CN104229810A - Preparation method of coarse-pore blocky silica gel - Google Patents
Preparation method of coarse-pore blocky silica gel Download PDFInfo
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- CN104229810A CN104229810A CN201310246249.6A CN201310246249A CN104229810A CN 104229810 A CN104229810 A CN 104229810A CN 201310246249 A CN201310246249 A CN 201310246249A CN 104229810 A CN104229810 A CN 104229810A
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Abstract
The invention relates to a preparation method of coarse-pore blocky silica gel. The method overcomes the defects that in the process of preparing coarse-pore silica gel currently, the cost is high, and the quality is not stable. By using continuous gel manufacturing technology and equipment self-designed and created and matched with the process, coarse-pore blocky silica gel with a purity of over 99% and strong pore structure performance index adaptability is prepared by taking sulphuric acid and sodium silicate with certain concentration as raw materials through the steps of carrying out reinforcing reaction on the raw materials, so that silica sol is generated; and then sequentially carrying out aging and condensation, water washing for desalination, ammonia treatment, drying and dehydration on the silica sol. The method specifically comprises the following steps: firstly, purifying a sodium silicate solution, filtering out impurities, adding water into sodium silicate, and adjusting the obtained mixture until the density of the mixture is 1.01-1.50 g/cm<3>; then, at a temperature of 20-40 DEG C, adding water for adjusting the concentration until the concentration of SiO2 is 20-23% and the density is 1.28-1.34 g/cm<3>, and fully and uniformly stirring the obtained product; and finally, preparing the gel from the obtained product and an acid solution with a concentration of 32.5-33.5% at a pressure of 0.30-0.40 MPa and a temperature of 20-53 DEG C, and drying and screening the obtained gel, so that coarse-pore blocky gel disclosed by the invention can be obtained.
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 silicon-dioxide, is a kind of porous adsorbent of structure image cavernous body, can adsorbs aqueous vapor, water insoluble and other solvents, nonpoisonous and tasteless, stable chemical nature, Chang Zuowei siccative and sorbent material use, the model of silica gel is varied, the silica gel of different model because of its Production Flow Chart and preparation method difference and form different skeleton structures.Varying in size according to 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, adsorb the silica gel of moisture after being exposed to the sun and being air-dry, its adsorptive power reducible.
Silica gel is main raw material with silicate, a kind of porous mass generated after adopting suitable mol ratio to add mineral acid.Chinese patent CN1158310 utilizes silicate and mineral acid to produce aperture and the limited silica gel of pore volume, aperture silica gel directly joins in alkaline solution and prepares macroporous silica gel by Chinese patent CN0215935518, and high-purity silica gel is prepared in the silicate after Chinese patent CN200510117271.6 utilizes purifying and mineral acid effect; In these inventions, the involved silica gel made also exists the shortcomings such as the not strong and original high expensive of larger individual character difference, hole structural property index adaptability, be difficult to obtain the stable prod of constant mass, therefore, development has advanced technology of preparing and manufactures High performance silica gel, has become technical barrier urgently to be resolved hurrily.
Summary of the invention
To the shortcoming existed in above-mentioned art methods, the present invention proposes a kind of preparation method of thick-hole block silica gel.The method overcome prepared silica gel and there is the shortcomings such as individual character difference, hole structural property index adaptability are not strong, silica gel quality is unstable, the silica gel steady quality obtained, and cost is lower, time-consuming is shorter, its purity is greater than 99%, hole structural property index strong adaptability.
Raw material standard used herein requires low, to take high density, high-temperature quick adhesive-preparing technology and uniqueness continuously chemical removal of iron technology, adopt the continuous glue making machine of Creative Design and process matching voluntarily and wash desalting plant, thus ensure that the steady quality of silica gel, petrochemical industry and the fine chemicals industry such as catalyzer and support of the catalyst, matting agent, plastics opening agent can be widely used in.
The present invention adopts certain density sulfuric acid and water glass to be raw material, through strengthening reaction, generates silicon sol, then through aging condensation, washing desalination, ammonia treatment, drying and dehydrating and obtaining.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 unstable weak acid, intermolecularly carry out condensation, 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, raw material configures
This step is that water glass and the vitriol oil are mixed with suitable solution respectively, stand-by.
1) in raw material configuration flow, be first by sodium silicate solution purifying, filter out impurity, being added water by water glass and being adjusted to density is 1.01-1.50g/cm
3, its temperature condition is at 20-40 DEG C, and cleaning plate-and-frame filter press, squeezes into the sodium silicate solution pump allocated in plate-and-frame filter press and filter, and then flows into and filters alkali pond.When filtration velocity is very slow, shut down, cleaning filter cloth.Filter and terminate, sodium silicate solution is squeezed into storage alkali tank.
2), be less than the condition of 25 DEG C in temperature under, squeeze into alkali-prepared tank by the sodium silicate solution after filtration from storage alkali tank with pump, open pneumatic blending, add water adjustment concentration, makes SiO
2content is: 20 ~ 23%, and density is 1.28-1.34g/cm
3, stir, after time of repose is greater than 36 hours, sampling analysis, if the as clear as crystal inclusion-free of solution, through set aside for use after the assay was approved.
3), be less than the condition of 25 DEG C in temperature under, first add clear water by complex acid tank, open pneumatic blending, more slowly add the vitriol oil, regulate concentration, make it to reach 32.5-33.5%, stir, sampling analysis, if as clear as crystal inclusion-free, cools stand-by through after the assay was approved.
Second step, glue
By the pressure adjusting of reaction chamber to 0.30-0.40Mpa, temperature adjusts to 20-53 DEG C, deployed raw material is configured in reaction chamber respectively, detect the pH value of colloidal sol, make it in 1.5-2.5 scopes, fully reaction is fused after 32 hours, detects free acid, make its concentration in 0.4%-0.9% scope, adjustment pressure is to normal pressure.The silica gel obtained, after rubber cutting machine cutting, forms the blob of viscose of 3.5 centimetres.
3rd step, washing
Through 3-6 level washing series-connection process, every grade of water rinses, 30 centimetres, water surface height plastic emitting face, first grading hot water, water temperature 50 DEG C, 30 centimetres, water surface height plastic emitting face, if certain one-level water surface does not reach requirement, water valve at the corresponding levels is opened automatically, and after making it to meet the demands, water valve cuts out, 6th grade of sewer, detect the acid content of the 6th grade of silica gel, in glue during acid content PH>5.8, water is all sealed in next washing pool, operation is steeped 4 hours, the final blob of viscose forming pH value and be greater than 6.7 through ammonia.
Finally, through drying and after screening, just can obtaining gross porosity blob of viscose involved in the present invention.
The present invention is compared with traditional method, and it has the advantage of following four aspects:
(1) reaction conditions is gentle, easy and simple to handle;
(2) this preparation method is under the condition of low cost ingredient requirement, can obtain the thick-hole block silica gel that purity is greater than 99%;
(3) silica gel utilizing this preparation method to produce, its hole structural property index strong adaptability;
(4) adopt the continuous glue making machine of Creative Design and process matching voluntarily and wash desalting plant, thus ensure that the steady quality of silica gel.
Embodiment
Further illustrate 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 DEG C of temperature condition, this sodium silicate solution is squeezed in pressure filter and filters, keep 30 minutes, then squeeze into cleaning filter cloth filtration vessel in.
From filtration vessel, take out sodium silicate solution, import to and be equipped with in container, under 20 DEG C of temperature condition, add water adjustment concentration, surveys concentration while stirring, make SiO
2content is: 19.5%, and density is 1.28g/cm
3, stir, leave standstill 38 hours.
Under 20 DEG C of temperature condition, add clear water by complex acid container, slowly add the vitriol oil, regulate concentration, make it to reach 32.5%, stir stand-by.
Second step, glue
The pressure adjusting of small-sized reaction chamber to 0.30 Mpa, get 800ml concentration be 32.5% sulphuric acid soln slowly inject small-sized reaction chamber, slowly add the SiO be configured
2content is the sodium silicate solution of 19.5%, and pH value data are surveyed on mixing limit, limit, make it in 1.5-2.5 scopes, leave standstill fused be converted into silicic acid after, aging 32 hours, survey the free acid concentration in glue, make its concentration in 0.4%-0.7% scope, adjustment pressure, to normal pressure, increases pH value, carry out 3 grades of washing series-connection processes, chopped-off head water temperature 50 DEG C, in glue during acid content PH>5.8, ammonia bubble operation 4 hours, the blob of viscose that final formation pH value is greater than 6.7, SiO
2purity 99.2%.
Embodiment 2:
The first step, batching
Getting density is 1.1g/cm
3sodium silicate solution 3000ml, under 30 DEG C of temperature condition, this sodium silicate solution is squeezed in pressure filter and filters, keep 50 minutes, then squeeze into cleaning filter cloth filtration vessel in.
From filtration vessel, take out sodium silicate solution, import to and be equipped with in container, under 22 DEG C of temperature condition, add water adjustment concentration, surveys concentration while stirring, make SiO
2content is: 20.12%, stirs, and leaves standstill 36 hours.
Second step, glue
The pressure adjusting of small-sized reaction chamber to 0.35 Mpa, get 800ml concentration be 32.8% sulphuric acid soln slowly inject small-sized reaction chamber, slowly add the SiO be configured
2content is the sodium silicate solution of 20.12%, and pH value data are surveyed on mixing limit, limit, make it in 1.8-2.0 scopes, leave standstill fused be converted into silicic acid after, aging 32 hours, survey the free acid concentration in glue, make its concentration in 0.5-0.7% scope, adjustment pressure, to normal pressure, increases pH value, carry out 3 grades of washing series-connection processes, chopped-off head water temperature 55 DEG C, in glue during acid content PH>5.9, ammonia bubble operation 4 hours, the blob of viscose that final formation pH value is greater than 6.8, SiO
2purity 99.12%.
Embodiment 3:
The first step, batching
Getting density is 1.35g/ cm
3sodium silicate solution 3000ml, under 38 DEG C of temperature condition, this sodium silicate solution is squeezed in pressure filter and filters, keep 40 minutes, then squeeze into cleaning filter cloth filtration vessel in.
From filtration vessel, take out sodium silicate solution, import to and be equipped with in container, under 22 DEG C of temperature condition, add water adjustment concentration, surveys concentration while stirring, make SiO
2content is: 21.5%, stirs, and leaves standstill 36 hours.
Second step, glue
The pressure adjusting of small-sized reaction chamber to 0.35 Mpa, get 1000ml concentration be 33.0% sulphuric acid soln slowly inject small-sized reaction chamber, slowly add the SiO be configured
2content is the sodium silicate solution of 21.5%, and pH value data are surveyed on mixing limit, limit, make it in 1.9-2.5 scopes, leave standstill fused be converted into silicic acid after, aging 32 hours, survey the free acid concentration in glue, make its concentration in 0.6-0.8% scope, adjustment pressure, to normal pressure, increases pH value, carry out 4 grades of washing series-connection processes, chopped-off head water temperature 54 DEG C, in glue during acid content PH>6.0, ammonia bubble operation 4 hours, the blob of viscose that final formation pH value is greater than 6.8, SiO
2purity 99.33%.
Embodiment 4:
The first step, batching
Getting density is 1.40g/ cm
3sodium silicate solution 3000ml, under 39 DEG C of temperature condition, this sodium silicate solution is squeezed in pressure filter and filters, keep 50 minutes, then squeeze into cleaning filter cloth filtration vessel in.
From filtration vessel, take out sodium silicate solution, import to and be equipped with in container, under 24 DEG C of temperature condition, add water adjustment concentration, surveys concentration while stirring, make SiO
2content is 22%, stirs, and leaves standstill 38 hours.
Second step, glue
The pressure adjusting of small-sized reaction chamber to 0.38 Mpa, get 1000ml concentration be 33.5% sulphuric acid soln slowly inject small-sized reaction chamber, slowly add the SiO be configured
2content is the sodium silicate solution of 22%, and pH value data are surveyed on mixing limit, limit, make it in 1.5 – 1.9 scopes, leave standstill fused be converted into silicic acid after, aging 32 hours, survey the free acid concentration in glue, make its concentration in 0.4-0.7% scope, adjustment pressure, to normal pressure, increases pH value, carry out 3 grades of washing series-connection processes, chopped-off head water temperature 36 DEG C, in glue during acid content PH>5.6, ammonia bubble operation 4 hours, the blob of viscose that final formation pH value is greater than 6.5, SiO
2purity 99.15%.
Embodiment 5:
The first step, batching
Getting density is 1.50g/ cm
3sodium silicate solution 3000ml, under 25 DEG C of temperature condition, this sodium silicate solution is squeezed in pressure filter and filters, keep 50 minutes, then squeeze into cleaning filter cloth filtration vessel in.
From filtration vessel, take out sodium silicate solution, import to and be equipped with in container, under 24 DEG C of temperature condition, add water adjustment concentration, surveys concentration while stirring, make SiO
2content is 22.32%, stirs, and leaves standstill 38 hours.
Second step, glue
The pressure adjusting of small-sized reaction chamber to 0.38 Mpa, get 1000ml concentration be 33.5% sulphuric acid soln slowly inject small-sized reaction chamber, slowly add the SiO be configured
2content is the sodium silicate solution of 22.32%, and pH value data are surveyed on mixing limit, limit, make it in 1.5 – 1.7 scopes, leave standstill fused be converted into silicic acid after, aging 32 hours, survey the free acid concentration in glue, make its concentration in 0.5-0.8% scope, adjustment pressure, to normal pressure, increases pH value, carry out 3 grades of washing series-connection processes, chopped-off head water temperature 40 DEG C, in glue during acid content PH>5.8, ammonia bubble operation 4 hours, the blob of viscose that final formation pH value is greater than 6.8, SiO
2purity 99.23%.
Claims (6)
1. the preparation method of a thick-hole block silica gel, it adopts sulfuric acid and water glass to be raw material, after Impurity removal, through strengthening reaction in reaction chamber, generate silica gel, then through aging condensation, washing desalination, ammonia treatment, the steps such as drying and dehydrating and obtained 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, prepares that purity is 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: the set aside for use when concentration of described sulfuric acid 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 when 20-40 DEG C.
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 reaches 20 ~ 23%, density reaches 1.28-1.34g/cm
3time 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 DEG C.
6. the preparation method of thick-hole block silica gel according to claim 1, is characterized in that: the silica gel pH value after described washing desalting steps is greater than 5.8.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112717874A (en) * | 2020-12-08 | 2021-04-30 | 福建南平三元循环技术有限公司 | Novel reaming manufacturing method of macroporous silica gel |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112717874A (en) * | 2020-12-08 | 2021-04-30 | 福建南平三元循环技术有限公司 | Novel reaming manufacturing method of macroporous silica gel |
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Application publication date: 20141224 |