CN111634917A - Preparation method of porous active silica gel - Google Patents
Preparation method of porous active silica gel Download PDFInfo
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- CN111634917A CN111634917A CN202010464611.7A CN202010464611A CN111634917A CN 111634917 A CN111634917 A CN 111634917A CN 202010464611 A CN202010464611 A CN 202010464611A CN 111634917 A CN111634917 A CN 111634917A
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- Prior art keywords
- solution
- gel
- silica gel
- magnesium oxide
- raw materials
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 23
- 239000000741 silica gel Substances 0.000 title claims abstract description 23
- 239000000499 gel Substances 0.000 claims abstract description 35
- 239000002994 raw material Substances 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 16
- 238000001354 calcination Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 12
- 238000012545 processing Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 51
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 27
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 27
- 239000000395 magnesium oxide Substances 0.000 claims description 27
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 27
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 27
- 239000011259 mixed solution Substances 0.000 claims description 24
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 22
- 239000001110 calcium chloride Substances 0.000 claims description 13
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 12
- 239000004094 surface-active agent Substances 0.000 claims description 12
- 235000019270 ammonium chloride Nutrition 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000004115 Sodium Silicate Substances 0.000 claims description 8
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 8
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 7
- 239000000428 dust Substances 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 239000007800 oxidant agent Substances 0.000 claims description 4
- 239000002244 precipitate Substances 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 4
- 230000035515 penetration Effects 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 2
- 238000001879 gelation Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 238000010586 diagram Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910002028 silica xerogel Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Classifications
-
- 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
Abstract
The invention discloses a preparation method of porous active silica gel, which comprises the following steps: the preparation method comprises the steps of material preparation, gelation, gel washing processing and drying and calcination, wherein sufficient basic raw materials and related solutions are selected, solid raw materials are selected and mixed with deionized water to obtain corresponding standby solutions, the raw materials and the solutions are mixed, gel is prepared through heating and multi-round stirring, deionized water is added into the gel for gel washing processing, and finally the porous active silica gel is obtained through drying and calcination processing. According to the preparation method of the porous active silica gel, sufficient raw materials for silica gel production are prepared, then the standby solution is prepared by adopting accurate proportioning, all the raw materials are fully reacted by heating and multi-round stirring to prepare the gel, the silica gel is prepared by washing, processing, drying and calcining, and the prepared silica gel is the porous active silica gel, so that the preparation method is more accurate and clear.
Description
Technical Field
The invention relates to the field of silica gel, and particularly relates to a preparation method of porous active silica gel.
Background
The silica gel is a silica xerogel with a two-dimensional space network structure, belongs to a porous solid substance, has wide pore distribution range, large specific surface and certain activity, and is widely applied to industrial production.
Disclosure of Invention
The invention mainly aims to provide a preparation method of porous active silica gel, which can effectively solve the problems in the background art.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of porous active silica gel comprises the following steps:
s1, in the material preparation stage, selecting sufficient solid raw materials of magnesium oxide, cobalt chloride and calcium chloride and deionized water, and then preparing 3-5 parts of surfactant, 20-25 parts of absolute ethyl alcohol, 18-22 parts of sodium silicate and 30-40 parts of ammonium chloride solution according to parts by weight;
s2, in the material preparation stage, firstly, grinding and processing raw materials of magnesium oxide, cobalt chloride and calcium chloride, then sieving the raw materials, respectively mixing powdery raw materials of magnesium oxide, cobalt chloride and calcium chloride with deionized water to prepare corresponding magnesium oxide solution, cobalt chloride solution and calcium chloride solution, wherein the corresponding parts of the magnesium oxide solution, the cobalt chloride solution and the calcium chloride solution are 3:4:3, and then mixing the prepared surface oxidizing agent and the deionized water to prepare 0.1mol/L surfactant solution;
s3, a gelling stage, namely mixing prepared absolute ethyl alcohol with a surfactant solution, adding sodium silicate into the mixed solution, stirring the mixed material for 10-15min in a first round, heating the mixed solution in a water bath at the temperature of 40-50 ℃, adding a prepared ammonium chloride solution into the mixed solution at the ammonium chloride solution adding rate of 1.5ml/min, adding a magnesium oxide solution into the mixed solution, stirring in a second round for 40min, sequentially adding a cobalt chloride solution and a calcium chloride solution into the mixed solution, stirring in a third round, and controlling the duration of the stirring in the third round to be 25-30min, so as to obtain gel;
s4, a step of washing gel, in which deionized water is added into the prepared gel for washing for 30-40min until the supernatant in the gel reaches a clear state;
and S5, drying and calcining, namely placing the gel into a vacuum drier for drying and processing, and then placing the gel into a muffle furnace at 500 ℃ for calcining to obtain the porous active silica gel.
Preferably, the standby material in step S1 should be in a ventilated and dry environment, and should be insulated from dust penetration, direct sunlight and away from the heat source.
Preferably, when the ground raw materials of magnesium oxide, cobalt chloride and calcium chloride are sieved in the step S2, a 200-mesh sieve is selected for sieving, and the concentrations of the prepared magnesium oxide solution, cobalt chloride solution and calcium chloride solution are all 1 mol/L.
Preferably, the first round of agitation in the step S3 is performed without visible precipitates in the mixed solution.
Preferably, the vacuum drying time in the S5 step is 3-4h, and the calcination time of the gel in a muffle furnace is 1 h.
Compared with the prior art, according to the preparation method of the porous active silica gel, sufficient raw materials are selected, the raw materials are guaranteed to be in a dry and ventilated environment, direct irradiation of sunlight and heat source away are avoided, the stability of the materials is guaranteed, the corresponding standby solution is prepared and is stirred and mixed according to a certain proportion, the accuracy of the components of the mixed solution is improved, the mixed solution is processed into gel through temperature rise and multi-round stirring, the quality of the gel is improved, and the drying and calcining time and temperature are accurately controlled through gel washing, so that the forming quality of the silica gel is improved.
Drawings
FIG. 1 is a flow chart of the preparation process of a porous activated silica gel according to the present invention;
FIG. 2 is a schematic diagram of a material preparation stage of a method for preparing porous reactive silica gel according to the present invention;
FIG. 3 is a schematic diagram of a material preparation stage of a method for preparing porous activated silica gel according to the present invention;
FIG. 4 is a schematic diagram of a gel stage structure of a method for preparing porous activated silica gel according to the present invention;
FIG. 5 is a schematic structural diagram of a washing step of a porous reactive silica gel preparation method of the present invention;
FIG. 6 is a schematic diagram of the structure of the drying and calcining stage of the preparation method of porous activated silica gel of the present invention.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "front", "rear", "both ends", "one end", "the other end", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "disposed," "connected," and the like are to be construed broadly, such as "connected," which may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
As shown in fig. 1-6, a method for preparing porous activated silica gel comprises the following steps:
s1, in the material preparation stage, selecting sufficient solid raw materials of magnesium oxide, cobalt chloride and calcium chloride and deionized water, and then preparing 3-5 parts of surfactant, 20-25 parts of absolute ethyl alcohol, 18-22 parts of sodium silicate and 30-40 parts of ammonium chloride solution according to parts by weight;
s2, in the material preparation stage, firstly, grinding and processing raw materials of magnesium oxide, cobalt chloride and calcium chloride, then sieving the raw materials, respectively mixing powdery raw materials of magnesium oxide, cobalt chloride and calcium chloride with deionized water to prepare corresponding magnesium oxide solution, cobalt chloride solution and calcium chloride solution, wherein the corresponding parts of the magnesium oxide solution, the cobalt chloride solution and the calcium chloride solution are 3:4:3, and then mixing the prepared surface oxidizing agent and the deionized water to prepare 0.1mol/L surfactant solution;
s3, a gelling stage, namely mixing prepared absolute ethyl alcohol with a surfactant solution, adding sodium silicate into the mixed solution, stirring the mixed material for 10-15min in a first round, heating the mixed solution in a water bath at the temperature of 40-50 ℃, adding a prepared ammonium chloride solution into the mixed solution at the ammonium chloride solution adding rate of 1.5ml/min, adding a magnesium oxide solution into the mixed solution, stirring in a second round for 40min, sequentially adding a cobalt chloride solution and a calcium chloride solution into the mixed solution, stirring in a third round, and controlling the duration of the stirring in the third round to be 25-30min, so as to obtain gel;
s4, a step of washing gel, in which deionized water is added into the prepared gel for washing for 30-40min until the supernatant in the gel reaches a clear state;
and S5, drying and calcining, namely placing the gel into a vacuum drier for drying and processing, and then placing the gel into a muffle furnace at 500 ℃ for calcining to obtain the porous active silica gel.
The standby material in the step S1 should be in a ventilated and dry environment, and should be isolated from dust penetration, so as to prevent direct sunlight and keep away from a heat source; when the ground magnesium oxide, cobalt chloride and calcium chloride raw materials are sieved in the step S2, a 200-mesh sieve is selected for sieving operation, and the concentrations of the prepared magnesium oxide solution, cobalt chloride solution and calcium chloride solution are all 1 mol/L; no visible precipitate is needed in the mixed solution after the first round of stirring in the step S3; the vacuum drying time in the S5 step is 3-4h, and the calcination time of the gel in a muffle furnace is 1 h.
The preparation method comprises the steps of preparing 3-5 parts of surfactant, 20-25 parts of absolute ethyl alcohol, 18-22 parts of sodium silicate and 30-40 parts of ammonium chloride solution, selecting sufficient magnesium oxide, cobalt chloride and calcium chloride raw materials, grinding the raw materials to obtain fine raw materials, sieving the fine raw materials by a 200-mesh sieve to obtain powdery raw materials, mixing the raw materials with deionized water respectively to obtain corresponding magnesium oxide solution, cobalt chloride solution and calcium chloride solution, mixing a surface oxidant with the deionized water to obtain surfactant solution, placing all the raw materials in a dry and ventilated environment, preparing anti-dust equipment such as a mask by operators, mixing the prepared absolute ethyl alcohol with the surfactant solution, adding the sodium silicate into the mixed solution, stirring the mixed solution for 12min until no visible precipitate exists in the solution, heating the solution in water bath to 50 ℃, adding ammonium chloride solution into the mixed solution at a rate of 1.5ml/min, adding magnesium oxide solution into the mixed solution, stirring for 40min for a second time, sequentially adding cobalt chloride solution and calcium chloride solution into the solution, stirring for 30min for a third time to obtain gel, adding deionized water into the prepared gel for washing for 35min until supernatant in the gel reaches a clear state, drying the gel in a vacuum dryer for 3h, calcining the gel in a muffle furnace at a temperature of 500 ℃, thereby preparing the porous active silica gel with excellent quality.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (5)
1. A preparation method of porous active silica gel is characterized in that: the method comprises the following steps:
s1, in the material preparation stage, selecting sufficient solid raw materials of magnesium oxide, cobalt chloride and calcium chloride and deionized water, and then preparing 3-5 parts of surfactant, 20-25 parts of absolute ethyl alcohol, 18-22 parts of sodium silicate and 30-40 parts of ammonium chloride solution according to parts by weight;
s2, in the material preparation stage, firstly, grinding and processing raw materials of magnesium oxide, cobalt chloride and calcium chloride, then sieving, then respectively mixing powdery raw materials of magnesium oxide, cobalt chloride and calcium chloride with deionized water to prepare corresponding magnesium oxide solution, cobalt chloride solution and calcium chloride solution, wherein the corresponding parts of the magnesium oxide solution, the cobalt chloride solution and the calcium chloride solution are 3:4:3, and then mixing the prepared surface oxidizing agent and the deionized water to prepare 0.1mol/L surfactant solution;
s3, a gelling stage, namely mixing prepared absolute ethyl alcohol with a surfactant solution, adding sodium silicate into the mixed solution, stirring the mixed material for 10-15min in a first round, heating the mixed solution in a water bath at the temperature of 40-50 ℃, adding a prepared ammonium chloride solution into the mixed solution at the ammonium chloride solution adding rate of 1.5ml/min, adding a magnesium oxide solution into the mixed solution, stirring in a second round for 40min, sequentially adding a cobalt chloride solution and a calcium chloride solution into the mixed solution, stirring in a third round, and controlling the duration of the stirring in the third round to be 25-30min, so as to obtain gel;
s4, a step of washing gel, in which deionized water is added into the prepared gel for washing for 30-40min until the supernatant in the gel reaches a clear state;
and S5, drying and calcining, namely placing the gel into a vacuum drier for drying and processing, and then placing the gel into a muffle furnace at 500 ℃ for calcining to obtain the porous active silica gel.
2. The method for preparing porous activated silica gel according to claim 1, wherein: the standby material in step S1 should be in a ventilated and dry environment, and should be protected from dust penetration, direct sunlight and away from the heat source.
3. The method for preparing porous activated silica gel according to claim 1, wherein: when the ground raw materials of magnesium oxide, cobalt chloride and calcium chloride are sieved in the step S2, a 200-mesh sieve is selected for sieving, and the concentrations of the prepared magnesium oxide solution, cobalt chloride solution and calcium chloride solution are all 1 mol/L.
4. The method for preparing porous activated silica gel according to claim 1, wherein: no visible precipitate was required in the mixed solution after the first round of agitation in the S3 step.
5. The method for preparing porous activated silica gel according to claim 1, wherein: the vacuum drying time in the S5 step is 3-4h, and the calcination time of the gel in a muffle furnace is 1 h.
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| CN202010464611.7A CN111634917A (en) | 2020-05-27 | 2020-05-27 | Preparation method of porous active silica gel |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112680049A (en) * | 2020-12-31 | 2021-04-20 | 滁州圣好材料科技有限公司 | High-weather-resistance anti-contamination siliceous real stone paint and preparation method thereof |
| CN113174232A (en) * | 2021-04-23 | 2021-07-27 | 深圳市红叶杰科技有限公司 | Heat-conducting and heat-storing multifunctional encapsulating silica gel and preparation method thereof |
| CN114835466A (en) * | 2022-05-16 | 2022-08-02 | 宿迁市日茂新材料有限公司 | Novel graphite antistatic silica gel surface |
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| CN1437563A (en) * | 2000-06-26 | 2003-08-20 | 旭化成株式会社 | Porous, fine inorganic particles |
| US20170081205A1 (en) * | 2014-04-10 | 2017-03-23 | Karnalyte Resources Inc. | Process for producing high grade hydromagnesite and magnesium oxide |
| US20180029022A1 (en) * | 2015-02-04 | 2018-02-01 | Pc-Cups Ltd. | Metallo-silicate catalyst (msc) compositions, methods of preparation and methods of use in partial upgrading of hydrocarbon feedstocks |
| CN108654569A (en) * | 2018-03-23 | 2018-10-16 | 长沙小新新能源科技有限公司 | A kind of porous active silica gel preparation method |
-
2020
- 2020-05-27 CN CN202010464611.7A patent/CN111634917A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1437563A (en) * | 2000-06-26 | 2003-08-20 | 旭化成株式会社 | Porous, fine inorganic particles |
| US20170081205A1 (en) * | 2014-04-10 | 2017-03-23 | Karnalyte Resources Inc. | Process for producing high grade hydromagnesite and magnesium oxide |
| US20180029022A1 (en) * | 2015-02-04 | 2018-02-01 | Pc-Cups Ltd. | Metallo-silicate catalyst (msc) compositions, methods of preparation and methods of use in partial upgrading of hydrocarbon feedstocks |
| CN108654569A (en) * | 2018-03-23 | 2018-10-16 | 长沙小新新能源科技有限公司 | A kind of porous active silica gel preparation method |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112680049A (en) * | 2020-12-31 | 2021-04-20 | 滁州圣好材料科技有限公司 | High-weather-resistance anti-contamination siliceous real stone paint and preparation method thereof |
| CN113174232A (en) * | 2021-04-23 | 2021-07-27 | 深圳市红叶杰科技有限公司 | Heat-conducting and heat-storing multifunctional encapsulating silica gel and preparation method thereof |
| CN114835466A (en) * | 2022-05-16 | 2022-08-02 | 宿迁市日茂新材料有限公司 | Novel graphite antistatic silica gel surface |
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Application publication date: 20200908 |