material is saturated and adsorbs the aerogel wet gel solution, and drying to obtain the heat preservation felt. The invention overcomes the problems of high cost and easy powder falling of the existing heat preservation felt, and the product has better performance and is more environment-friendly.
Description
The application is a divisional application of a Chinese invention patent with the patent application number of 201710279127.5 (application date: 2017, 25.04 and the name: an anti-loose powder aerogel composite heat-preservation felt and a preparation method thereof).
Technical Field
The invention belongs to the technical field of energy-saving and environment-friendly materials, and particularly relates to a preparation method of a powder-dropping-preventing aerogel composite heat-insulating felt for energy-saving and heat-insulating of buildings and industries.
Background
With the rapid development of social economy, the increasing shortage of global energy has become a worldwide problem, and the development of new energy, the improvement of the utilization rate of the existing energy and the energy conservation have attracted high attention of various countries. China is an energy-poor country, so that reasonable utilization of energy and energy conservation have important significance on sustainable development of China's society. The development of environment-friendly high-efficiency heat-insulating materials by adopting new technology and new process is one of the most effective and economic measures for saving energy.
The aerogel is also called blue smoke, is a light porous amorphous inorganic nano material with a controllable structure, has a continuous three-dimensional network structure, and has the porosity of 80-99.8 percent, the pore size of 1-100 nm, the high specific surface area of 200-1000 square meters per gram and the low density variation range of 50-100 kg/m3The thermal conductivity coefficient is less than 0.016-0.022W/(m.K) at normal temperature and normal pressure, is lower than the thermal conductivity of 0.026W/(m.K) of static air, and is the solid material with the lowest thermal conductivity at present.
Currently, companies and research institutes engaged in the research and commercialization of aerogels abroad are mainly focused on the european and american regions and japan; in China, 4-6 enterprises enter the aerogel heat insulation industry from 2012 onwards. The traditional heat-insulating materials commonly used for the existing industrial pipelines comprise rock wool, common glass wool felt, high-alumina silicate cotton, polyurethane and the like, and the rock wool and the high-alumina silicate cotton have the defects of poor heat-insulating property, easy moisture absorption and large installation thickness; the common glass wool felt has the defect of intolerance to high temperature; polyurethanes have the disadvantage of not being resistant to high temperatures and being flammable. A hydrophobic and fireproof material with excellent heat-insulating property can be accepted by the market and popularized and applied. Therefore, it would be of great interest if the aerogel could be used in insulation blankets in industry. However, the traditional aerogel is expensive, and aerogel powder attached to the aerogel heat insulation blanket is easy to fall off, which is a fatal weakness of the material. First, the powder falling can cause pollution and cause health damage to constructors, and meanwhile, due to vibration of the heat-insulated industrial pipeline during material conveying, powder can be accumulated downwards, so that the heat-insulation effect is reduced. The problems of no powder falling and low heat conductivity coefficient and the problems of aerogel adhesion and aerogel hydrophobicity are serious and difficult, and the problem of no powder falling of the aerogel heat insulation felt becomes a world problem. Secondly, the aerogel heat preservation felt is subjected to a traditional supercritical drying process or takes ethyl orthosilicate as a silicon source and the like, the process is long, the equipment cost is high, and the product cost is high, so that how to realize low-cost industrialization is a commonly pursued target.
The Chinese patent application with publication number CN1749214A proposes a preparation method of an aerogel heat insulation composite material, the composition of the aerogel composite material mainly comprises silicon dioxide aerogel, an infrared opacifier and reinforcement fibers, the preparation method is that a fiber felt or fibers are immersed into silica sol to be gelatinized through an in-situ synthesis process, and finally the aerogel composite material is prepared through supercritical drying. The aerogel composite material prepared by the method has good hydrophobicity and good heat insulation, but the preparation cost is high, powder is easy to fall off, and the supercritical drying adopted in the process has certain danger, is only suitable for high-end application and is not beneficial to mass production and commercialization.
The chinese patent application with publication number CN102557577A provides a preparation method of a silica aerogel composite material, in which tetraethoxysilane is used as a silicon source, and industrially produced glass fiber or cellucotton material is used as a reinforcement, and the prepared silica aerogel composite material has the characteristics of high porosity, high specific surface area, low density, low dielectric constant, low thermal conductivity and the like, and has good formability, but tetraethoxysilane is toxic and expensive, and silicon alkoxide is used as a silicon source and is suitable for industrial production.
The Chinese patent with publication number 103723995A discloses a method for preparing a mixed felt of glass wool felt and silicon dioxide aerogel, which comprises the steps of preparing glass wool by a centrifugal blowing process, spraying a resin binder, and spraying silicon dioxide aerogel slurry on the surface of the glass wool felt to form a composite material formed by overlapping the glass wool felt and the aerogel, wherein the composite material has the advantages of excellent mechanical property, good heat insulation property and sound absorption property; the method has the disadvantages of high requirement on equipment and invisibly increased cost, and the prepared aerogel mixed felt has high aerogel content, so that the mixed felt has high rigidity and insufficient flexibility, is easy to fall powder and limits the application of the aerogel mixed felt in certain fields.
Disclosure of Invention
The invention aims to provide a preparation method of an aerogel composite heat preservation felt which is low in cost and prevents powder shedding, aiming at the technical defects in the prior art.
The technical scheme adopted by the invention is as follows:
the anti-falling powder aerogel composite heat preservation felt comprises an aerogel wet gel solution and a fiber framework material, wherein the weight ratio of the aerogel wet gel solution to the fiber framework material is 2-30: 1;
the aerogel wet gel solution comprises an aerogel precursor and a binder, wherein the addition amount of the binder is 0.1-5% of the solid content of the aerogel precursor;
the solid content of the aerogel precursor is 5-35%, which means that the content of the aerogel solid in the aerogel precursor is 5-35%;
the binder comprises, by weight, 10-65 parts of sodium silicate A, 10-40 parts of potassium silicate, 30-90 parts of water A, 5-40 parts of silica sol, 1-15 parts of aluminum phosphate, 1-10 parts of coupling agent A, 1-15 parts of film forming aid and 5-30 parts of bentonite.
Preferably, the coupling agent A is one or two of KH560 and TM-12.
Preferably, the film forming auxiliary agent is one or two of alcohol ester 12 and ethylene glycol butyl ether.
Preferably, the fiber framework material is one or more of a ceramic fiber felt, a polymer fiber felt, a glass fiber felt, a plant fiber felt or a carbon fiber felt.
Preferably, the length of the fiber framework material is 2-80 m, the width is 0.8-1.5 m, the thickness is 1-30 mm, and the density is 100-300 kg/m3And the texture was uniform.
Preferably, the water content of the silica sol is less than or equal to 70%, and the silica sol is a dispersion of nano-scale silica particles in water.
Specifically, the preparation method of the aerogel precursor comprises the following steps:
(1) preparation of a mixed solution of a silicon source and a solvent
Putting 3.0-4.0 mol of sodium silicate B into a reaction kettle, adding water B which is 1-3 times of the mass of the sodium silicate B for dilution, stirring the reaction kettle at the speed of 80-200 r/min for 30min, and filtering the solution through a 200-mesh sieve to obtain a sodium silicate solution B;
the aqueous solution of sodium silicate is commonly called water glass, which is composed of alkali metal and silicon dioxide in different proportions and has the chemical formula R2O·nSiO2In the formula, R2O is an alkali metal oxide, n is the ratio of the number of moles of silica to the number of moles of alkali metal oxide, called the number of moles of water glass, most commonly sodium silicate waterglass Na2O·nSiO2；
(2) Sol gel
Taking acid A, adding metal salt A and rare earth acid salt A into the acid A, uniformly mixing, and adding into the sodium silicate solution B obtained in the step (1) in a spraying manner; rapidly stirring the materials in the reaction kettle at the speed of 1200-2000 r/min while spraying, controlling the pH value of the sodium silicate solution B to be 1.5-3.0, and controlling the average pore diameter to be 15-30 nanometers to obtain sol, wherein the time of the step is 60-120 min;
preferably, in the step (2), the acid A is sulfuric acid, hydrochloric acid, oxalic acid or nitric acid, and is adjusted to be 6-15mol/L by using water D;
preferably, in the step (2), the metal salt A is zirconium A acid salt or aluminum A acid salt;
preferably, in the step (2), the rare earth A acid salt is cerium A acid salt, yttrium A acid salt or lanthanum A acid salt;
the metal salt A and the rare earth A acid salt are easy to absorb moisture and cause inaccurate metering, so in order to accurately quantify the addition amount of the metal salt A and the rare earth A acid salt, the mole ratio of the metal salt A and the rare earth A acid salt in step (2) is 100: 1-6; in the step (2), the mole ratio of the oxide of the metal salt A to the silicon oxide in the sodium silicate B is 2-5: 100, respectively; for example, the metal salt A is aluminum sulfate, and calculated by oxides thereof, namely, the molar ratio of the aluminum oxide to the silicon oxide in the sodium silicate B is 2-5: 100, respectively;
(3) gel
Taking sodium hydroxide or ammonia water, adding water C to dilute until the pH value is 10-11.5, and adding the mixture into a reaction kettle in a spraying manner; rapidly stirring the materials in the reaction kettle at the speed of 1200-2000 r/min while spraying, stopping spraying when the pH value of the materials in the reaction kettle is 4.5-5.5, and obtaining gel, wherein the time of the step is 80-180 min;
(4) aging of
Continuously stirring the mixture in the reaction kettle at a speed of 20-50 r/min for 3-10 hours, aging the material in the reaction kettle, and controlling the temperature of the material in the reaction kettle to be 35-50 ℃; in the prior art, the aging is generally carried out in a standing mode, the time is consumed for 3-5 days, and the gel is not stirred, because the aging process is generally considered to be required to be carried out in the prior art, and the structural growth of the aerogel can be facilitated by standing;
(5) solvent replacement
Continuously stirring in the reaction kettle for 60-180 min, and simultaneously adding a displacement solvent with the same volume as the aged material in the reaction kettle in the step (4) to displace the residual water; in the prior art, the structure of the stirring tank is damaged, the stirring tank cannot be used for stirring during replacement, and standing treatment is adopted, so that the consumed time is long; according to the preparation method provided by the invention, the solvent is stirred for 60-180 min during replacement, the replacement period can be greatly shortened, and the microstructure is not damaged;
preferably, the replacement solvent is one or a mixture of methanol, acetone, n-hexane or heptane.
(6) Surface modification
Continuously stirring in the reaction kettle, and simultaneously continuously adding the coupling agent B with the same volume as the aged material in the reaction kettle in the step (4); and stirring for 60-180 min to obtain the rare earth toughened silicon aerogel precursor coated with the replacement solvent and the coupling agent B, namely the aerogel precursor adopted in the heat-insulating felt.
The coupling agent B added in the surface modification step (6) replaces water in the silica aerogel micropores, and the coupling agent B is filled in the silica aerogel micropores, so that the stability of the micropore structure can be improved, and the average of the pore size can be improved; in addition, the hydrophobic and hydrophilic functions of the silica aerogel can be adjusted by adding different coupling agents B for surface modification.
Preferably, in the step (6), the coupling agent B is one or more of hexamethyldisilazane, bis (trimethylsilyl) acetamide, methoxytrimethylsilane, dimethoxydimethylsilane, phenyltriethoxysilane, phenyltrimethoxysilane, vinyltrimethoxysilane, methyltriethoxysilane and methyltrimethoxysilane;
preferably, the stirring in the step (5) or the step (6) is performed in a reaction kettle;
preferably, the stirring is realized by providing rapid forward stirring (a high-speed shearing disc) for the center of the reaction kettle and providing a baffle plate at the periphery of the center of the reaction kettle;
preferably, the water A, the water B, the water C and the water D are deionized water.
The aerogel precursor is produced and prepared by adopting a normal-temperature normal-pressure process, is a light porous amorphous inorganic nano material with a controllable structure, has a continuous three-dimensional net structure, has the porosity of more than 80 percent, the average pore diameter of about 20nm, the specific surface area of more than 500 square meters per gram, the density of less than 70kg/m3, the heat conductivity coefficient of less than 0.020W/(m.K) at normal temperature and normal pressure and the heat conductivity of less than 0.022W/(m.K) of static air, and is a solid material with low cost, industrialization and low heat conductivity which is difficult to obtain at present.
A preparation method of the anti-falling powder aerogel composite heat preservation felt comprises the following steps:
(1) taking an aerogel precursor with solid content of 5-35% and prepared at normal temperature and normal pressure;
(2) preparing the binder by weight method:
mixing 10-65 parts by weight of sodium silicate A, 10-40 parts by weight of potassium silicate, 5-30 parts by weight of bentonite and 30-90 parts by weight of water A, and uniformly stirring at a stirring speed of 20-500 r/min for 5-30 min;
secondly, adding 5-40 parts by weight of silica sol, and stirring uniformly at a stirring speed of 20-500 r/min for 5-30 min;
thirdly, adding 1-15 parts by weight of aluminum phosphate, uniformly stirring at a stirring speed of 20-500 r/min for 10-30 min, and adjusting the pH value to 7-8;
adding 1-10 parts by weight of coupling agent A and 1-15 parts by weight of film forming additive, stirring at a speed of 20-500 r/min for 5-30 min, and sanding for 10-40 min at a speed of 500-2700 r/min by using a high-speed dispersion sand mill to prepare a uniformly dispersed binder;
(3) adding a binder according to 0.1-5% of the solid content of the aerogel precursor, stirring for 10-50 min at 500-1500 r/min by using a stirrer to obtain a uniformly stirred mixed solution, and circularly grinding the uniformly stirred mixed solution for 20-60 min at a rotating speed of 500-2500 r/min by using a horizontal sand mill to obtain a formed aerogel wet gel solution;
(4) taking a fiber framework material, and preparing a wet aerogel solution: and (3) soaking the fiber framework material into the aerogel wet gel solution according to the weight ratio of 2-30: 1, so that the fiber framework material is saturated and adsorbs the aerogel wet gel solution, and drying to obtain the heat preservation felt.
Preferably, the frequency of immersing the fiber framework material into the aerogel wet gel solution is more than or equal to 2 times, the fiber framework material is extruded by an extrusion roller under the pressure of 0.5-2 Mpa/n square meter after each immersion, and the extrusion speed is 0.1-1.5 m/min; the purpose is to uniformly distribute the aerogel precursor on the heat preservation felt.
Preferably, in the step (4), the recovery solution is collected intensively when the fibrous skeleton material is dried.
The working principle of the invention is as follows:
aerogels, also known as blue smoke, have the following properties: 1. the inside of the aerogel is distributed with a plurality of infinite nano holes and air hole walls, air can not flow freely in the nano holes and is relatively adsorbed on the air hole walls, the aerogel material is in a state similar to vacuum, convection heat transfer is effectively reduced, and heat can be transferred along the air hole walls when being transferred in the solid material; these porous walls constitute an infinitely long heat conduction path, which will significantly reduce heat conduction; 2. infinite air hole walls exist in the aerogel, and the air hole walls are equivalent to infinite heat insulation baffles, so that light and heat can be reflected, and radiation heat transfer is greatly reduced; 3. the aerogel can effectively penetrate through sunlight and prevent infrared heat radiation of the ambient temperature, and becomes an ideal transparent heat-insulating material, so that the heat conductivity of the material is greatly reduced;
based on the characteristics of the aerogel, a proper bonding agent is selected to bond the aerogel with the heat preservation felt manufacturing material for industrial and building heat preservation, so that the mechanical strength of the heat preservation felt for industrial and building heat preservation can be enhanced, the heat conductivity coefficient can be effectively reduced, the heat preservation and insulation capacity can be improved, the hydrophobic rate can be improved, and the bonding capacity between the surface of the heat preservation felt for industrial and building heat preservation and the material can be improved.
Compared with the traditional process, the invention has the beneficial effects that:
1. the traditional aerogel composite heat-insulating felt has the two defects of high cost and easy powder falling, the application and development of the new material are seriously hindered, the problems of high cost and easy powder falling of the existing heat-insulating felt are solved, the performance of the product is better, and the product is more environment-friendly;
2. aerogel in the traditional aerogel heat-insulating felt is added in the form of aerogel powder, the aerogel powder needs to be dried in the preparation process, the drying process is completed by adopting a supercritical drying process at high temperature and high pressure, the production conditions are harsh, the process is complex and dangerous, the investment of production devices is large, the preparation efficiency is low, the raw material mainly adopts high-price silanol, and the cost is high;
the aerogel in the aerogel heat-preservation felt is added in the form of an aerogel precursor, and the drying treatment step is not carried out, so that the production cost is low; in addition, the aerogel precursor is prepared at normal temperature and normal pressure, the process is simple and stable, the safety is high, the process is reduced from 300h to 30h, the investment of a production device with the same production capacity is only 1/20 of the traditional method, the price of raw materials is 100 times lower than that of the traditional silicon source, and the product cost is only 1/10 of the traditional method;
3. the traditional aerogel heat preservation felt is easy to fall off powder for three reasons: (1) the adopted aerogel powder is not subjected to toughening treatment, so that the toughness is low, and the particles are easy to break; (2) the thermal insulation felt is not added with inorganic bonding components, and the bonding strength of the aerogel powder and the thermal insulation felt is small; (3) the aerogel heat-preservation felt is added in the form of aerogel powder, the aerogel powder is composed of single particles, and the particles cannot be effectively connected together, so that the heat-preservation felt is easy to fall off;
the aerogel heat preservation felt of the invention is improved aiming at the powder dropping reason: (1) the aerogel heat preservation felt adopts an aerogel precursor, the aerogel precursor is a rare earth toughening aerogel precursor prepared by adding rare earth A acid salt and A metal salt, and the rare earth toughening aerogel precursor has high toughness, and particles are not easy to break and further not easy to fall off from the heat preservation felt; (2) the inorganic binder is added into the heat preservation felt to bond the aerogel precursor and the fiber material together, the bonding strength of the aerogel precursor and the heat preservation felt is high, the influence of the inorganic binder on the heat conductivity coefficient is small, and the powder falling probability is further reduced; (3) the aerogel precursor is in the form of sol and is not an independent particle individual, the components are connected more tightly, and the aerogel precursor wraps the single fiber component in the process of extruding into the sol, so that the aim of difficult powder falling is fulfilled;
4. the three-dimensional structure of the aerogel plays an important role in the performance exertion process, and the aerogel cannot play a role if the holes in the aerogel are blocked by the binding agent;
the aerogel adopted in the traditional aerogel heat preservation felt is prepared under high temperature and high pressure, and if special treatment is not carried out in the later period, the porous three-dimensional space is easily blocked by a binder or other raw materials to lose the heat insulation effect; in addition, the porous three-dimensional space of the aerogel is combined together to play a better heat insulation effect, and the three-dimensional space inside the aerogel can be cut into isolated islands after being separated by the adhesive, so that the isolated island effect is generated, and the heat insulation effect of the aerogel is reduced;
the aerogel precursor prepared by the method contains the replacement solvent, the replacement solvent occupies a porous three-dimensional space in the aerogel precursor, the binder or other raw materials cannot intrude into the pores to occupy the three-dimensional space, the replacement solvent naturally volatilizes in the drying process of the heat preservation felt, and the porous three-dimensional structure can still be kept in the aerogel precursor after the solvent naturally volatilizes, so that the failure and the island effect caused by the blockage of the pores are overcome, and the heat insulation performance is stronger;
5. the anti-dropping powder aerogel composite heat-insulating felt has the advantages that the heat conductivity coefficient is 0.018-0.022W/(m.K) at normal temperature and normal pressure, the powder dropping degree is 5-20 per mill, and the heat-insulating felt has super-hydrophobicity, fire resistance, good flexibility, flatness and strength;
6. the preparation process of the heat-insulating felt is simple, the production operation is safe, the cost is low, and the technical problems of complex preparation process, long period, large solvent consumption, more waste liquid, low strength, large brittleness, low flexibility and the like in the traditional aerogel heat-insulating felt industrialization are solved;
7. the preparation method of the heat preservation felt is an industrialized method suitable for the production of the aerogel composite heat preservation felt, and the method realizes the molding of the aerogel composite heat preservation felt through a unique production process on the premise of keeping the properties of the aerogel unchanged, thereby shortening the preparation time and greatly improving the production efficiency;
8. the deionized water with the conductivity index less than or equal to 10 is selected by water, so that impurities are reduced, and the production cost can be saved;
9. the traditional heat-insulating felt adopts an organic binder, the organic binder contains volatile organic components, and the performance of the heat-insulating felt is reduced due to volatilization of the organic components; in the invention, an organic binder is abandoned, and the adopted binder is an inorganic binder, so that the volatilization phenomenon does not exist, and the heat-insulating property of the heat-insulating felt is better;
10. in the preparation process, the fiber framework material is immersed in the aerogel wet gel solution, so that the fiber framework material completely adsorbs the solution;
11. the fiber framework material is subjected to multiple times of dipping in the aerogel wet gel solution, and after each time of dipping, the fiber framework material is subjected to pressurization treatment, and is subjected to multiple times of dipping and multiple times of pressurization, so that the aerogel precursor is uniformly distributed on the heat preservation felt;
12. the pH values of all the added raw materials and the heat preservation felt body are close, the combination effect of the raw materials and the aerogel felt is better, and the powder falling probability is further reduced;
13. when the fiber framework material is immersed in the aerogel wet gel solution, the solution is recovered in a centralized manner, so that the production cost is saved;
14. the working principle of the preparation of the rare earth toughening aerogel precursor is as follows: in the preparation method of the aerogel precursor, the metal salt A and the rare earth A acid salt are added in the gelling process, so that the effects of toughening and improving the heat resistance of the silica aerogel can be achieved; the aging and solvent replacement steps are carried out under the stirring state, so that the reaction efficiency is greatly improved, the process time is shortened, and the method is suitable for industrialization;
15. compared with the prior art, the preparation method of the rare earth toughening aerogel precursor has the following advantages:
(1) in recent years, some relevant reports and patent documents about preparation of silica aerogel under normal temperature and differential pressure exist in the prior art, but most of the reports and patent documents stay in a laboratory preparation stage, the process is long, and the process implementation range is too narrow, so that large-scale industrial production and application are difficult to realize; the invention provides a preparation method under normal temperature and normal pressure, which changes the relative static process in the prior art, applies stirring in the key process, accelerates the realization of the hydrolysis, polycondensation and modification of aerogel, realizes the process of synthesizing aerogel precursor within 30h, provides a method for industrially preparing rare earth toughening silicon aerogel in batches, and provides a premise for the mass production and use of silicon aerogel;
(2) one of the reasons for hindering the development of the aerogel in the prior art is that the aerogel has a net-shaped structure, but the structure has thin and fragile edges, low compressive strength and easy collapse under pressure, so that the performance is unstable; according to the invention, rare earth A acid salt and metal salt A are added, so that the toughness of the material is improved, and the strength of the silica aerogel is improved;
(3) the silica aerogel prepared by the prior art has low use temperature, is generally stable when used below 500 ℃, and can cause the internal structure change of the silica aerogel above 500 ℃ to reduce the heat conductivity coefficient; the rare earth A acid salt and the metal salt A are added, so that the temperature resistance of the material is improved, and the heat resistance temperature of the silica aerogel is increased.
Detailed Description
The invention is further illustrated by the following examples:
examples 1 to 8
1. The formula of the anti-falling powder aerogel composite heat-insulation felt comprises an aerogel wet gel solution and a fiber framework material, wherein the weight ratio of the aerogel wet gel solution to the fiber framework material is 2-30: 1;
the aerogel wet gel solution comprises an aerogel precursor and a binder, wherein the addition amount of the binder is 0.1-5% of the solid content of the aerogel precursor;
the solid content of the aerogel precursor is 5-35%, which means that the content of the aerogel solid in the aerogel precursor is 5-35%;
the adhesive comprises, by weight, 10-65 parts of sodium silicate A, 10-40 parts of potassium silicate, 30-90 parts of deionized water A, 5-40 parts of silica sol, 1-15 parts of aluminum phosphate, 1-10 parts of coupling agent A, 1-15 parts of film forming aid and 5-30 parts of bentonite;
the amounts of the components used in examples 1 to 8 are shown in Table 1, and the amounts of the binders used in examples 1 to 8 are shown in Table 2.
TABLE 1 detailed tables of the amounts of the components of examples 1-8
TABLE 2 dosage of each component of the binder in examples 1-8
Wherein the coupling agent A is one or two of KH560 and TM-12; the film forming auxiliary agent is one or two of alcohol ester 12 and ethylene glycol monobutyl ether; the fiber framework material is one or more of ceramic fiber felt, polymer fiber felt, glass fiber felt, plant fiber felt or carbon fiber felt; the fiber skeleton material has a length of 2 to 80m, a width of 0.8 to 1.5m, a thickness of 1 to 30mm, and a density of 100 to 300kg/m3And the texture is uniform; the water content of the silica sol is less than or equal to 70 percent; the specific species used in each example are shown in Table 3.
TABLE 3 detailed tables of parameters of the coupling agent, the fibrous skeleton material and the silica sol used in examples 1 to 8
2. A preparation method of the anti-falling powder aerogel composite heat preservation felt comprises the following steps:
(1) taking an aerogel precursor with solid content of 5-35% and prepared at normal temperature and normal pressure;
(2) preparing the binder by weight method:
mixing 10-65 parts by weight of sodium silicate A, 10-40 parts by weight of potassium silicate, 5-30 parts by weight of bentonite and 30-90 parts by weight of deionized water A, and uniformly stirring at a stirring speed of 20-500 r/min for 5-30 min;
secondly, adding 5-40 parts by weight of silica sol, and stirring uniformly at a stirring speed of 20-500 r/min for 5-30 min;
thirdly, adding 1-15 parts by weight of aluminum phosphate, uniformly stirring at a stirring speed of 20-500 r/min for 10-30 min, and adjusting the pH value to 7-8;
adding 1-10 parts by weight of coupling agent A and 1-15 parts by weight of film forming additive, stirring at a speed of 20-500 r/min for 5-30 min, and sanding for 10-40 min at a speed of 500-2700 r/min by using a high-speed dispersion sand mill to prepare a uniformly dispersed binder;
(3) adding a binder according to 0.1-5% of the solid content of the aerogel precursor, stirring for 10-50 min at 500-1500 r/min by using a stirrer to obtain a uniformly stirred mixed solution, and circularly grinding the uniformly stirred mixed solution for 20-60 min at a rotating speed of 500-2500 r/min by using a horizontal sand mill to obtain a formed aerogel wet gel solution;
(4) taking a fiber framework material, and preparing a wet aerogel solution: soaking a fiber framework material into an aerogel wet gel solution according to the weight ratio of 2-30: 1 to enable the fiber framework material to be in saturated adsorption on the aerogel wet gel solution, wherein the soaking times of the fiber framework material into the aerogel wet gel solution are more than or equal to 2 times, extruding the fiber framework material by using an extruding roller under the pressure of 0.5-2 Mpa/n square meter after each soaking is finished, the extruding speed is 0.1-1.5 m/min, and finally, drying by using a conventional method to obtain the heat preservation felt; when the fiber framework material is dried, the recovered solution is collected in a centralized manner, and the specific parameter values in each step of the examples 1-8 are shown in Table 4.
Table 4 concrete parameters adopted in each step of the preparation method of the anti-dusting aerogel composite insulation blanket in embodiments 1 to 8
3. The specific preparation steps of the aerogel precursor adopted in the anti-falling powder aerogel composite heat-insulation felt are as follows:
(1) preparation of a mixed solution of a silicon source and a solvent
Filling water glass B (equivalent to sodium silicate B) with the mole number of 3.0-4.0 into a reaction kettle, adding deionized water B with the mass of 1-3 times that of the water glass B for dilution, stirring the reaction kettle at the speed of 80-200 r/min for 30min, and filtering the mixture through a 200-mesh sieve to obtain a water glass solution B;
(2) sol gel
Taking acid A, adding metal salt A and rare earth acid salt A into the acid A, uniformly mixing, and adding the mixture into the water glass solution B obtained in the step (1) in a spraying manner; rapidly stirring the materials in the reaction kettle at the speed of 1200-2000 r/min while spraying, controlling the pH value to 1.5-3.0, stopping spraying, and controlling the spraying time to be 60-120 min to obtain sol;
the acid A is sulfuric acid, hydrochloric acid, oxalic acid or nitric acid, and the concentration of the acid A is adjusted to be 6-15mol/L by using deionized water D;
the A metal salt is A acid zirconium salt or A acid aluminum salt, and the rare earth A acid salt is A acid cerium salt, A acid yttrium salt or A acid lanthanum salt;
the molar ratio of the metal salt A to the rare earth A acid salt is 100: 1-6;
the molar ratio of the oxide of the metal salt A to the silicon oxide in the water glass solution B is 2-5: 100, respectively;
(3) gel
Taking sodium hydroxide or ammonia water, adding deionized water C to dilute until the pH value is 10-11.5, and adding the sodium hydroxide or ammonia water into the sol obtained in the reaction kettle in the step (2) in a spraying manner; rapidly stirring the materials in the reaction kettle at the speed of 1200-2000 r/min while spraying, and when the pH value of the materials in the reaction kettle is 4.5-5.5, spraying for 80-180 min to obtain gel;
(4) aging of
Continuously stirring the mixture in the reaction kettle at a speed of 20-50 r/min for 3-10 hours, aging the material in the reaction kettle, and controlling the temperature of the material in the reaction kettle to be 35-50 ℃;
(5) solvent replacement
Adding a displacement solvent with the same volume as the aged material in the reaction kettle in the step (4) while stirring in the reaction kettle to displace the residual water, and stirring for 60-180 min;
the replacement solvent is one or a mixture of methanol, acetone, n-hexane or heptane;
(6) surface modification
Continuously stirring in the reaction kettle, simultaneously continuously adding a coupling agent B with the same volume as the aged material in the reaction kettle in the step (4), stirring for 60-180 min, and performing surface modification to obtain a rare earth toughened silicon aerogel precursor coated with a replacement solvent and the coupling agent B, namely the aerogel precursor;
the stirring in the step (5) or the step (6) is to provide rapid forward stirring in the center of the reaction kettle, and baffle plates are provided at the periphery of the center of the reaction kettle;
the coupling agent B is one or a mixture of more of hexamethyldisilazane, bis (trimethylsilyl) acetamide, methoxytrimethylsilane, dimethoxydimethylsilane, phenyltriethoxysilane, phenyltrimethoxysilane, vinyltrimethoxysilane, methyltriethoxysilane and methyltrimethoxysilane;
the variable parameters and specific values for each example of the aerogel precursor preparation process are shown in table 5.
TABLE 5 specific parameters used in Steps (1) - (6) of the methods of preparation of aerogel precursors in examples 1-8
Second, performance test
(1) Detecting the heat conductivity coefficient of the heat-insulating felt products in the embodiments 1-8 according to a YB/T4130-2005 refractory material heat conductivity coefficient test method (a water flow flat plate method);
(2) detecting the tensile strength of the heat preservation felt products in the embodiments 1-8 according to JGJ 144;
(3) the aerogel content determination method comprises the following steps: taking a sample of 1m with a thickness of 10mm2Placing the aerogel heat preservation felt sample block and the heat preservation felt sample block without aerogel in the same size in a drying box, drying at 200 ℃ for 1h to remove moisture, weighing, and obtaining the mass difference value of the aerogel heat preservation felt sample block and the heat preservation felt sample block without aerogel in the same size as the aerogel content;
(4) the determination method of the powder falling rate comprises the following steps: drying the heat preservation felt sample block in the embodiment 1-8 at 200 ℃ for 1h to remove water, placing the dried heat preservation felt finished product on a vibrating screen for processing for 3min, wherein the vibrating frequency of the vibrating screen is 120-150 rad/s, collecting the dropped powder, and sieving the powder through a 200-mesh sieve to remove impurities in the powder, wherein the mass of the powder/the total content of aerogel in the heat preservation felt is the powder dropping rate;
(5) method for measuring fire resistance: burning the finished product of the heat preservation felt in the embodiment 1-8 for 10min under flame at 1200 ℃, and observing the change of the heat preservation felt;
(6) method for measuring flexibility: folding the finished products of the heat preservation felts in the embodiments 1-8 for 180 degrees, then unfolding, and observing whether folds exist;
(7) the hydrophobic property detection method comprises the following steps: pouring water on the upper surface of the heat preservation felt in the embodiment 1-8, and measuring the contact angle of the heat preservation felt by using a contact angle measuring instrument;
the specific test results of the traditional heat-insulating felt used as a control group are shown in Table 6.
Table 6 Performance test results of the insulation blankets in examples 1 to 8
From the results of the tests in Table 6Compared with the traditional heat-preservation felt, the anti-falling powder aerogel composite heat-preservation felt has the advantages that the heat conductivity coefficient is 0.018-0.022W/(m.K) at normal temperature and normal pressure, and the heat conductivity coefficient is further reduced; the tensile strength is 0.06-0.08 MPa, and the tensile property is obviously improved; 10mm thick, 1m2The aerogel content in the heat preservation felt is 160-220 g, and the aerogel content is obviously reduced; the powder dropping rate is 5-20 per mill, and the powder dropping degree is obviously reduced; in addition, the contact angle reaches 140-150 degrees, the super-hydrophobic grade is achieved, and the hydrophobic performance is obviously improved; the fire resistance reaches A1 grade, and the fire resistance is obviously improved; the folding is carried out for a plurality of times, and the non-crease fabric has good flexibility.
Third, application example
The product provided by the invention is applied to heat preservation of a medium-pressure steam part pipeline of an oil refining department, rock wool is adopted as a heat preservation material of a test section pipeline before transformation, and the product provided by the embodiment 3 in the invention is adopted as a heat preservation material after transformation.
1. According to the GB8174-2008 'test and evaluation of equipment and pipeline heat preservation effect', the temperature of the outer surface of the pipeline is different, and the maximum allowable heat dissipation loss is different. Compared with the standard, the maximum allowable heat dissipation loss of the pipeline is 198w/m2；
2. Detection before modification: the environmental temperature is 10 ℃, the wind speed is 0.1m/s, when the test section pipeline is made of rock wool heat-insulating material, the thickness is 200mm, the outer surface temperature is about 35 ℃, and according to calculation, the heat dissipation loss of the section pipeline is 327w/m2Over maximum allowable heat dissipation loss 198w/m2The length of the pipeline is 1.5m, and the total heat dissipation loss is 1152 w;
3. detection after modification: the environmental temperature is 10 ℃, the wind speed is 0.1m/s, the product of the invention is adopted after transformation, the thickness is 30mm, the temperature of the outer surface is about 32 ℃, and the heat dissipation loss of the pipeline is 281w/m according to calculation2Over maximum allowable heat dissipation loss 198w/m2The length of the pipeline is 1.5m, and the total heat dissipation loss is 543 w;
4. compared with the pipeline before modification, the modified pipeline has the advantages that the heat preservation thickness is reduced to 30mm from 200mm, and the heat dissipation loss is 327w/m2Reduced to 281w/m2The total heat dissipation loss is reduced from 1152w to 543w, and the temperature is highThe degree distribution is even.
Although the 8 embodiments of the present invention have been described in detail, the description is only for the preferred embodiments of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (9)
1. The preparation method of the anti-falling powder aerogel composite heat-insulation felt is characterized by comprising the following steps of:
(1) taking an aerogel precursor with solid content of 5-35%;
(2) preparing the binder by weight method:
mixing 10-65 parts by weight of sodium silicate A, 10-40 parts by weight of potassium silicate, 5-30 parts by weight of bentonite and 30-90 parts by weight of water A, and uniformly stirring;
adding 5-40 parts by weight of silica sol, and uniformly stirring;
thirdly, adding 1-15 parts by weight of aluminum phosphate, uniformly stirring, and adjusting the pH value to 7-8;
adding the coupling agent A1-10 parts by weight and the film-forming assistant 1-15 parts by weight, uniformly stirring, and sanding by using a high-speed dispersion sand mill to prepare a uniformly dispersed binder;
(3) adding a binder according to 0.1-5% of the solid content of the aerogel precursor, uniformly stirring, and circularly grinding the obtained mixed solution through a sand mill to obtain a formed aerogel wet gel solution;
(4) taking a fiber framework material, and preparing a wet aerogel solution: soaking the fiber framework material into the aerogel wet gel solution according to the weight ratio of the fiber framework material = 2-30: 1, so that the fiber framework material is saturated and adsorbs the aerogel wet gel solution, and drying to obtain the heat preservation felt;
the preparation method of the aerogel precursor comprises the following steps:
(1) preparation of a mixed solution of a silicon source and a solvent
Putting sodium silicate B with the modulus of 3.0-4.0 into a reaction kettle, adding water B with the mass of 1-3 times that of the sodium silicate B for dilution, stirring the reaction kettle at the speed of 80-200 r/min for 30min, and filtering the solution through a 200-mesh sieve to obtain a sodium silicate solution B;
(2) sol gel
Taking acid A, adding metal salt A and rare earth acid salt A into the acid A, uniformly mixing, and adding into the sodium silicate solution B obtained in the step (1) in a spraying manner; quickly stirring the materials in the reaction kettle at 1200-2000 r/min while spraying, and controlling the pH value of the sodium silicate solution B to be 1.5-3.0 to obtain sol; the acid A is sulfuric acid, hydrochloric acid, oxalic acid or nitric acid, and is adjusted to 6-15mol/L by deionized water; the metal salt A is zirconium salt A or aluminum salt A; the rare earth A acid salt is cerium salt A acid, yttrium salt A acid or lanthanum salt A acid;
(3) gel
Taking sodium hydroxide or ammonia water, adding water C to dilute until the pH value is 10-11.5, and adding the mixture into a reaction kettle in a spraying manner; rapidly stirring the materials in the reaction kettle at the speed of 1200-2000 r/min while spraying, and stopping spraying when the pH value of the materials in the reaction kettle is 4.5-5.5 to obtain gel;
(4) aging of
Continuously stirring the mixture in the reaction kettle at a speed of 20-50 r/min for 3-10 hours, aging the material in the reaction kettle, and controlling the temperature of the material in the reaction kettle to be 35-50 ℃;
(5) solvent replacement
Continuously stirring in the reaction kettle for 60-180 min, and simultaneously adding a displacement solvent with the same volume as the aged material in the reaction kettle in the step (4) to displace the residual water;
(6) surface modification
Continuously stirring in the reaction kettle, and simultaneously continuously adding the coupling agent B with the same volume as the aged material in the reaction kettle in the step (4); stirring for 60-180 min to obtain a rare earth toughened silicon aerogel precursor coated with a replacement solvent and a coupling agent B, namely the aerogel precursor;
the prepared anti-falling powder aerogel composite heat preservation felt comprises an aerogel wet gel solution and a fiber framework material, wherein the weight ratio of the aerogel wet gel solution to the fiber framework material is 2-30: 1;
the aerogel wet gel solution comprises an aerogel precursor and a binder, wherein the addition amount of the binder is 0.1-5% of the solid content of the aerogel precursor;
the binder comprises, by weight, 10-65 parts of sodium silicate A, 10-40 parts of potassium silicate, 30-90 parts of water A, 5-40 parts of silica sol, 1-15 parts of aluminum phosphate, 1-10 parts of coupling agent A, 1-15 parts of film forming aid and 5-30 parts of bentonite.
2. The preparation method of the anti-loose powder aerogel composite heat preservation felt according to claim 1, characterized in that in the step (4), the fiber framework material is immersed in the aerogel wet gel solution for more than or equal to 2 times, and is extruded by an extrusion roller under the pressure of 0.5-2 MPa after each immersion, and the extrusion rate is 0.1-1.5 m/min.
3. The preparation method of the anti-loosening aerogel composite heat-insulating felt according to claim 1, wherein the coupling agent A is one or two of KH560 and TM-12; the film-forming auxiliary agent is one or two of alcohol ester 12 and ethylene glycol monobutyl ether.
4. The preparation method of the anti-falling powder aerogel composite heat-preservation felt according to claim 1, wherein the fiber framework material is one or more of a ceramic fiber felt, a polymer fiber felt, a glass fiber felt, a plant fiber felt and a carbon fiber felt.
5. The preparation method of the anti-loosening aerogel composite heat-preservation felt according to claim 1, wherein the fiber framework material is 2-80 m long, 0.8-1.5 m wide, 1-30 mm thick and 100-300 kg/m thick for thin film cultivation.
6. The preparation method of the anti-loosening aerogel composite heat-preservation felt according to claim 1, wherein the water content of the silica sol is less than or equal to 70%.
7. The preparation method of the anti-loosening aerogel composite heat-preservation felt according to claim 1, wherein the water A, the water B and the water C are deionized water.
8. The method for preparing the anti-dusting aerogel composite heat-insulating felt according to claim 1, wherein the coupling agent B in the step (6) is one or more of hexamethyldisilazane, bis (trimethylsilyl) acetamide, methoxytrimethylsilane, dimethoxydimethylsilane, phenyltriethoxysilane, phenyltrimethoxysilane, vinyltrimethoxysilane, methyltriethoxysilane and methyltrimethoxysilane.
9. The preparation method of the anti-loosening aerogel composite heat-preservation felt according to claim 1, wherein the replacement solvent is one or a mixture of methanol, acetone, n-hexane or heptane.
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| CN108275886B (en) * | 2018-01-12 | 2020-11-17 | 江苏迈路达节能新材料科技有限公司 | Aerogel heat preservation felt prepared from industrial solid waste and preparation method |
| CN108611913B (en) * | 2018-03-30 | 2020-11-13 | 重庆纤维研究设计院股份有限公司 | Fireproof heat-insulating glass fiber material and preparation method thereof |
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| CN108658574A (en) | 2018-10-16 |
| CN107140938A (en) | 2017-09-08 |
| CN107140938B (en) | 2018-09-04 |
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| CN108658574B (en) | 2021-01-29 |
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