CN105819884A - Waterproof alumina-silica gel particle product and production method thereof - Google Patents
Waterproof alumina-silica gel particle product and production method thereof Download PDFInfo
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- CN105819884A CN105819884A CN201610134179.9A CN201610134179A CN105819884A CN 105819884 A CN105819884 A CN 105819884A CN 201610134179 A CN201610134179 A CN 201610134179A CN 105819884 A CN105819884 A CN 105819884A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/0045—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by a process involving the formation of a sol or a gel, e.g. sol-gel or precipitation processes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/16—Preparation of silica xerogels
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B30/00—Compositions for artificial stone, not containing binders
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
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Abstract
The invention provides a waterproof alumina-silica gel particle product. The SiO2 content of the product is 80-88.5wt%, the Al2O3content of the product is 10-17wt%, the average specific surface area of the product is 400-700m<2>/g, the average aperture of the product is 2.0-5.0nm, the average granularity of gel granules is 0.5-8mm, and the average pore volume is 0.3-0.6ml/g. The invention also provides a production method of the waterproof alumina-silica gel particle product. The waterproof alumina-silica gel particle product with the advantages of good granule integrality, high compressive strength, small regeneration breaking rate, long service life and multi-time repeated regeneration can be prepared through the method, and a detection result shows that the pressure resistance of the finished product is not smaller than 70N/granule; and the waterproof rate can reach 95% or above, and the product difficulty cracks under a very high content of free water. The product can be used as a liquid adsorbent and a catalyst carrier, and also can be used as a protection layer of common silica gel and alumina-silica gel.
Description
Technical field
The invention belongs to silica gel production field, particularly relate to a kind of water-fast Guanulated gelatinized silica-alumina product and production method thereof.
Background technology
Industrial silicone is a kind of important inorganic chemical product, the chemical constituent of silica gel and physical arrangement, determine it and there is the unexistent feature of many other materials: absorption property is high, Heat stability is good, stable chemical nature, there is higher mechanical strength etc., therefore dehumidification desiccant it is widely used in, water absorbing agent, anti-blushing agent, catalyst carrier, filler etc., along with modern petrochemical, medicine, biochemistry, analytical technology, pesticide, papermaking, the development of coating technology, silica gel the most progressively moves towards to become more meticulous, specialized, apply more and more extensive, analyzing, separate and catalyst carrier, the application of the aspects such as coating constantly expands.Silica gel is classified according to shape, size, aperture, purposes, absorption feature etc., and kind is different, applies different, but common silica gel all has a shortcoming being difficult to overcome, and meets water and bursts.This shortens the service life of silica gel to a certain extent, improves use cost.
Summary of the invention
The present invention is directed to existing silica gel poor water resistance, meet the technical problem that water bursts, propose a kind of have higher resistance to water, the broken rate of regeneration is little, makes Guanulated gelatinized silica-alumina and the production method thereof of life-span length.
In order to achieve the above object, the technical solution used in the present invention is: a kind of water-fast Guanulated gelatinized silica-alumina, SiO in described gel particles2Content is 80wt%～88.5wt%, Al2O3Content is 10wt%～17wt%, and its average specific surface area is 400m2/ g～700m2/ g, average pore size is 2.0nm～5.0nm, and described gel particles particle mean size is 0.5mm～8mm, and average pore volume is 0.3ml/g～0.6ml/g.
As preferably, Al in described gel particles2O3Content is 14.8wt%～15.5wt%.
As preferably, described gel particles is relative humidity 10% time, and absorption 3～the steam of 7%, relative humidity 20% time, absorption 6～the steam of 9%, at relative humidity 80% time, absorption 30～the steam of 45%；Crushing resistance >=70N/, water-fast rate >=95%.
The present invention also proposes a kind of method producing above-mentioned water-fast Guanulated gelatinized silica-alumina product: will contain SiO210%～14%, Al (OH)3The aqueous slkali of 2.0%～3.0%, content be 8%～12% sulphuric acid or nitric acid or hydrochloric acid solution and content be 2.5%～4.5% aluminum sulfate solution, under pressure, react through suspendible formula prilling granulator, spray to air, and then be polycondensed into gel particles.This gel particles processes through bubble aging, sour, washing, drying process, thus obtains the water-fast Guanulated gelatinized silica-alumina of form of spherical particles again.
As preferably, SiO will be contained212 ± 0.5%, containing Al (OH)3The aqueous slkali of 2.5 ± 0.5%, content be 10 ± 0.5% sulfuric acid solution and content be the aluminum sulfate solution of 3.5 ± 0.5%, under pressure, react through suspendible formula prilling granulator, spray to air, and then it is polycondensed into gel particles, this gel particles processes through bubble aging, sour, washing, drying process, thus obtains the water-fast Guanulated gelatinized silica-alumina of form of spherical particles again.
As preferably, described aging technique is the gel particles that injection formed hot water temperature 20～80 DEG C of isothermal holding 0.5～2 hours；Again through acid bubble technique: mineral acid aluminum content be 1～5% solution in soak 2～10 hours；Again through washing: 30～60 DEG C of warm water washings to micelle PH=2.0～6.0；Finally it is dried technique: high-temperature process 3～5 hours at 100～150 DEG C, final finished product.
As preferably, in described aging technique, the isothermal holding time is 0.5～1.5 hour.
As preferably, described acid bubble technique use the acidifying solution containing 2%～3% aluminum sulfate to soak.
Compared with prior art, advantages of the present invention and have the active effect that by production method of the present invention, SiO can be prepared2Content is 80wt%～88.5wt%, Al2O3Content is the water-fast Guanulated gelatinized silica-alumina of 10wt%～17wt%；Gel particles granule percentage of head rice is good, and compressive resistance is high；The broken rate of regeneration is little, makes the life-span long, iterative regenerable repeatedly, the crushing resistance of finished product >=70N/ after testing；Water-fast rate, up to more than 95%, is used alone in the case of free water content is the highest and is not easy to burst.Can be used as liquid absorbent and catalyst carrier, it is possible to as ordinary silicon glue, the protective layer of Alusil.
Detailed description of the invention
In order to be better understood from the present invention, illustrate below in conjunction with embodiment.
Embodiment:
Preparation is containing SiO210%～14%, Al (OH)3The aqueous slkali of 2.0%～3.0%, content be 8%～12% sulfuric acid solution and content be that 2.5%～4.5% aluminum sulfate solution is stand-by；Sulfuric acid solution also can be selected for nitric acid or hydrochloric acid solution replaces, and selects sulfuric acid solution safer.
Under the pressure of 0.1～1.0MPa, above-mentioned solution carries out gradual reaction through suspendible formula prilling granulator, in nozzle injection to air, and then is polycondensed into graininess gel particle.Then gel particle is processed through following process technique successively:
Aging technique: inserted by gel particle in the ageing can being contained with 20～80 DEG C of hot water, soaks 0.5～2.0 hour.
Acid bubble technique: by the gel particle after aging mineral acid aluminum content be 1～5% solution in immersion 2～10 hours；This mineral acid aluminum solutions is the one in sulfuric acid solution, salpeter solution, hydrochloric acid solution.
Washing process: by the gel particle after acidifying as in rinsing bowl, with warm water washing, control water temperature 30～60 DEG C.Detect its pH value after rinsing every time, stop to during gel particle PH=2.0～6.0；
Drying process: being dried under high-temperature hot-air at 100～150 DEG C by the qualified gel particle of washing, drying time controls at 3～5 hours, final finished product.
Technological condition and the performance indications of four specific embodiments are shown in Table 1.
Table 1 is water-fast Alusil technological condition and main performance index thereof
After testing, SiO in ready gels grain2Content is 80wt%～88.5wt%, Al2O3Content is 10wt%～17wt%, its average specific surface area 400m2/ g～700m2/ g, average pore size is 2.0nm～5.0nm, and described gel particles particle mean size is 0.5mm～8mm, and average pore volume is 0.3ml/g～0.6ml/g.This product has acidproof (except HF acid), alkaline-resisting a, solvent resistant, Heat stability is good, the advantage such as nontoxic, tasteless.Suitably aperture and specific surface area so that it is there is good adsorptivity.Relative humidity 10% time, absorption 3～the steam of 7%, relative humidity 20% time, absorption 6～the steam of 9%, at relative humidity 80% time, absorption 30～the steam of 45%.Granule percentage of head rice is good, and compressive resistance is high；The broken rate of regeneration is little, makes the life-span long, iterative regenerable repeatedly, the crushing resistance of finished product >=70N/ after testing；In four embodiments, the water-fast rate of gel particle of preparation is all higher than 95%.Resistance to water is much better than industrial various bulk and the common silica gel such as spherical, has higher resistance to water.Al in described gel particles2O3When content is 14.8wt%～15.5wt%, water-fast rate is up to more than 99%.It is used alone in the case of free water content is the highest and is not easy to burst.
The production method of the present invention is water-fast Guanulated gelatinized silica-alumina product, will contain SiO on raw materials for production2Aqueous slkali in add content be 2.0%～3.0%Al (OH)3, under pressure, react through suspendible formula prilling granulator, spray to air, and then be polycondensed into gel particles.The addition of aluminium hydroxide, the Guanulated gelatinized silica-alumina prepared is made to have special framing structure, in addition particular procedure time and the control of temperature parameter in subsequent treatment process, throughout under the synergism of science and engineering skill, making aluminium sesquioxide content in the aluminium glue gel particles product prepared is 10wt%～17wt%, has good resistance to water.Wherein, the aluminum sulfate solution using content to be 1～5% in acid bubble technique, in acid bubble processing procedure, gel skeleton is carried out mends aluminum and increases the strengthening effect of aluminum, effectively prevent the Al in gel skeleton3+Washing process is eluted, in the Guanulated gelatinized silica-alumina content of aluminium oxide has been effectively ensured.The aluminum sulfate solution using content to be 1～4%, better, water-fast rate is up to 99%.
Produced the water-fast Alusil of pore obtained by above method, be typically used as Kiselgel A and the protective layer of pore Alusil, it is possible to be used alone in the case of free water (aqueous water) content is the highest.Containing in the case of aqueous water in operating system, this product is used also to can reach than relatively low dew point.The air being mainly used in air separation process is dried, and at petrochemical industry, electric industry, brewages etc. in industry and does liquid absorbent and catalyst carrier, as common silica gel, the protective layer of Alusil.When this product is used as protective layer, its consumption is use total amount about 20%.
The above; it it is only presently preferred embodiments of the present invention; it it is not the restriction that the present invention is made other form; any those skilled in the art are changed possibly also with the technology contents of the disclosure above or are modified as the Equivalent embodiments of equivalent variations is applied to other field; but it is every without departing from technical solution of the present invention content; any simple modification, equivalent variations and the remodeling made above example according to the technical spirit of the present invention, still falls within the protection domain of technical solution of the present invention.
Claims (8)
1. a water-fast Guanulated gelatinized silica-alumina product, it is characterised in that: SiO in described gel particles2Content is 80wt% ~ 88.5wt%, Al2O3Content is 10wt% ~ 17wt%, and its average specific surface area is 400m2/g~700m2/ g, average pore size is 2.0nm ~ 5.0nm, and described gel particles particle mean size is 0.5mm ~ 8mm, and average pore volume is 0.3ml/g ~ 0.6ml/g.
Water-fast Guanulated gelatinized silica-alumina product the most according to claim 1, it is characterised in that: Al in described gel particles2O3Content is 14.8wt% ~ 15.5wt%.
Water-fast Guanulated gelatinized silica-alumina product the most according to claim 1, it is characterised in that: described gel particles is at relative humidity 10% time, the steam of absorption 3 ~ 7%, relative humidity 20% time, the steam of absorption 6 ~ 9%, at relative humidity 80% time, the steam of absorption 30 ~ 45%；Crushing resistance >=70N/, water-fast rate >=95%.
4. the method for the water-fast Guanulated gelatinized silica-alumina product produced described in claim 1 ~ 3, it is characterised in that: SiO will be contained210%~14%、Al(OH)3The aqueous slkali of 2.0% ~ 3.0%, content be 8% ~ 12% sulphuric acid or nitric acid or hydrochloric acid solution and content be 2.5% ~ 4.5% aluminum sulfate solution, under pressure, react through suspendible formula prilling granulator, spray to air, and then it being polycondensed into gel particles, this gel particles processes through bubble aging, sour, washing, drying process, thus obtains the water-fast Guanulated gelatinized silica-alumina of form of spherical particles again.
Method the most according to claim 4, it is characterised in that: SiO will be contained212 ± 0.5%, containing Al (OH)3The aqueous slkali of 2.5 ± 0.5%, content be 10 ± 0.5% sulfuric acid solution and content be the aluminum sulfate solution of 3.5 ± 0.5%, under pressure, react through suspendible formula prilling granulator, spray to air, and then it is polycondensed into gel particles, this gel particles processes through bubble aging, sour, washing, drying process, thus obtains the water-fast Guanulated gelatinized silica-alumina of form of spherical particles again.
Method the most according to claim 5, it is characterised in that: described aging technique is that gel particles injection formed was 20 ~ 80 DEG C of isothermal holding of hot water temperature 0.5 ~ 2 hour；Again through acid bubble technique: soak 2 ~ 10 hours in the solution that mineral acid aluminum content is 1 ~ 5%；Again through washing: 30 ~ 60 DEG C of warm water washings are to micelle PH=2.0 ~ 6.0；Finally it is dried technique: high-temperature process 3 ~ 5 hours at 100 ~ 150 DEG C, final finished product.
Method the most according to claim 6, it is characterised in that: in described aging technique, the isothermal holding time is 0.5 ~ 1.5 hour.
Method the most according to claim 7, it is characterised in that: described acid bubble technique use the acidifying solution containing 2% ~ 3% aluminum sulfate to soak.
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| CN201610134179.9A CN105819884B (en) | 2016-03-10 | 2016-03-10 | Water-fast Guanulated gelatinized silica-alumina product and its production method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108046280A (en) * | 2017-12-25 | 2018-05-18 | 青岛美高集团有限公司 | A kind of Alusil and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1358667A (en) * | 2001-07-06 | 2002-07-17 | 青岛海洋化工集团公司 | Method for producing silico-aluminium gelatinized granule product |
| CN1522958A (en) * | 2003-02-21 | 2004-08-25 | 青岛海洋化工有限公司 | Process for manufacturing macroreticular spherical silica gel |
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- 2016-03-10 CN CN201610134179.9A patent/CN105819884B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1358667A (en) * | 2001-07-06 | 2002-07-17 | 青岛海洋化工集团公司 | Method for producing silico-aluminium gelatinized granule product |
| CN1522958A (en) * | 2003-02-21 | 2004-08-25 | 青岛海洋化工有限公司 | Process for manufacturing macroreticular spherical silica gel |
Non-Patent Citations (1)
| Title |
|---|
| 王力等: "耐水硅胶材料的制备及其研究进展", 《广东化工》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108046280A (en) * | 2017-12-25 | 2018-05-18 | 青岛美高集团有限公司 | A kind of Alusil and preparation method thereof |
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Effective date of registration: 20170726 Address after: The 29 floor International Building 8 Business District of Laoshan Quan Ling Road 266061 Shandong city of Qingdao Province Applicant after: Qingdao Gulf Group Co Ltd Address before: 266700, 1, Jin Shui Road, New River eco chemical industry base, Pingdu City, Shandong, Qingdao Applicant before: Qingdao Marine Chemical Co., Ltd. |
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