CN101591021A - A kind of preparation method of thick-hole block silica gel - Google Patents
A kind of preparation method of thick-hole block silica gel Download PDFInfo
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- CN101591021A CN101591021A CNA2009100166237A CN200910016623A CN101591021A CN 101591021 A CN101591021 A CN 101591021A CN A2009100166237 A CNA2009100166237 A CN A2009100166237A CN 200910016623 A CN200910016623 A CN 200910016623A CN 101591021 A CN101591021 A CN 101591021A
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Abstract
The present invention relates to a kind of preparation method of thick-hole block silica gel, this method has overcome higher, the unsettled shortcoming of quality of cost in the present preparation silochrom process, utilize and create the supporting continuous glue technology and equipment of design and craft voluntarily, adopting certain density sulfuric acid and water glass is raw material, through strengthening reaction, generate silicon sol, again through aging condensation, washing desalination, ammonia treatment, drying and dehydrating and make purity greater than 99%, the adaptable thick-hole block silica gel of hole structural property index; This method at first is with the sodium silicate solution purifying, filters out impurity, and water glass is added water, and to be adjusted to density be 1.01-1.50g/cm
3, its temperature condition will add water then and regulate concentration at 20-40 ℃, make SiO
2Concentration be: 20～23%, density is 1.28-1.34g/cm
3, stir; Last and concentration is that the acid solution of 32.5-33.5% is that 0.30-0.40MPa, temperature are glue under 20-53 ℃ condition at pressure, after oven dry and screening, can obtain gross porosity blob of viscose involved in the present invention.
Description
Technical field
The invention belongs to the preparing technical field of silica gel, be specifically related to a kind of preparation method of thick-hole block silica gel.
Background technology
Silica gel is divided into organic silica gel and inorganic silica gel, organic silica gel belongs to special synthetic rubber, the major ingredient of inorganic silica gel is a silicon-dioxide, is a kind of porous adsorbent of structure image cavernous body, can adsorb aqueous vapor, water insoluble and other solvents, nonpoisonous and tasteless, chemical property is stable, and Chang Zuowei siccative and sorbent material use, the model of silica gel is varied, and the silica gel of different model forms different skeleton structures because of its Production Flow Chart and preparation method different.According to varying in size of aperture, silica gel can be divided into macropore, gross porosity, pore etc., and silochrom has high absorption capacity at high humidity environment, and Kiselgel A has high absorption capacity at low-humidity environment, the silica gel that has adsorbed moisture through being exposed to the sun and air-dry after, reducible its adsorptive power.
Silica gel is to be main raw material with silicate, adopts suitable mol ratio to add behind the mineral acid and a kind of porous mass that generates.Chinese patent CN1158310 utilizes silicate and mineral acid to produce aperture and the limited silica gel of pore volume, Chinese patent CN0215935518 directly joins aperture silica gel and prepares macroporous silica gel in the alkaline solution, and Chinese patent CN200510117271.6 utilizes silicate and the mineral acid effect behind the purifying to prepare high-purity silica gel; The silica gel of related making exists shortcomings such as bigger individual character difference, the not strong and original cost of hole structural property index adaptability is higher in these inventions, be difficult to obtain the stable prod of constant mass, therefore, development has advanced technology of preparing and makes high-performance silica gel, has become the technical barrier that needs to be resolved hurrily.
Summary of the invention
At the shortcoming that exists in the above-mentioned art methods, the present invention proposes a kind of preparation method of thick-hole block silica gel.This method has overcome prepared silica gel and has existed shortcomings such as individual character difference, hole structural property index adaptability are not strong, silica gel quality instability, resulting silica gel steady quality, and cost is lower, and time-consuming is shorter, its purity is greater than 99%, and hole structural property index adaptability is strong.
That raw material standard used herein requires is low, take high density, high-temperature adhesive-preparing technology and unique chemical iron removal technology continuously fast, adopt and create supporting continuous glue making machine of design and craft and washing desalting plant voluntarily, thereby guaranteed the steady quality of silica gel, can be widely used in petrochemical industry and fine chemicals industries such as catalyzer and support of the catalyst, matting agent, the agent of plastics opening.
It is raw material that the present invention adopts certain density sulfuric acid and water glass, through strengthening reaction, generates silicon sol, again through aging condensation, washing desalination, ammonia treatment, and drying and dehydrating and making.The ultimate principle of production process is: sulfuric acid and water glass reaction generate silicic acid and sodium sulfate.Because silicic acid is a kind of very unsettled weak acid, the intermolecular condensation that carries out, and form poly silicic acid, silica gel is exactly the final product of polycondensation.Its reaction equation (signal formula) is:
N
aSiO
3+H
2SO
4→N
aSiO
4+H
2SiO
3
H
2SiO
3→SiO
2·nH
2O+H
2O
In process of production, the implementation step of the technical process of silica gel is:
The first step, the raw material configuration
This step is that the water glass and the vitriol oil are mixed with suitable solution respectively, and is stand-by.
1) in the raw material configuration flow, at first be with the sodium silicate solution purifying, filter out impurity, water glass is added water, and to be adjusted to density be 1.01-1.50g/cm
3, its temperature condition is at 20-40 ℃, the cleaning plate-and-frame filter press, and the sodium silicate solution that allotment is finished is squeezed in the plate-and-frame filter press with pump and is filtered, and then flows into and filters the alkali pond.Serve as the filtering velocity degree when very slow, shut down, cleaned filter cloth.Filter and finish, sodium silicate solution is squeezed into storage alkali jar.
2) temperature less than 25 ℃ condition under, the sodium silicate solution after will filtering with pump is squeezed into the alkali-prepared tank from storage alkali jar, opens pneumatic blending, adds water and regulates concentration, makes SiO
2Content is: 20～23%, and density is 1.28-1.34g/cm
3, stirring, time of repose is greater than after 36 hours, and if sampling analysis is the as clear as crystal inclusion-free of solution, through set aside for use after the assay was approved.
3) temperature less than 25 ℃ condition under, earlier with adding clear water in the complex acid jar, open pneumatic blending, slowly add the vitriol oil again, regulate concentration, make it to reach 32.5-33.5%, stir, sampling analysis is if as clear as crystal inclusion-free is stand-by through the postcooling that is up to the standards.
Second step, glue
The pressure of reaction chamber is adjusted to 0.30-0.40Mpa, temperature is adjusted to 20-53 ℃, be configured to deployed raw material in the reaction chamber respectively, detect the pH value of colloidal sol, make it in the 1.5-2.5 scope, fully reaction is fused after 32 hours, detects free acid, make its concentration in the 0.4%-0.9% scope, adjust pressure to normal pressure.The silica gel that obtains forms 3.5 centimetres blob of viscose after cutting through the rubber tapping machine.
The 3rd step, washing
Through 3-6 level series connection water washing process, every grade of washing stage, 30 centimetres in the high plastic emitting face of the water surface, the first progressive hot water, 50 ℃ of water temperatures, 30 centimetres in the high plastic emitting face of the water surface, if certain one-level water surface does not reach requirement, water valve at the corresponding levels is opened automatically, and the back water valve that makes it to meet the demands cuts out, the 6th grade of sewer, detect the acid content of the 6th grade of silica gel, acid content PH＞5.8 o'clock in the glue all seal in water in next washing pool, through ammonia bubble operation 4 hours, finally form pH value greater than 6.7 blob of viscose.
At last, after oven dry and screening, just can obtain gross porosity blob of viscose involved in the present invention.
The present invention compares with traditional method, and it has the advantage of following four aspects:
(1) the reaction conditions gentleness is easy and simple to handle;
(2) this preparation method is under the condition of low-cost ingredient requirement, can obtain purity greater than 99% thick-hole block silica gel;
(3) silica gel that utilizes this preparation method to produce, its hole structural property index adaptability is strong;
(4) supporting continuous glue making machine of design and craft and washing desalting plant are created in employing voluntarily, thereby have guaranteed the steady quality of silica gel.
Embodiment
Further specify below in conjunction with embodiment, and unrestricted scope involved in the present invention.
Embodiment 1:
The first step, batching
Getting density is 1.20g/cm
3Sodium silicate solution 3000ml, under 35 ℃ of temperature condition, this sodium silicate solution squeezed in the pressure filter filters, kept 30 minutes, then squeeze into and have in the filtration vessel that cleans filter cloth.
From filtration vessel, take out sodium silicate solution, import in the outfit container, under 20 ℃ of temperature condition, add water and regulate concentration, survey concentration while stirring, make SiO
2Content is: 19.5%, and density is 1.28g/cm
3, stir, left standstill 38 hours.
Under 20 ℃ of temperature condition, will add clear water in the complex acid container, slowly add the vitriol oil, regulate concentration, make it to reach 32.5%, stir stand-by.
Second step, glue
The pressure of small-sized reaction chamber is adjusted to 0.30Mpa, get 800ml concentration and be 32.5% sulphuric acid soln and slowly inject small-sized reaction chamber, slowly add the SiO that has been configured
2Content is 19.5% sodium silicate solution, surveys the pH value data while mixing, and makes it in the 1.5-2.5 scope, leave standstill fused be converted into silicic acid after, aging 32 hours, survey the free acid concentration in the glue, make its concentration in the 0.4%-0.7% scope, adjust pressure, increase pH value to normal pressure, carry out 3 grades of series connection water washing process, 50 ℃ of chopped-off head water temperatures, acid content PH＞5.8 o'clock in the glue, ammonia bubble operation 4 hours, the final pH value that forms is greater than 6.7 blob of viscose, SiO
2Purity 99.2%.
Embodiment 2:
The first step, batching
Getting density is 1.1g/cm
3Sodium silicate solution 3000ml, under 30 ℃ of temperature condition, this sodium silicate solution squeezed in the pressure filter filters, kept 50 minutes, then squeeze into and have in the filtration vessel that cleans filter cloth.
From filtration vessel, take out sodium silicate solution, import in the outfit container, under 22 ℃ of temperature condition, add water and regulate concentration, survey concentration while stirring, make SiO
2Content is: 20.12%, stir, and left standstill 36 hours.
Second step, glue
The pressure of small-sized reaction chamber is adjusted to 0.35Mpa, get 800ml concentration and be 32.8% sulphuric acid soln and slowly inject small-sized reaction chamber, slowly add the SiO that has been configured
2Content is 20.12% sodium silicate solution, surveys the pH value data while mixing, and makes it in the 1.8-2.0 scope, leave standstill fused be converted into silicic acid after, aging 32 hours, survey the free acid concentration in the glue, make its concentration in the 0.5-0.7% scope, adjust pressure, increase pH value to normal pressure, carry out 3 grades of series connection water washing process, 55 ℃ of chopped-off head water temperatures, acid content PH＞5.9 o'clock in the glue, ammonia bubble operation 4 hours, the final pH value that forms is greater than 6.8 blob of viscose, SiO
2Purity 99.12%.
Embodiment 3:
The first step, batching
Getting density is 1.35g/cm
3Sodium silicate solution 3000ml, under 38 ℃ of temperature condition, this sodium silicate solution squeezed in the pressure filter filters, kept 40 minutes, then squeeze into and have in the filtration vessel that cleans filter cloth.
From filtration vessel, take out sodium silicate solution, import in the outfit container, under 22 ℃ of temperature condition, add water and regulate concentration, survey concentration while stirring, make SiO
2Content is: 21.5%, stir, and left standstill 36 hours.
Second step, glue
The pressure of small-sized reaction chamber is adjusted to 0.35Mpa, get 1000ml concentration and be 33.0% sulphuric acid soln and slowly inject small-sized reaction chamber, slowly add the SiO that has been configured
2Content is 21.5% sodium silicate solution, surveys the pH value data while mixing, and makes it in the 1.9-2.5 scope, leave standstill fused be converted into silicic acid after, aging 32 hours, survey the free acid concentration in the glue, make its concentration in the 0.6-0.8% scope, adjust pressure, increase pH value to normal pressure, carry out 4 grades of series connection water washing process, 54 ℃ of chopped-off head water temperatures, acid content PH＞6.0 o'clock in the glue, ammonia bubble operation 4 hours, the final pH value that forms is greater than 6.8 blob of viscose, SiO
2Purity 99.33%.
Embodiment 4:
The first step, batching
Getting density is 1.40g/cm
3Sodium silicate solution 3000ml, under 39 ℃ of temperature condition, this sodium silicate solution squeezed in the pressure filter filters, kept 50 minutes, then squeeze into and have in the filtration vessel that cleans filter cloth.
From filtration vessel, take out sodium silicate solution, import in the outfit container, under 24 ℃ of temperature condition, add water and regulate concentration, survey concentration while stirring, make SiO
2Content is 22%, stirs, and leaves standstill 38 hours.
Second step, glue
The pressure of small-sized reaction chamber is adjusted to 0.38Mpa, get 1000ml concentration and be 33.5% sulphuric acid soln and slowly inject small-sized reaction chamber, slowly add the SiO that has been configured
2Content is 22% sodium silicate solution, surveys the pH value data while mixing, and makes it in the 1.5-1.9 scope, leave standstill fused be converted into silicic acid after, aging 32 hours, survey the free acid concentration in the glue, make its concentration in the 0.4-0.7% scope, adjust pressure, increase pH value to normal pressure, carry out 3 grades of series connection water washing process, 36 ℃ of chopped-off head water temperatures, acid content PH＞5.6 o'clock in the glue, ammonia bubble operation 4 hours, the final pH value that forms is greater than 6.5 blob of viscose, SiO
2Purity 99.15%.
Embodiment 5:
The first step, batching
Getting density is 1.50g/cm
3Sodium silicate solution 3000ml, under 25 ℃ of temperature condition, this sodium silicate solution squeezed in the pressure filter filters, kept 50 minutes, then squeeze into and have in the filtration vessel that cleans filter cloth.
From filtration vessel, take out sodium silicate solution, import in the outfit container, under 24 ℃ of temperature condition, add water and regulate concentration, survey concentration while stirring, make SiO
2Content is 22.32%, stirs, and leaves standstill 38 hours.
Second step, glue
The pressure of small-sized reaction chamber is adjusted to 0.38Mpa, get 1000ml concentration and be 33.5% sulphuric acid soln and slowly inject small-sized reaction chamber, slowly add the SiO that has been configured
2Content is 22.32% sodium silicate solution, surveys the pH value data while mixing, and makes it in the 1.5-1.7 scope, leave standstill fused be converted into silicic acid after, aging 32 hours, survey the free acid concentration in the glue, make its concentration in the 0.5-0.8% scope, adjust pressure, increase pH value to normal pressure, carry out 3 grades of series connection water washing process, 40 ℃ of chopped-off head water temperatures, acid content PH＞5.8 o'clock in the glue, ammonia bubble operation 4 hours, the final pH value that forms is greater than 6.8 blob of viscose, SiO
2Purity 99.23%.
Claims (8)
1, a kind of preparation method of thick-hole block silica gel, it adopts sulfuric acid and water glass is raw material, through behind the Impurity removal, in reaction chamber, react through strengthening, generate silica gel, again through aging condensation, washing desalination, ammonia treatment, step such as drying and dehydrating and make thick-hole block silica gel, it is characterized in that: the preparation method of described thick-hole block silica gel under the condition of low-cost raw material, prepare purity greater than 99%, the adaptable thick-hole block silica gel of hole structural property index.
2, the preparation method of thick-hole block silica gel according to claim 1 is characterized in that: set aside for use when described vitriolic concentration is 32.5-33.5%.
3, the preparation method of thick-hole block silica gel according to claim 1 is characterized in that: described water glass is 1.01-1.50g/cm in density
3, temperature impurity screening in the time of 20-40 ℃.
4, the preparation method of thick-hole block silica gel according to claim 3 is characterized in that: described sodium silicate solution is at SiO
2Content reach 20～23%, density reaches 1.28-1.34g/cm
3The time set aside for use.
5, the preparation method of thick-hole block silica gel according to claim 1 is characterized in that: the pressure of described reaction chamber is 0.30-0.40Mpa, and temperature is 20-53 ℃.
6, the preparation method of thick-hole block silica gel according to claim 1 is characterized in that: the silica gel pH value after the described washing desalination step is greater than 5.8.
7, the preparation method of thick-hole block silica gel according to claim 1 is characterized in that: the time of described ammonia treating step is 4 hours.
8, the preparation method of thick-hole block silica gel according to claim 7 is characterized in that: the silica gel pH value after the described ammonia treating step is greater than 6.7.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103030150A (en) * | 2012-12-26 | 2013-04-10 | 青岛中能集团有限公司 | Technological process of mesoporous silica gel |
| CN103043670A (en) * | 2012-12-26 | 2013-04-17 | 青岛中能集团有限公司 | Process flow of novel water-absorbent silica gel |
| CN103043669A (en) * | 2012-12-26 | 2013-04-17 | 青岛中能集团有限公司 | Microporous silica gel preparing flow |
| CN103058205A (en) * | 2012-12-26 | 2013-04-24 | 青岛中能集团有限公司 | Process flow for microporous adsorption silica gel |
| CN103086386A (en) * | 2012-12-26 | 2013-05-08 | 青岛中能集团有限公司 | Supermacroporous silica gel process flow |
| CN109796020A (en) * | 2019-04-02 | 2019-05-24 | 青岛硕远硅胶科技有限公司 | A kind of preparation method of the dedicated fine silica powder of catalyst |
| CN114057200A (en) * | 2022-01-18 | 2022-02-18 | 河北鑫鹏新材料科技有限公司 | Application of C-type silica gel preparation method in ZSM-5 molecular sieve mother liquor treatment and C-type silica gel |
-
2009
- 2009-06-29 CN CNA2009100166237A patent/CN101591021A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103030150A (en) * | 2012-12-26 | 2013-04-10 | 青岛中能集团有限公司 | Technological process of mesoporous silica gel |
| CN103043670A (en) * | 2012-12-26 | 2013-04-17 | 青岛中能集团有限公司 | Process flow of novel water-absorbent silica gel |
| CN103043669A (en) * | 2012-12-26 | 2013-04-17 | 青岛中能集团有限公司 | Microporous silica gel preparing flow |
| CN103058205A (en) * | 2012-12-26 | 2013-04-24 | 青岛中能集团有限公司 | Process flow for microporous adsorption silica gel |
| CN103086386A (en) * | 2012-12-26 | 2013-05-08 | 青岛中能集团有限公司 | Supermacroporous silica gel process flow |
| CN109796020A (en) * | 2019-04-02 | 2019-05-24 | 青岛硕远硅胶科技有限公司 | A kind of preparation method of the dedicated fine silica powder of catalyst |
| CN114057200A (en) * | 2022-01-18 | 2022-02-18 | 河北鑫鹏新材料科技有限公司 | Application of C-type silica gel preparation method in ZSM-5 molecular sieve mother liquor treatment and C-type silica gel |
| CN114057200B (en) * | 2022-01-18 | 2022-04-19 | 河北鑫鹏新材料科技有限公司 | Application of C-type silica gel preparation method in ZSM-5 molecular sieve mother liquor treatment and C-type silica gel |
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Application publication date: 20091202 |