CN108610000A - A kind of preparation method of anti-shedding aeroge complex heat-preservation felt - Google Patents

A kind of preparation method of anti-shedding aeroge complex heat-preservation felt Download PDF

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CN108610000A
CN108610000A CN201810483382.6A CN201810483382A CN108610000A CN 108610000 A CN108610000 A CN 108610000A CN 201810483382 A CN201810483382 A CN 201810483382A CN 108610000 A CN108610000 A CN 108610000A
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aeroge
reaction kettle
preparation
weight
framework materials
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CN108610000B (en
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郑善
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Tianjin Longhua Ruibo Technology Co., Ltd
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郑善
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Abstract

The invention belongs to energy conservation and environmental protection field of material technology, more particularly to a kind of preparation method of building and the anti-shedding aeroge complex heat-preservation felt of industrial energy saving heat preservation, including aeroge wet gel solution, fibre framework materials, the aeroge wet gel solution, fibre framework materials weight ratio be 2~30:1；Preparation method is according to aeroge wet gel solution：Fibre framework materials=2~30:1 weight ratio immerses fibre framework materials in aeroge wet gel solution, makes fibre framework materials saturation absorption aeroge wet gel solution, up to insulation quilt after drying.The problem of that the present invention overcomes existing insulation quilts is of high cost, easy picking, the performance of product is more preferable, more environmentally-friendly.

Description

A kind of preparation method of anti-shedding aeroge complex heat-preservation felt
The application is the Chinese invention patent (applying date that number of patent application is 201710279127.5：04 month 2017 25 Day, patent name：A kind of anti-shedding aeroge complex heat-preservation felt and preparation method thereof) divisional application.
Technical field
The invention belongs to energy conservation and environmental protection field of material technology more particularly to a kind of building and industrial energy saving heat preservation anticreeps The preparation method of powder aeroge complex heat-preservation felt.
Background technology
With the high speed development of social economy, the problem of having become world wide increasingly in short supply of global energy, exploitation New energy improves existing energy utilization rate and the energy saving great attention for having caused various countries.China is that an energy is poor Lean country, therefore, reasonable energy utilization, the energy saving sustainable development to Chinese society have great importance.Using The environmentally friendly high efficiency heat insulation material of new technology, new process development is energy saving most effective most economical one of measure.
Aeroge is also known as blue smoke, is a kind of light porous amorphous inorganic nano material of structure-controllable, has continuous three Reticular structure is tieed up, porosity is up to 80%~99.8%, and bore hole size is 1~100nm, 200~1000m of high-specific surface area2/ G, 50~100kg/m of low-density variation range3, thermal coefficient is less than 0.016~0.022W/ (mK) under normal temperature and pressure, than quiet Only the thermal conductivity 0.026W/ (mK) of air is also low, is the minimum solid material of current thermal conductivity.
Currently, the external research for being engaged in aeroge and commercialized company and research institution be concentrated mainly on European and American areas and Japan；At home, 4~6 enterprises enter aerogel heat-insulating heat preservation industry in succession since 2012.And now industrial pipeline is normal Conventional insulation has rock wool, simple glass blanket, high aluminium silicate wool, polyurethane etc., and rock wool, high aluminium silicate wool, which exist, to be protected The big disadvantage of warm poor performance, the easy moisture absorption, installation thickness；There is the shortcomings that not tolerating high temperature in simple glass blanket；Polyurethane exists Non-refractory and inflammable disadvantage.A kind of excellent thermal insulation performance, hydrophobic, fireproof material can obtain the approval in market and be able to It promotes and applies.Therefore, it is very significant if aeroge can be applied on the insulation quilt in industry.But traditional gas Gel is expensive, while being attached to the airsetting rubber powder among aerogel heat-insulating insulation quilt and being easy to fall off, and airsetting rubber powder is easily de- Fall be the material deadly defect.First, picking can pollute, and can cause health hazards to constructor, simultaneously as its institute Vibrations when the industrial pipeline conveying material of heat preservation, can cause powder to be accumulated downwards, so that heat insulation effect declines.And it is not losing powder Reduce thermal coefficient between, airsetting gluing knot and aeroge it is hydrophobic between, there are heavy difficult point, aerogel heat-insulating felt does not lose powder Problem becomes for world-famous puzzle.Second, aeroge insulation quilt is with traditional supercritical drying process or with ethyl orthosilicate Silicon source etc., technical process is long, high equipment cost, causes product cost high, and therefore, how inexpensive industrialization is also that everybody is common The target of pursuit.
The Chinese invention patent application of Publication No. CN1749214A proposes a kind of preparation of aerogel heat-insulating composite material The composition of method, the aerogel composite includes mainly aerosil, infrared light screening agent, reinforcement fiber, system Preparation Method is the gelation after immersing fibrofelt or fiber in Ludox, most afterwards through supercritical drying by fabricated in situ technique Aerogel composite is made.Aerogel composite prepared by this method has preferable hydrophobicity and good thermal insulation, But manufacturing cost is higher, is easy to powder away, and technique has certain danger using supercritical drying, is only suitable for high-end applications, no Conducive to producing in enormous quantities and be commercialized.
The Chinese invention patent application of Publication No. CN102557577A provides a kind of aerosil composite wood The preparation of material and method, using ethyl orthosilicate as silicon source, the glass fibre or fiber cotton material of industrialized production as reinforcement, Obtained silicon dioxide silica aerogel composite material has high porosity, high-specific surface area, low-density, low-k and low-heat The characteristics such as conductance have good mouldability, but ethyl orthosilicate is toxic and expensive, and silicon alkoxide is suitble to work as silicon source Industry produces.
It is mixed with aerosil that the Chinese invention patent of Publication No. 103723995A discloses a kind of blanket of glass wool The method for closing felt, the invention are to prepare mineral wool using centrifugal injection technique, spray resinoid bond, while by silica Aeroge slurry is sprayed at blanket of glass wool surface, forms the composite material that blanket is superimposed with aeroge, its advantage is that prepare Composite material has excellent mechanical performance, good heat-insulating property and sound absorbing performance；The disadvantage is that the requirement to equipment is high, nothing Cost is increased in shape, the content of aeroge is larger in the aeroge combination mat in addition prepared so that the rigidity of combination mat is big soft Property it is insufficient, it is easier to powder away, limit its application in certain fields.
Invention content
In view of the technical drawbacks of the prior art, it is an object of the present invention to provide a kind of at low cost and anti-sheddings Aeroge complex heat-preservation felt preparation method.
The technical solution adopted in the present invention is：
A kind of anti-shedding aeroge complex heat-preservation felt, including aeroge wet gel solution, fibre framework materials, the airsetting Glue wet gel solution, fibre framework materials weight ratio be 2~30:1；
The aeroge wet gel solution includes aerogel precursor body, binder, and the additive amount of the binder is airsetting The 0.1~5% of glue presoma solid content；
The solid content of the aerogel precursor body is 5~35%, refers to the content of aeroge solid content in aerogel precursor body It is 5~35%；
The binder includes the silicon of the sodium metasilicate A of 10~65 parts by weight, 10~40 parts by weight in parts by weight Sour potassium, the water A of 30~90 parts by weight, the Ludox of 5~40 parts by weight, the aluminum phosphates of 1~15 parts by weight, 1~10 parts by weight The bentonite of coupling agent A, the coalescents of 1~15 parts by weight, 5~30 parts by weight.
Preferably, the coupling agent A is one or both of KH560, TM-12.
Preferably, the coalescents are the one or two of alcohol ester 12, butyl glycol ether.
Preferably, the fibre framework materials are fine using ceramic fiber blanket, polymer fiber felt, glass mat, plant Tie up one or more of felt or carbon fiber felt.
Preferably, the length of the fibre framework materials is 2~80m, and width is 0.8~1.5m, and thickness is 1~30mm, Density is 100~300kg/m3And it is homogeneous.
Preferably, water content≤70% of the Ludox, Ludox be nano level silica dioxide granule in water Dispersion liquid.
Specifically, the preparation method of the aerogel precursor body, includes the following steps：
(1) mixed solution of silicon source and solvent is prepared
The sodium metasilicate B for the number 3.0~4.0 that rubs is taken to be fitted into reaction kettle, the water B progress that 1~3 times of sodium metasilicate B mass is added is dilute It releases, reaction kettle obtains sodium silicate solution B with the speed stirring 30min of 80~200r/min through 200 mesh screens；
The aqueous solution of sodium metasilicate is commonly called as waterglass, it is made of the alkali metal and silica of different proportion, changes Formula is R2O·nSiO2, R in formula2O is alkali metal oxide, and n is the ratio of silica and alkali metal oxide molal quantity, The referred to as number that rubs of waterglass, the most commonly used is sodium silicate water glass Na2O·nSiO2；
(2) colloidal sol
It takes A sour, A acid metal salts is added in A acid and rare earth A hydrochlorates are added in a manner of spray to step after mixing Suddenly the sodium silicate solution B that (1) obtains；The material in reaction kettle is carried out with the speed of 1200~2000r/min while spray The pH value of quickly stirring, control sodium silicate solution B is 1.5~3.0, and it is 15~30 nanometers to control its average pore size, obtains colloidal sol, 60~120min of this step used time；
Preferably, in the step (2), A acid is sulfuric acid, hydrochloric acid, oxalic acid or nitric acid, and 6~15mol/L is adjusted to water D；
Preferably, in the step (2), A acid metal salts are A acid zirconates or A acid aluminium salts；
Preferably, in the step (2), rare earth A hydrochlorates are A acid cerium salt, A acid yttrium salt or A acid lanthanum salts；
A acid metal salts and rare earth A hydrochlorates are easy the moisture absorption, and metering can be caused inaccurate, so for its addition of accurate quantitative analysis Amount, in terms of oxide, the molar ratio of the two is 100 for A acid metal salts described in step (2) and rare earth A hydrochlorates：1~6；Step (2) The molar ratio 2~5 of silica in the oxide and sodium metasilicate B of middle A acid metal salts：100；For example, A acid metal salts are aluminum sulfate, In terms of its oxide, i.e., with the molar ratio of silica in aluminium oxide and sodium metasilicate B for 2~5：100；
(3) gel
Sodium hydroxide or ammonium hydroxide are taken, it is 10~11.5 that water C, which is added, and is diluted to pH value, is added in a manner of spray to reaction kettle In；The material in reaction kettle is quickly stirred with the speed of 1200~2000r/min while spray, when object in reaction kettle When the pH value of material is 4.5~5.5, spray is terminated, gel, 80~180min of this step used time are obtained；
(4) aging
3~10h of stirring is continued with the speed of 20~50r/min in reaction kettle, aging, control are carried out to the material in reaction kettle Material in reactor temperature processed is 35~50 DEG C；The mode that standing is usually used in the prior art carries out aging, takes 3~5 days, Gel can't be stirred, the reason is that the prior art needs to stand during generally believing aging, standing can Convenient for the structure growth of aeroge；
(5) solvent is replaced
It carries out continuing 60~180min of stirring in reaction kettle, while being added same with aging material in step (4) reaction kettle The displacement solvent of volume, to displace remaining moisture；The prior art worries that stirring can destroy its structure, will not generally replace When be stirred, stewing process can be taken, cause take it is longer；Preparation method provided by the invention is stirred when solvent is replaced 60~180min is mixed, can greatly shorten period of a permutation, there is no destroyed microstructure；
Preferably, the displacement solvent is one or more of mixtures of methanol, acetone, n-hexane or heptane.
(6) surface modification
It carries out continuing stirring in reaction kettle, while continuously adding and aging material same volume in step (4) reaction kettle Coupling agent B；By stirring 60~180min, obtain before being coated with displacement solvent and the silica aerogel of the rare earth toughening of coupling agent B Drive body, the aerogel precursor body as used in insulation quilt.
The coupling agent B that above-mentioned steps (6) surface modification is added cements out the water in silica aerogel micropore, coupling agent B It is filled into silica aerogel micropore, the stability of microcellular structure can be improved, improve the evenness of pore size；In addition, passing through After the coupling agent B different to addition is surface modified, silica aerogel hydrophobicity, hydrophilic sexual function can be adjusted.
Preferably, coupling agent B described in above-mentioned steps (6) is hexamethyldisilazane, bis- (trimethylsilyl) acetamides, first Oxygroup trimethyl silane, dimethoxydimethylsilane, phenyl triethoxysilane, phenyltrimethoxysila,e, vinyl three The one or more of methoxy silane, methyltriethoxysilane and methyl trimethoxy oxygroup alkane；
Preferably, the stirring described in above-mentioned steps (5) or step (6) is to be stirred in reaction kettle；
Preferably, the stirring provides for reaction kettle center and quickly forward stirs (high speed shear disk), reaction kettle center Periphery provide baffle plate to realize；
Preferably, the water A, water B, water C, water D are deionized water.
The aerogel precursor body is prepared using normal temperature and pressure technique productions, is a kind of the light porous non-of structure-controllable There is crystalline inorganic nano material continuous tridimensional network, porosity to be up to 80% or more, and average pore size is 20nm left The right side, specific surface area are more than 500m2/ g, density are less than 70kg/m3, and thermal coefficient is less than 0.020W/ (mK) under normal temperature and pressure, than The thermal conductivity 0.022W/ (mK) of still air is also low, be at present rare low cost, industrialization, low heat conductivity solid material Material.
A kind of preparation method of anti-shedding aeroge complex heat-preservation felt, includes the following steps：
(1) it is aerogel precursor body prepared by 5~35%, normal temperature and pressure to take solid content；
(2) binder is prepared with gravimetric method：
1. taking 10~65 parts by weight of sodium metasilicate A, 10~40 parts by weight of potassium silicate, the bentonite of 5~30 parts by weight, water A It is stirred evenly after the mixing of 30~90 parts by weight, speed of agitator is 20~500r/min, and the stirring used time is 5~30min；
2. be added 5~40 parts by weight of Ludox, stir evenly, speed of agitator be 20~500r/min, stirring the used time be 5~ 30min；
3. 1~15 parts by weight of aluminum phosphate are added, stir evenly, speed of agitator is 20~500r/min, and the stirring used time is 10 ~30min adjusts pH value to 7-8；
4. adding 1~15 parts by weight of 1~10 parts by weight of coupling agent A and coalescents, speed of agitator is 20~500r/ Min, stirring used time are 5~30min, and 10~40min, system is sanded with the speed of 500~2700r/min with high speed dispersion sand mill It is standby go out finely dispersed binder；
(3) binder is added according to the 0.1~5% of aerogel precursor body solid content, then with blender with 500~1500r/ Min stirs the mixed solution that 10~50min is stirred evenly, and the mixed solution stirred evenly is recycled by horizontal sand mill 20~60min is ground with the rotating speed of 500~2500r/min, obtains molding aeroge wet gel solution；
(4) fibre framework materials are taken, according to aeroge wet gel solution：Fibre framework materials=2~30:1 weight ratio, Fibre framework materials are immersed in aeroge wet gel solution, fibre framework materials saturation absorption aeroge wet gel solution is made, Up to insulation quilt after drying.
Preferably, fibre framework materials immerse number >=2 time in aeroge wet gel solution, equal after the completion of dipping every time In 0.5~2Mpa/nm2Pressure under use compression roller extrusion process, extruding rate be 0.1~1.5m/min；The purpose is to make Aerogel precursor body is evenly distributed on insulation quilt.
Preferably, in the step (4), when fibre framework materials are dried, centralized collection recycles solution.
The present invention operation principle be：
Aeroge is also known as blue smoke, with following characteristic：1, several infinite more nano-pores are distributed in the inside of aeroge And air vent wall, air can not be flowed freely in nanometer stomata, be relatively adsorbed on air vent wall, aerogel material is in class Likelihood dummy status, effectively reduces convection current heat transfer, and heat is transmitted in solid material and can be transmitted along air vent wall；These air vent wall structures At the heat conduction path of infinite length, this will substantially reduce heat conduction；2, there are infinite more air vent wall, gas inside aeroge Hole wall is equivalent to infinite more thermal baffle, the reflection to light and heat may be implemented, to which radiant heat transfer be greatly lowered；3, gas Gel can effectively penetrate sunlight, and prevent the infrared emanation of environment temperature, become a kind of ideal transparent heat-insulated material, The thermal conductivity of material is set to substantially reduce；
Based on the characteristic of above-mentioned aeroge, suitable bonding agent is selected, by aeroge and industry, building heat preservation insulation quilt Making material combines, and can not only enhance industrial, building heat preservation insulation quilt mechanical strength, additionally it is possible to effectively reduce its heat conduction Coefficient improves its insulation ability, improves hydrophobic rate, improves the combination of industry and building heat preservation insulation quilt surface and material Ability.
Compared with traditional handicraft, the beneficial effects of the present invention are：
1, traditional aeroge complex heat-preservation felt have the shortcomings that it is of high cost, easily lose powder two big, seriously hinder this new The problem of application of material and development, that the present invention overcomes existing insulation quilts is of high cost, easy picking, the performance of product is more preferable, more Add environmental protection；
2, the aeroge in traditional aeroge insulation quilt is added in the form of aerogel powder, prepared by aerogel powder Drying process is had to pass through in the process, and drying process is to use supercritical drying process to complete at high temperature under high pressure, production Condition is harsh, complex process, dangerous big, and process units investment is big, and preparation efficiency is low, and raw material are with the silanol of high price It is main, it is of high cost；
Aeroge in aeroge insulation quilt of the present invention is added in the form of aerogel precursor body, is walked without being dried Suddenly, production cost is low；In addition, aerogel precursor body is to prepare at normal temperatures and pressures, and stabilization simple for process, safe, technique Process is down to 30h from 300h, and the process units investment of same production capacity is only the 1/20 of conventional method, and the prices of raw materials compare traditional silicon Low 100 times of source or more, product cost are only the 1/10 of conventional method；
3, there are three aspects for the reason of traditional aeroge insulation quilt easily loses powder：(1) use aerogel powder without Toughening processing, toughness is small, and particle is broken；(2) insulation quilt is not added with inorganic bond ingredient, and aerogel powder is combined with insulation quilt Dynamics is small；(3) due to being added in the form of aerogel powder in aeroge insulation quilt, aerogel powder is by single particle Body forms, and can not effectively link together between particle and particle, easily lose powder to cause insulation quilt；
Aeroge insulation quilt in the present invention has made improvement for above-mentioned picking reason：(1) aeroge insulation quilt uses Be aerogel precursor body, aerogel precursor body is is added to rare earth toughening airsetting prepared by rare earth A hydrochlorates and A acid metal salts Glue presoma, rare earth toughening aerogel precursor body toughness is big, and particle is non-breakable, and then is not easy to fall off from insulation quilt；(2) it protects It is added to inorganic binder in warm felt, aerogel precursor body is bonded together with fibrous material, aerogel precursor body and heat preservation Felt combination great efforts, inorganic binder are small on thermal coefficient influence, further decrease picking probability；(3) aerogel precursor body is The form of colloidal sol is not individual individual particles, and what is connected between component is even closer, and aerogel precursor body is squeezing into colloidal sol Single fibre composition is wrapped in the process, to achieve the purpose that be not easy to lose powder；
4, the three-dimensional structure of aeroge plays an important role during its performance plays, if in aeroge Hole is blocked by binder and can not just play a role；
The aeroge used in traditional aeroge insulation quilt is prepared at high temperature under high pressure, if the later stage is not specially treated, Porous three-dimensional space is easy to be blocked and failed by binder or other raw materials, and then it is made to lose heat insulation；In addition, The porous three-dimensional space of aeroge, which is united, can play better thermal insulation, can be incited somebody to action after being separated by binder Three-dimensional space inside aeroge isolates into isolated island, and then generates island effect, reduces the heat insulation of aeroge；
Containing displacement solvent in the aerogel precursor body prepared using method in the present invention, before displacement solvent occupies aeroge Drive porous three-dimensional space in vivo, binder or other raw materials can not invade it is porous in occupy its three-dimensional space, protect In warm felt drying process, displacement solvent volatilizees naturally, remains able to protect in aerogel precursor body after solvent volatilizees naturally Porous three-dimensional structure is held, overcomes failure and island effect caused by hole is blocked, therefore, heat-proof quality is stronger；
5, the anti-shedding aeroge complex heat-preservation felt of present invention gained, under normal temperature and pressure thermal coefficient be 0.018~ 0.022W/ (mK), picking degree is 5~20 ‰, in addition, the insulation quilt has super-hydrophobicity, fire resistance, is had soft well Toughness, flatness and intensity；
6, the preparation process of insulation quilt is simple, production operation is safe, at low cost, solves traditional aeroge insulation quilt industry Change the technologies such as the preparation process faced is complicated, the period is long, solvent-oil ratio is big, waste liquid is more, intensity is low, brittleness is big, flexibility is low Problem；
7, the insulation quilt preparation method in the present invention is the industrialization method produced suitable for aeroge complex heat-preservation felt, should Method under the premise of keeping properties of aerogels constant, by original production technology realize aeroge complex heat-preservation felt at Type shortens preparation time, greatly improves production efficiency；
8, the deionized water of wet concentration conductivity indices≤10 in the present invention reduces impurity and can save production cost；
9, organic binder is used in traditional insulation quilt, and volatile organic principle is contained in organic binder, it is organic Ingredient, which volatilizees, can reduce the performance of its insulation quilt；Organic binder is abandoned in the present invention, the binder used is inorganic bond Agent, there is no volatilization phenomenons, and the heat-insulating property of insulation quilt is more preferably；
10, fibre framework materials are immersed in aeroge wet gel solution in preparation process, make fiber reinforcement by the present invention The complete adsorbent solution of material；
11, fibre framework materials need, by repeatedly dipping, to adopt after dipping every time in aeroge wet gel solution With pressurized treatments, repeatedly dipping, repeatedly pressurization, make aerogel precursor body be evenly distributed on insulation quilt；
12, the pH value of all raw materials added in the present invention and insulation quilt felt body is close, and raw material is combined with aerogel blanket Effect is more preferable, further decreases picking probability；
13, when fibre framework materials immerse aeroge wet gel solution, centralized recovery solution saves production cost；
14, operation principle prepared by middle rare earth toughening aerogel precursor body of the present invention is：The preparation side of aerogel precursor body In method, the A acid metal salts and rare earth A hydrochlorates being added in gel process can reach toughening and improve silica aerogel heat resistance Effect；Aging and solvent swap step are carried out in the state of stirring, reaction efficiency are substantially increased, when having compressed technique Between, it is suitble to industrialization；
15, compared with prior art, advantage has following several middle rare earth toughening aerogel precursor preparation of the present invention Point：
(1) in recent years, there are some about the relevant report and patent for preparing silica aerogel under room temperature differential pressure in the prior art Document, but be to rest on laboratory preparatory phase mostly, technical process is longer, while process implementing narrow limits, it is difficult to real Existing large-scale industrialized production and application；The present invention provides the preparation methods under normal temperature and pressure, and it is relatively quiet to change the prior art Technique only applies in critical process process and stirs, speeded up to the hydrolysis, polycondensation and modification of aeroge, realized in 30h The technique of synthesis gas Gel Precursor provides a kind of method that industrial batch prepares rare earth toughening silica aerogel, is silicon gas A large amount of manufacture and use of gel provide premise；
(2) one of hinder the reason of aeroge development that be aeroge have reticular structure, but the structure in the prior art Edge it is relatively thin, more crisp, compression strength is low, and easy compression is caved in, and causes performance unstable；Present invention addition rare earth A hydrochlorates With A acid metal salts, the toughness of the material is improved, improves the intensity of silica aerogel；
(3) temperature in use of the silica aerogel of prior art preparation is relatively low, generally used below also relatively more steady at 500 DEG C Fixed, 500 DEG C or more the internal structure changes that can lead to silica aerogel cause thermal coefficient to decline；The present invention is sour with rare earth A is added Salt and A acid metal salts, improve the heat resistance of the material, improve the heat resisting temperature of silica aerogel.
Specific implementation mode
With reference to embodiment, the invention will be further described：
One, Examples 1 to 8
1, a kind of formula of anti-shedding aeroge complex heat-preservation felt, including aeroge wet gel solution, fibre framework materials, Aeroge wet gel solution, fibre framework materials weight ratio be 2~30:1；
Aeroge wet gel solution includes aerogel precursor body, binder, and the additive amount of binder is aerogel precursor body The 0.1~5% of solid content；
The solid content of aerogel precursor body be 5~35%, refer to aeroge solid content in aerogel precursor body content be 5~ 35%；
Binder, in parts by weight, including the potassium silicate of the sodium metasilicate A of 10~65 parts by weight, 10~40 parts by weight, The deionized water A of 30~90 parts by weight, the Ludox of 5~40 parts by weight, the aluminum phosphates of 1~15 parts by weight, 1~10 parts by weight The bentonite of coupling agent A, the coalescents of 1~15 parts by weight, 5~30 parts by weight；
The dosage detail of each component is shown in Table 1 in Examples 1 to 8, and the dosage detail of binder is shown in Table 2 in Examples 1 to 8.
The detailed list of usage of each component in 1 Examples 1 to 8 of table
In 2 Examples 1 to 8 of table in binder each component detailed list of usage
Wherein, coupling agent A is one or both of KH560, TM-12；Coalescents are alcohol ester 12, butyl glycol ether It is one or two kinds of；Fibre framework materials use ceramic fiber blanket, polymer fiber felt, glass mat, plant fiber felt or carbon One or more of fibrofelt；The length of fibre framework materials be 2~80m, width be 0.8~1.5m, thickness be 1~ 30mm, density are 100~300kg/m3And it is homogeneous；Water content≤70% of Ludox；The tool used in each embodiment Body type is shown in Table 3.
The parameter detail list of the coupling agent, fibre framework materials, Ludox that are used in 3 Examples 1 to 8 of table
2, a kind of preparation method of anti-shedding aeroge complex heat-preservation felt, includes the following steps：
(1) it is aerogel precursor body prepared by 5~35%, normal temperature and pressure to take solid content；
(2) binder is prepared with gravimetric method：
1. take 10~65 parts by weight of sodium metasilicate A, 10~40 parts by weight of potassium silicate, 5~30 parts by weight bentonite, go from It is stirred evenly after sub- 30~90 parts by weight of water A mixing, speed of agitator is 20~500r/min, and the stirring used time is 5~30min；
2. be added 5~40 parts by weight of Ludox, stir evenly, speed of agitator be 20~500r/min, stirring the used time be 5~ 30min；
3. 1~15 parts by weight of aluminum phosphate are added, stir evenly, speed of agitator is 20~500r/min, and the stirring used time is 10 ~30min adjusts pH value to 7-8；
4. adding 1~15 parts by weight of 1~10 parts by weight of coupling agent A and coalescents, speed of agitator is 20~500r/ Min, stirring used time are 5~30min, and 10~40min, system is sanded with the speed of 500~2700r/min with high speed dispersion sand mill It is standby go out finely dispersed binder；
(3) binder is added according to the 0.1~5% of aerogel precursor body solid content, then with blender with 500~1500r/ Min stirs the mixed solution that 10~50min is stirred evenly, and the mixed solution stirred evenly is recycled by horizontal sand mill 20~60min is ground with the rotating speed of 500~2500r/min, obtains molding aeroge wet gel solution；
(4) fibre framework materials are taken, according to aeroge wet gel solution：Fibre framework materials=2~30:1 weight ratio, Fibre framework materials are immersed in aeroge wet gel solution, fibre framework materials saturation absorption aeroge wet gel solution is made, Fibre framework materials immerse number >=2 time in aeroge wet gel solution, every time in 0.5~2Mpa/nm after the completion of dipping2 Pressure under use compression roller extrusion process, extruding rate be 0.1~1.5m/min, finally, using conventional method dry to get Insulation quilt；When fibre framework materials are dried, centralized collection recycles solution, the design parameter numerical value in each step of Examples 1 to 8 It is shown in Table 4.
The design parameter that each step of the preparation method of anti-shedding aeroge complex heat-preservation felt uses in 4 Examples 1 to 8 of table
3, the specific preparation process of the aerogel precursor body used in anti-shedding aeroge complex heat-preservation felt is as follows：
(1) mixed solution of silicon source and solvent is prepared
The waterglass B (being equivalent to sodium metasilicate B) for the number 3.0~4.0 that rubs is taken to be fitted into reaction kettle, addition waterglass B mass 1~ 3 times of deionized water B is diluted, and reaction kettle is obtained with the speed stirring 30min of 80~200r/min through 200 mesh screens Water glass solution B；
(2) colloidal sol
It takes A sour, A acid metal salts is added in A acid and rare earth A hydrochlorates are added in a manner of spray to step after mixing Suddenly the water glass solution B that (1) obtains；The material in reaction kettle is carried out with the speed of 1200~2000r/min while spray Quickly stirring, control ph to 1.5~3.0 stop spray, and spray time is controlled in 60~120min, obtains colloidal sol；
A acid is sulfuric acid, hydrochloric acid, oxalic acid or nitric acid, its concentration is adjusted to 6~15mol/L with deionized water D；
A acid metal salts are A acid zirconates or A acid aluminium salts, and rare earth A hydrochlorates are A acid cerium salt, A acid yttrium salt or A acid lanthanum salts；
In terms of oxide, the molar ratio of the two is 100 for A acid metal salts and rare earth A hydrochlorates：1~6；
The molar ratio 2~5 of silica in the oxide and water glass solution B of A acid metal salts：100；
(3) gel
Take sodium hydroxide or ammonium hydroxide, it is 10~11.5 that deionized water C, which is added, and is diluted to pH value, be added in a manner of spray to In step (2) reaction kettle in gained colloidal sol；While spray with the speed of 1200~2000r/min to the material in reaction kettle into Row quickly stirring sprays 80~180min of used time, obtains gel when the pH value of material in reactor is 4.5~5.5；
(4) aging
3~10h of stirring is continued with the speed of 20~50r/min in reaction kettle, aging, control are carried out to the material in reaction kettle Material in reactor temperature processed is 35~50 DEG C；
(5) solvent is replaced
The displacement solvent with aging material same volume in step (4) reaction kettle is added while stirring in reaction kettle, with Remaining moisture is displaced, 60~180min is stirred；
Displacement solvent is one or more of mixtures of methanol, acetone, n-hexane or heptane；
(6) surface modification
It carries out continuing stirring in reaction kettle, while continuously adding and aging material same volume in step (4) reaction kettle Coupling agent B obtains being coated with the rare earth toughening for replacing solvent and coupling agent B after surface modification by stirring 60~180min Silica aerogel presoma, as aerogel precursor body；
Stirring in step (5) or step (6) is that heart offer is quickly forward stirred in a kettle, reaction kettle center Periphery provides baffle plate；
Coupling agent B is hexamethyldisilazane, bis- (trimethylsilyl) acetamides, methoxytrimethylsilane, dimethoxy Dimethylsilane, phenyl triethoxysilane, phenyltrimethoxysila,e, vinyltrimethoxysilane, methyl triethoxy One or more of mixtures of silane and methyl trimethoxy oxygroup alkane；
The variable parameter of each embodiment and concrete numerical value are shown in Table 5 in the preparation method of aerogel precursor body.
The design parameter that step (1)~(6) use in the preparation method of aerogel precursor body in 5 Examples 1 to 8 of table
Two, performance test
(1) according to YB/T 4130-2005 Refractory Thermal Conductivities test method (water flow flat band method) to embodiment 1 The thermal coefficient of heat preservation felt product in~8 is detected；
(2) tensile strength of the heat preservation felt product in Examples 1 to 8 is detected according to JGJ144；
(3) aeroge content assaying method：Take 10mm thickness, 1m2Examples 1 to 8 in aeroge heat preservation felt type block and The heat preservation felt type block of an equal amount of not aerogel-congtg, is placed in drying box, and dry 1h removes moisture at 200 DEG C, weighs, gas The difference that gel keeps the temperature the heat preservation felt type block quality of felt type block and an equal amount of not aerogel-congtg is aeroge content；
(4) assay method of picking rate：Felt type block dry 1h at 200 DEG C will be first kept the temperature in Examples 1 to 8 removes water Point, insulation quilt finished product placement after drying is handled into 3min on the vibrating, the vibration frequency of vibrating screen is 120~150rad/s, Collect the powder that falls down, powder is crossed 200 mesh and weeded out except the impurity in powder, and aeroge is total in quality/insulation quilt of powder Content is picking rate；
(5) assay method of fire resistance：Insulation quilt finished product in Examples 1 to 8 is burnt into 10min under 1200 DEG C of flame, Observe the variation of insulation quilt；
(6) flexible assay method：180 ° of insulation quilt finished product doubling in Examples 1 to 8 is reinflated, and whether there is or not foldings for observation Trace；
(7) hydrophobic performance detection method：Water is poured in Examples 1 to 8 on insulation quilt upper surface, using contact angle Analyzer measures the size of its contact angle；
Using conventional vacuum felt as control group, specific testing result is shown in Table 6.
The performance test results of insulation quilt in 6 Examples 1 to 8 of table
By testing result in table 6 it is found that compared with conventional vacuum felt, the anti-shedding aeroge complex heat-preservation of present invention gained Felt, thermal coefficient is 0.018~0.022W/ (mK) under normal temperature and pressure, and thermal coefficient further decreases；Its tensile strength exists 0.06~0.08MPa, tensile property are obviously improved；10mm thickness, 1m2Aeroge content in insulation quilt is 160~220g, airsetting Glue content is substantially reduced；Picking rate is 5~20 ‰, and picking degree significantly reduces；In addition, its contact angle has reached 140~150 °, Super-hydrophobic rank is reached, hydrophobic performance is obviously improved；Fire resistance has reached A1 grades, and fire resistance is obviously improved；Doubling is countless Secondary, no folding line has extraordinary flexibility.
Three, application examples
By the products application in the present invention in the middle pressure steam part pipeline heat preservation in oil refining portion, depot siding is tested before being transformed Thermal insulation material uses rock wool, and thermal insulation material uses the product of the embodiment 3 in the present invention after transformation.
1, according to the regulation of GB8174-2008 " test and evaluation of equipment and pipe insulation effect ", pipeline external surface temperature Degree is different, and maximum allowable radiation loss is then different.Contrast standard, the maximum allowable radiation loss of this pipeline are 198w/m2；
2, detection before transformation：10 DEG C, wind speed 0.1m/s of environment temperature, when which uses rock wool heat-preservation material, Thickness is 200mm, and hull-skin temperature is at 35 DEG C or so, and according to calculating, which is 327w/m2, it is more than maximum The radiation loss 198w/m of permission2, pipeline long 1.5m, total radiation loss amount 1152w；
3, it is detected after being transformed：10 DEG C, wind speed 0.1m/s of environment temperature, using product in the present invention after transformation, thickness is 30mm, hull-skin temperature is at 32 DEG C or so, and according to calculating, the radiation loss of the pipeline is 281w/m2, it is more than maximum allowable dissipate Heat loss 198w/m2, pipeline long 1.5m, total radiation loss amount 543w；
4, after depot siding transformation compared with before transformation, insulation thickness is reduced to 30mm by 200mm, radiation loss by 327w/m2It is reduced to 281w/m2, total radiation loss amount is reduced to 543w, and uniformity of temperature profile by 1152w.
8 embodiments of the present invention are described in detail above, but the content is only the preferable implementation of the present invention Example should not be construed as limiting the practical range of the present invention.It is all according to all the changes and improvements made by the present patent application range Deng should all still fall within the scope of the patent of the present invention.

Claims (9)

1. a kind of preparation method of anti-shedding aeroge complex heat-preservation felt, which is characterized in that include the following steps：
（1）It is 5~35% aerogel precursor body to take solid content；
（2）Binder is prepared with gravimetric method：
1. take 10~65 parts by weight of sodium metasilicate A, 10~40 parts by weight of potassium silicate, the bentonite of 5~30 parts by weight, water A 30~ It is stirred evenly after the mixing of 90 parts by weight；
2. 5~40 parts by weight of Ludox are added, stir evenly；
3. 1~15 parts by weight of aluminum phosphate are added, stir evenly, adjusts pH value to 7-8；
4. adding 1~15 parts by weight of the parts by weight of coupling agent A1~10 and coalescents, stir evenly, then uses high speed dispersion sand Grinding machine is sanded, and prepares finely dispersed binder；
（3）Binder is added according to the 0.1~5% of aerogel precursor body solid content, is stirred evenly, obtained mixed solution passes through Sand mill circular grinding obtains molding aeroge wet gel solution；
（4）Fibre framework materials are taken, according to aeroge wet gel solution：Fibre framework materials=2~30:1 weight ratio, will be fine It ties up framework material to immerse in aeroge wet gel solution, makes fibre framework materials saturation absorption aeroge wet gel solution, it is dry Afterwards up to insulation quilt；
The preparation method of the aerogel precursor body, includes the following steps：
（1）Prepare the mixed solution of silicon source and solvent
The sodium metasilicate B for the number 3.0~4.0 that rubs is taken to be fitted into reaction kettle, the water B that 1~3 times of sodium metasilicate B mass is added is diluted, instead Kettle is answered to obtain sodium silicate solution B through 200 mesh screens with the speed stirring 30min of 80~200r/min；
（2）Colloidal sol
It takes A sour, A acid metal salts is added in A acid and rare earth A hydrochlorates are added in a manner of spray to step after mixing （1）Obtained sodium silicate solution B；The material in reaction kettle is carried out soon with the speed of 1200~2000r/min while spray The pH value of speed stirring, control sodium silicate solution B is 1.5~3.0, obtains colloidal sol；
Gel
Sodium hydroxide or ammonium hydroxide are taken, it is 10~11.5 that water C, which is added, and is diluted to pH value, is added into reaction kettle in a manner of spray； The material in reaction kettle is quickly stirred with the speed of 1200~2000r/min while spray, works as material in reactor PH value be 4.5~5.5 when, terminate spray, obtain gel；
（4）Aging
3~10h of stirring is continued with the speed of 20~50r/min in reaction kettle, aging is carried out to the material in reaction kettle, control is anti- It is 35~50 DEG C to answer material temperature in kettle；
（5）Solvent is replaced
It carries out continuing 60~180min of stirring, while addition and step in reaction kettle（4）Aging material same volume in reaction kettle Displacement solvent, to displace remaining moisture；
（6）Surface modification
It carries out continuing stirring in reaction kettle, while continuously adding and step（4）The coupling of aging material same volume in reaction kettle Agent B；By 60~180min of stirring, the silica aerogel presoma for being coated with displacement solvent and the rare earth toughening of coupling agent B is obtained, As aerogel precursor body.
2. very according to a kind of preparation method of anti-shedding aeroge complex heat-preservation felt described in claim 1, which is characterized in that including Aeroge wet gel solution, fibre framework materials, the aeroge wet gel solution, fibre framework materials weight ratio be 2~ 30:1。
3. a kind of preparation method of anti-shedding aeroge complex heat-preservation felt according to claim 1, which is characterized in that described Coupling agent A is one or both of KH560, TM-12.
4. a kind of preparation method of anti-shedding aeroge complex heat-preservation felt according to claim 1, which is characterized in that described Coalescents are the one or two of alcohol ester 12, butyl glycol ether.
5. a kind of preparation method of anti-shedding aeroge complex heat-preservation felt according to claim 1, which is characterized in that described Fibre framework materials use one in ceramic fiber blanket, polymer fiber felt, glass mat, plant fiber felt or carbon fiber felt Kind is several.
6. a kind of preparation method of anti-shedding aeroge complex heat-preservation felt according to claim 1, which is characterized in that described Water A, water B, water C are deionized water.
7. a kind of preparation method of anti-shedding aeroge complex heat-preservation felt according to claim 1, which is characterized in that step （6）Described in coupling agent B be hexamethyldisilazane, bis- (trimethylsilyl) acetamides, methoxytrimethylsilane, dimethoxy Base dimethylsilane, phenyl triethoxysilane, phenyltrimethoxysila,e, vinyltrimethoxysilane, three ethoxy of methyl The one or more of base silane and methyl trimethoxy oxygroup alkane.
8. a kind of preparation method of anti-shedding aeroge complex heat-preservation felt according to claim 1, which is characterized in that step （5）Or step（6）Described in stirring be stirred in reaction kettle.
9. a kind of preparation method of anti-shedding aeroge complex heat-preservation felt according to claim 1, which is characterized in that preferably Stirring provide for reaction kettle center and quickly forward stir（High speed shear disk）, the periphery at reaction kettle center provides baffle plate It realizes.
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