CN1287892C - Aluminium modified silica-gel adsorbent material and its preparing process - Google Patents
Aluminium modified silica-gel adsorbent material and its preparing process Download PDFInfo
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- CN1287892C CN1287892C CN 200410050867 CN200410050867A CN1287892C CN 1287892 C CN1287892 C CN 1287892C CN 200410050867 CN200410050867 CN 200410050867 CN 200410050867 A CN200410050867 A CN 200410050867A CN 1287892 C CN1287892 C CN 1287892C
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Abstract
The present invention discloses a preparing process of aluminium modified silica-gel adsorbent material, which comprises the following steps: (1), inorganic fiber paper is immersed in water glass at room temperature; after 2 to 5 hours, the inorganic fiber paper is taken out and dried for 10 to 24 hours; (2), soluble aluminum salt is prepared into water solution; dilute acid is added for adjusting a pH value from 0.5 to 2; the temperature is raised to 30 to 80 DEG C; under intense stir, the obtained solution is used for immersing the inorganic fiber paper; a coprecipitation reaction is generated on an inorganic fiber surface and a gap; the reaction is sufficiently carried out for 12 to 24 hours; (3), the inorganic fiber paper after the reaction is taken out and flushed with clear water until the pH is neutral; the inorganic fiber paper is taken out and aired; temperature programming treatment is adopted for obtaining aluminium modified silica-gel adsorbent material. The aluminium modified silica-gel adsorbent material prepared by the process has the advantages of large adsorption quantity, high dehumidification efficiency, low regeneration temperature, good thermoduric performance, high mechanical strength and long service life, and can be widely applied to the production and the manufacture of dehumidification rotary wheels.
Description
Technical field
The present invention relates to a kind of adsorbent technology, particularly a kind of aluminum modified silica gel adsorbent material and preparation method thereof.
Background technology
The absorption type gas purification technique significantly becomes one of technology of sustainable development in advantage aspect low-grade energy utilization and the environmental protection.In the absorption type gas purification technique, absorption working pair is the key of decision adsorption system performance, absorption working pair of having developed and combination thereof reach over one hundred kind, but select from the practicality of adsorbent, the adsorbent that is used for absorption type rotation dehumidifier at present only limits to the contour hygroscopic matter of lithium chloride, silica gel and molecular sieve; The lithium chloride good hygroscopicity, regeneration temperature is low, but peripheral hardware is had corrosivity; Molecular sieve is suitable for low dew point degree of depth dehumidifying, but regeneration temperature height (more than 250 ℃); The performance of silica gel is between between the two, not only be applicable to conventional dehumidifying (silochrom) but also be applicable to low dew point degree of depth dehumidifying (Kiselgel A), wherein Kiselgel A is applicable to that making the silica gel dehumidifying changes core, and the key of making silica gel dehumidifying commentaries on classics core is the combination of silica gel and inorfil base material; It can adopt adhesive with silica gel powder bonding making on the inorfil base material, but because a little less than powder and the base material interface interaction power, adhesion is relatively poor, under higher temperature, use repeatedly under (more than 150 ℃), be prone to the dry linting phenomenon, make silica gel change the core performance instability, simultaneously, base material and silica gel duct can be partly stopped up in the use of adhesive, and the silica gel specific area is descended, thereby adsorption efficiency is reduced; Also can adopt sol-gel process on inorfil, to flood sodium metasilicate, obtaining silica gel with acid reaction then is deposited in fiber surface and the space thereof: owing to restricted by collosol stability and fiber factor such as non-solubility in water, adsorbent kiss-coating amount on fiber is few, be difficult to form high concentration colloidal sol, thereby the colloidal sol amount of adhering on inorfil is few, the silica gel that generates is few, and dehumidification rate is low, and the made attached efficient of dehumidifying commentaries on classics wicking is lower.In order to overcome the shortcoming of these technology, a kind of " nano aperture silica gel absorber preparation methods and application thereof " disclosed in number of patent application is 02149717.6 application for a patent for invention, this sorbent material is prepared by the method for interpolation soluble calcium salt as precipitating reagent, but also there is following deficiency in this technology: (1) absorption property has much room for improvement; (2) heat resistance needs to strengthen; Since the silica gel heat resistance a little less than, dehumidifying is changeed core and is in for a long time in 80～150 ℃ of regenerative environ-ment, is prone to fusion, subsides, stops up phenomenon such as duct, thereby make system's adsorption efficiency reduction; (3) mechanical strength remains to be strengthened; Since silica gel and ceramic fibre active force a little less than, make that commentaries on classics core material mechanical strength is relatively poor, in system's running, be prone to efflorescence, dry linting phenomenon, thereby influence its service life.
Summary of the invention
The objective of the invention is to overcome the shortcoming of prior art, the aluminum modified silica gel adsorbent material of superior functions such as a kind of adsorbance is big, regeneration temperature is lower, good heat resistance, mechanical strength height is provided.
Another object of the present invention is to provide the preparation method of above-mentioned aluminum modified silica gel adsorbent material.
The object of the invention is achieved through the following technical solutions: the preparation method of this aluminum modified silica gel adsorbent material comprises the steps---
(1) under the room temperature inorganic fibre paper is immersed in the waterglass, takes out behind 2～5h, dry 10～24h;
(2) aluminum soluble salt is made into the aqueous solution, and adds weak acid regulator solution pH value 0.5～2, be warming up to 30～80 ℃, the powerful stirring down, with the above-mentioned inorganic fibre paper of gained solution impregnation, coprecipitation reaction takes place in the surface of inorfil and space thereof, fully reacted 12～24 hours;
(3) reacted inorganic fibre paper is taken out, it is neutral washing to pH with clear water, and taking-up is dried, and adopts temperature programming to handle and obtains aluminum modified silica gel adsorbent material.
Modulus of water glass is 2.0～3.5 in the described step (1), and concentration is 10～40% (percentage by weights); Not stopping up the honeycomb duct when selection of modulus of water glass is changeed core with the dehumidifying of dipping honeycomb is prerequisite, and the selection of its concentration then mostly is condition as far as possible with base material kiss-coating amount; The inventor finds that by repetition test the modulus of waterglass is 2.8～3.5, and the waterglass weight percent concentration is 20～35% o'clock, and silica obtained dehumidifying is changeed core and had best external form and better absorption property.
Aluminum soluble salt is aluminium chloride, aluminum nitrate, aluminum sulfate etc. in the described step (2), and its concentration is 5%～25% (percentage by weight); The aluminium salinity is too low then to be unfavorable for deposition, too high then deposit inhomogeneous, the experiment proved that effect preferably matched proportion density be 10～25% (percentage by weights).
PH value of solution value preferred 1～1.8 in the described step (2); When selecting acid to regulate salting liquid pH value, must consider that acid solution is to changeing the corrosivity (as high concentrated acid, strong acid) of core, pH value amplitude of variation (the pH value is minor swing as far as possible) in the consideration system simultaneously, should use low concentration weak acid (as acetic acid, lactic acid, gluconic acid etc.) to regulate the pH value, make that the porous material that generates is that pore size is even, narrow distribution.
Temperature is preferred 40～60 ℃ in the described step (2); Temperature is too low, and reaction speed is slow, is unfavorable for producing, and temperature is too high, to the corrosiveness enhancing of impregnating equipment and sorbent material, and what is more important, reaction temperature and sorbent material absorption property are closely related.
Stir speed (S.S.) is a prerequisite with reaction system concentration homogeneous in the described step (2), the pH value that particularly needs regulator solution, because along with constantly carrying out of reaction, the pH value of solution constantly raises, and therefore needs constantly the outer acid solution of adding to keep the pH value of solution value at a constant value range.
The program hyperthermic treatment is slowly to heat up down at 200～300 ℃ earlier in the described step (3), and cooling naturally, 2～3 times repeatedly, slowly be warmed up to 450～550 ℃ again, and be incubated 1～3 hour, then cooling naturally; Taking temperature programming technology is for moisture and volatile impurity in removing the commentaries on classics core, and in the process that forms Si-O-Si (or Si-O-Al) network, reduce the contraction rate of gel as much as possible, avoid the material internal regional stress to concentrate and crack, reduce the fragility of material.
The present invention is by the method for dipping co-precipitation, adopt steep water glass, aluminium salt successively, and technology such as regulator solution pH value, intensification, powerful splash bar, make the aluminum modified silica of generation be deposited on the space and the surface of inorfil in a large number, again through moulding, sintering processes, thus synthesize have high adsorption capacity, low regeneration temperature, the better aluminum modified silica gel adsorbent material of heat resistance and mechanical strength; The dehumidifying that prepared sorbent material can be applied in absorption type gas dehumidification drying or the absorption type refrigerating air-conditioning is changeed in the core apparatus.
The mechanism of action of the present invention is: the inorganic fibre paper that will contain sodium metasilicate is immersed in the soluble aluminum salting liquid of certain acidity, because Al
3+Modifying function makes that the Al atomic component substitutes the Si atom in the tetrahedron, because [AlO
4]
5-Than [SiO
4]
4-More negative electrical charge is arranged, make to form stronger hydrogen bond, i.e. Al by the top O active force bigger in angle the proton of OH
3+Hydrone is had stronger affinity, easily adsorb more hydrone; On the other hand, because Al
3+Modification, the network structure that the appreciable impact silica gel particle forms in sol-gel process, the specific area and the pore volume of raising aluminium modified adsorbent material increase the activated adoption position, thereby can improve the absorption property of sorbent material; Simultaneously,, not only strengthened the support force of duct skeleton, improved the heat resistance of material, and strengthened the interaction of adsorbent and inorfil, improved the mechanical strength of material owing to the formation of aluminium modified adsorbent material surface Al-O-Si key.
The present invention has following advantage and effect with respect to prior art: (1) adsorbance is big, dehumidification rate is high; (2) regeneration temperature lower (suitable) with silica gel; (3) heat resistance is good, mechanical strength is high, long service life; The experiment proved that, utilize its performance of aluminum modified silica gel adsorbent material of the inventive method preparation obviously to be better than silica gel product of the same type (number of patent application is 02149717.6 the disclosed nano aperture silica gel absorption of application for a patent for invention agent material), this aluminum modified silica gel adsorbent material can make its adsorbance improve 12.0%～25.0%, heat resistance strengthens, mechanical strength improves 35.0～74.0%, improves 1～2 times service life.
Description of drawings
Fig. 1 is different adsorbents absorption property comparison diagrams when 298K.
Fig. 2 is different adsorbents thermogravimetric curve figure under 298K～973K temperature.
Fig. 3 is different adsorbent mechanical strength comparison diagrams.
Fig. 4 is different adsorbent pore-size distribution situation schematic diagrames.
Fig. 5 is different adsorbent specific areas and pore volume situation schematic diagram.
The specific embodiment
The inventor has a lot of successful implementation examples through in a few years development; In order to illustrate that better the present invention had both increased moisture removal, improved absorption property, material thermal resistance energy and mechanical strength have been improved again, thereby improved material service life, enumerate three embodiment of the present invention below and also in conjunction with the accompanying drawings its technical performance index is compared, but embodiments of the present invention are not limited thereto.
Embodiment 1
The inventive method comprises following concrete steps: under (1) room temperature, in 250L round plastic container, add 100L water, add modulus then and be 3.0 waterglass 80Kg, after stirring, ( 300mm * 150mm) puts into and wherein floods 3 hours will to be changeed core by the honeycomb of inorganic fibre paper hot-roll forming, it is fully soaked into, taking-up is dried, and 60 ℃ of following air blast low temperature dryings 18 hours, is cooled to room temperature then; (2) the crystalline sulfuric acid aluminium that takes by weighing 30Kg is dissolved in the water of 120L, and adding acetic acid regulator solution pH value is 1.0, is warming up to 50 ℃, under brute force stirs, above-mentioned honeycomb is changeed core immerses wherein, and in the pH value of solution value be under 1.0 the condition strict control reaction (along with constantly carrying out of reaction, the pH value of solution value raises, need add acid solution frequently, as follows), take out after 12 hours, wash with clear water, dry, place baking oven again, be cooled to room temperature in 60 ℃ of low temperature dryings 24 hours; (3) will change core and be placed in the intelligent constant-temperature sintering furnace, elder generation slowly heats up down at 200～300 ℃, and cooling naturally, and 2～3 times repeatedly, slowly be warmed up to 450 ℃ again, be incubated 3 hours, naturally cool to the dehumidifying commentaries on classics core that room temperature obtains containing the aluminum modified silica adsorbent then.
The inventive method comprises following concrete steps: under (1) room temperature, in 250L round plastic container, add 100L water, add modulus then and be 3.5 waterglass 100Kg, after stirring, the honeycomb of inorganic fibre paper hot-roll forming is changeed core, and ( 5300mm * 150mm) puts into and wherein floods 5 hours, it is fully soaked into, taking-up is dried, and 60 ℃ of following low temperature dryings 24 hours, is cooled to room temperature then; (2) taking by weighing the 40Kg crystal aluminum chloride is dissolved in the water of 120L, be warming up to 60 ℃, under brute force stirs, above-mentioned honeycomb is changeed core to be immersed wherein, adding lactic acid regulator solution pH value is 1.5, reacts after 18 hours and takes out, and dries with the clear water flushing, place baking oven in 60 ℃ of low temperature dryings 24 hours again, be cooled to room temperature; (3) will change core and be placed in the intelligent constant-temperature sintering furnace, elder generation slowly heats up down at 200～300 ℃, and cooling naturally, and 2～3 times repeatedly, slowly be warmed up to 500 ℃ again, be incubated 2 hours, naturally cool to the dehumidifying commentaries on classics core that room temperature obtains containing the aluminum modified silica adsorbent then.
Embodiment 3
The inventive method comprises following concrete steps: under (1) room temperature, in 250L round plastic container, add 100L water, add modulus then and be 2.8 waterglass 100Kg, after stirring, the honeycomb of inorganic fibre paper hot-roll forming is changeed core, and ( 300mm * 150mm) puts into wherein to flood and it was fully soaked in 2 hours, and taking-up is dried, at 60 ℃ of following low temperature drying 12h, be cooled to room temperature then; (2) the crystallization aluminum nitrate that takes by weighing 45Kg is dissolved in the water of 120L, adding gluconic acid regulator solution pH value is 1.8, be warming up to 40 ℃, under brute force stirs, above-mentioned honeycomb is changeed core immerse wherein, it is neutral washing to pH with clear water after 24 hours, and taking-up is dried, place baking oven in 60 ℃ of low temperature dryings 24 hours again, be cooled to room temperature; (3) will change core and be placed in the intelligent constant-temperature sintering furnace, earlier 200～300 ℃ of slow down intensifications, and cooling naturally, 2～3 times repeatedly, slowly be warmed up to 550 ℃ again, insulation 1h naturally cools to room temperature then and obtains containing aluminum modified silica gel adsorbent material dehumidifying commentaries on classics core.
The sorbent material prepared to the foregoing description carries out performance test, for comparative effectiveness more directly, be that disclosed nano aperture silica gel (hereinafter to be referred as " silica gel ") sorbent material compares in 02149717.6 the application for a patent for invention (hereinafter to be referred as " in first to file ") simultaneously with aluminum modified silica gel adsorbent material of the present invention and number of patent application.Fig. 1 is the comparison of different adsorbents absorption property when 298K, as seen from Figure 1, adopt the aluminum modified silica adsorbents adsorb performance of the inventive method gained all to be higher than the silica gel that utilization is generated in the first to file technology under the equal conditions, amplification reaches 12.0～25.0%, and is that best (saturated extent of adsorption reaches 148.8gm with the aluminum modified silica absorption property that adopts embodiment 2 gained
-2).
Fig. 2 is different adsorbents thermogravimetric curves under 298K～973K temperature, its weightlessness was divided into for two megastages: 25～150 ℃ and 150～700 ℃, and based on phase I weightlessness, be embodied in absorption, the desorption performance of material, from the I stage as can be seen, aluminum modified silica is the same with silica gel, and desorption temperature is suitable, but absorption property is apparently higher than silica gel; (M=Si, Al) the condensation dehydration between embody the heat resistance of material, and from the percentage loss of weight in II stage as can be seen, the weightless order of sample is: silica gel＞embodiment 1 ≈ embodiment 2＞embodiment 3 and the weightlessness of second stage shows as M-OH.Show that aluminum modified silica adsorbent heat resistance is better than silica gel, and the modification aluminium composition is many more, hear resistance good more (embodiment 3).
Different adsorbent mechanical strengths more as shown in Figure 3, as seen from Figure 3, the breaking length of aluminum modified silica all is better than silica gel, amplification reaches 35.0～74.0%, and is optimum with the mechanical strength of embodiment 2.
Fig. 4 is different adsorbent pore-size distribution situations, as can be seen from Figure 4, aluminum modified silica (comprising silica gel), its aperture is in the scope of 0.3～8nm, because the aperture is little, specific area is big, thereby water vapour is had huge adsorption capacity, and Modification on Al
3+Exist, less to micropore size influence in the adsorbent surface structure, and the mesopore aperture obviously increases.
Fig. 5 is different adsorbent specific areas and pore volume situation, from eigenstate (silica gel) to Modification on Al
3+When accounting for 5.530wt% (embodiment 2), specific area is by 347.4m
2G
-1Suddenly increase to 472.1m
2G
-1, amplification reaches 35.90%; Equally, the pore volume of adsorbent also enlarges markedly; To embodiment 2, the variation of pore volume is by 0.2690cm by silica gel
3G
-1Increase to 0.4765cm
3G
-1, amplification is up to 47.65%.Obviously, the aluminium ion modification makes silica gel specific area and pore volume increase, and shows that the aluminium ion modification affects the formation of network structure in the system sol-gel process significantly.
In sum, utilize prepared its performance parameter of aluminum modified silica adsorbent of the inventive method obviously to be better than adsorbent of the same type, it is big to have adsorbance, regeneration temperature lower (＜150 ℃) good heat resistance, the mechanical strength advantages of higher can be widely applied in the manufacturing of desiccant wheel.
Claims (10)
1, a kind of preparation method of aluminum modified silica gel adsorbent material is characterized in that comprising the steps:
(1) under the room temperature inorganic fibre paper is immersed in the waterglass, takes out behind 2～5h, dry 10～24h;
(2) aluminum soluble salt is made into the aqueous solution, and adds weak acid regulator solution pH value 0.5～2, be warming up to 30～80 ℃, the powerful stirring down, with the above-mentioned inorganic fibre paper of gained solution impregnation, coprecipitation reaction takes place in the surface of inorfil and space thereof, fully reacted 12～24 hours;
(3) reacted inorganic fibre paper is taken out, it is neutral washing to pH with clear water, and taking-up is dried, and adopts temperature programming to handle and obtains aluminum modified silica gel adsorbent material.
2, the preparation method of aluminum modified silica gel adsorbent material according to claim 1 is characterized in that: modulus of water glass is 2.0～3.5 in the described step (1), and concentration is 10～40%.
3, the preparation method of aluminum modified silica gel adsorbent material according to claim 1 is characterized in that: aluminum soluble salt is aluminium chloride, aluminum nitrate, aluminum sulfate in the described step (2).
4, the preparation method of aluminum modified silica gel adsorbent material according to claim 1 is characterized in that: the soluble aluminum salinity is 5%～25% in the described step (2).
5, the preparation method of aluminum modified silica gel adsorbent material according to claim 1 is characterized in that: describedly state that the pH value of solution value is 1～1.8 in the step (2).
6, the preparation method of aluminum modified silica gel adsorbent material according to claim 1 is characterized in that: weak acid is acetic acid, lactic acid, gluconic acid described in the step (2).
7, the preparation method of aluminum modified silica gel adsorbent material according to claim 1 is characterized in that: the intensification temperature is 40～60 ℃ in the described step (2).
The preparation method of 8 aluminum modified silica gel adsorbent material according to claim 1 is characterized in that: add acid solution in the whipping process of described step (2) and keep the pH value of solution value at a constant value range.
9, the preparation method of aluminum modified silica gel adsorbent material according to claim 1, it is characterized in that: the program hyperthermic treatment is slowly to heat up down at 200～300 ℃ earlier in the described step (3), and cooling naturally, 2～3 times repeatedly, slowly be warmed up to 450～550 ℃ again, be incubated 1～3 hour, then cooling naturally.
10, according to each a kind of aluminum modified silica gel adsorbent material of preparation method preparation of aluminum modified silica gel adsorbent material of claim 1～9.
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|---|---|---|---|
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|---|---|---|---|
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| CN109589929B (en) * | 2018-11-20 | 2022-02-15 | 华东理工大学 | Structured silica gel adsorption material and preparation method thereof |
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| CN111408337A (en) * | 2020-03-17 | 2020-07-14 | 江苏苏净集团有限公司 | Silica gel dehumidification rotating wheel and preparation method thereof |
| CN111408338B (en) * | 2020-03-17 | 2023-03-14 | 江苏苏净集团有限公司 | Silica gel rotating wheel adsorbing material for dehumidification and preparation method thereof |
| CN115219490A (en) * | 2022-08-05 | 2022-10-21 | 青岛美高集团有限公司 | PH color-changing indicating silica gel and preparation method thereof |
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