CN114768748A - Preparation method of all-silicon micro-mesoporous composite molecular sieve VOCs adsorbent - Google Patents
Preparation method of all-silicon micro-mesoporous composite molecular sieve VOCs adsorbent Download PDFInfo
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- CN114768748A CN114768748A CN202210429473.8A CN202210429473A CN114768748A CN 114768748 A CN114768748 A CN 114768748A CN 202210429473 A CN202210429473 A CN 202210429473A CN 114768748 A CN114768748 A CN 114768748A
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- 239000002808 molecular sieve Substances 0.000 title claims abstract description 38
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 38
- 239000010703 silicon Substances 0.000 title claims abstract description 38
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 239000003463 adsorbent Substances 0.000 title claims abstract description 31
- 239000012855 volatile organic compound Substances 0.000 title claims abstract description 29
- 239000002131 composite material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 36
- 238000002425 crystallisation Methods 0.000 claims abstract description 31
- 230000008025 crystallization Effects 0.000 claims abstract description 31
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000013078 crystal Substances 0.000 claims abstract description 16
- 238000001914 filtration Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 8
- BGQMOFGZRJUORO-UHFFFAOYSA-M tetrapropylammonium bromide Chemical compound [Br-].CCC[N+](CCC)(CCC)CCC BGQMOFGZRJUORO-UHFFFAOYSA-M 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 12
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 3
- 239000004115 Sodium Silicate Substances 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 13
- 238000009826 distribution Methods 0.000 abstract description 4
- 238000011049 filling Methods 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 5
- 239000005416 organic matter Substances 0.000 description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0251—Compounds of Si, Ge, Sn, Pb
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28078—Pore diameter
- B01J20/28083—Pore diameter being in the range 2-50 nm, i.e. mesopores
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/708—Volatile organic compounds V.O.C.'s
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The embodiment of the invention provides a preparation method of an all-silicon micro-mesoporous composite molecular sieve VOCs adsorbent, belonging to the technical field of adsorbent preparation. The preparation method comprises the following steps: dissolving hexadecyl trimethyl ammonium bromide in water, adding sodium hydroxide to adjust the pH value, gradually adding a silicon source at a certain temperature, then carrying out ultrasonic crystallization for a certain time, and filtering to obtain an MCM-41 crystal cluster; dissolving tetrapropylammonium bromide in water, adding the MCM-41 crystal cluster, adding sodium hydroxide to adjust the pH value, gradually adding a silicon source at a certain temperature, and then carrying out ultrasonic crystallization for a certain time; and (3) filling the crystallization liquid into a crystallization kettle, continuously crystallizing for a certain time at a certain temperature, and filtering, washing, drying and roasting to obtain the all-silicon micro-mesoporous composite molecular sieve VOCs adsorbent. The invention can enlarge the distribution range of the molecular sieve aperture, thereby having good adsorption capacity to macromolecular organic matters.
Description
Technical Field
The invention relates to the technical field of adsorbent preparation, in particular to a preparation method of a full-silicon micro-mesoporous composite molecular sieve VOCs adsorbent.
Background
With the increasingly outstanding environmental pollution problems and the increasing environmental protection requirements, especially with the increasing pollution problems such as haze in recent years, the requirements for emissions polluted by VOCs (Volatile Organic Compounds) are becoming more and more strict. Among numerous VOCs treatment processes, the adsorption method is favored because of simple operation, safe process and high treatment efficiency, and is particularly widely applied under the working condition of large air volume and low concentration. The key to the adsorption process is the adsorbent for VOCs, and the adsorbent for VOCs with large capacity has been the focus of attention in the industry.
The molecular sieve has the advantages of large specific surface area, pore volume, pore diameter and the like, so that the molecular sieve is widely applied to the fields of adsorption separation and the like. Wherein, due to the limitation of the self aperture of the microporous molecular sieve, when some macromolecular organic matters are adsorbed, the organic matter molecules cannot be trapped because the organic matter molecules cannot enter the microporous pore channels of the microporous molecular sieve, so that the actual application of the microporous molecular sieve is limited to a certain extent.
Disclosure of Invention
The embodiment of the invention aims to provide a preparation method of an all-silicon micro-mesoporous composite molecular sieve VOCs adsorbent, which can expand the pore size distribution range of a molecular sieve, thereby having good adsorption capacity on macromolecular organic matters.
The preparation method of the all-silicon micro-dielectric composite molecular sieve VOCs adsorbent provided by the embodiment of the invention comprises the following steps:
s10: dissolving cetyl trimethyl ammonium bromide in water, adding sodium hydroxide to adjust the pH value, gradually adding a silicon source at a certain temperature, then carrying out ultrasonic crystallization for a certain time, and filtering to obtain MCM-41 crystal clusters;
s20: dissolving tetrapropylammonium bromide in water, adding the MCM-41 crystal cluster, adding sodium hydroxide to adjust the pH value, gradually adding a silicon source at a certain temperature, and then carrying out ultrasonic crystallization for a certain time;
s30: and (3) filling the crystallization liquid into a crystallization kettle, continuously crystallizing for a certain time at a certain temperature, and filtering, washing, drying and roasting to obtain the all-silicon micro-mesoporous composite molecular sieve VOCs adsorbent.
Preferably, in the S10, the temperature for adding the silicon source is 40-70 ℃, and the ultrasonic crystallization time is 0.5-2 h.
Preferably, in the step S20, the temperature for adding the silicon source is 20-50 ℃, and the ultrasonic crystallization time is 10-30 min.
Preferably, in both S10 and S20, the pH is adjusted to 10-12.
Preferably, in the S30, the crystallization temperature is 150-180 ℃, and the crystallization time is 12-36 h.
Preferably, the silicon source is one of normal ethyl acetate, silica sol, sodium silicate and silicon dioxide.
Preferably, the silicon source, the hexadecyl trimethyl ammonium bromide and the tetrapropyl ammonium bromide correspond to molar ratios of (1: 0.1) - (0.2: 0.15) - (0.25), respectively.
The invention has the beneficial effects that:
according to the preparation method of the all-silicon micro-dielectric composite molecular sieve VOCs adsorbent provided by the embodiment of the invention, the MCM-41 crystal cluster is prepared firstly, then the MCM-41 crystal cluster is added in the process of synthesizing the composite molecular sieve VOCs adsorbent, and a silicon source is added to carry out ultrasonic crystallization, so that the pore size distribution range of the molecular sieve is expanded, and the molecular sieve has good adsorption capacity on macromolecular organic matters.
In order to make the aforementioned and other objects, features and advantages of the present invention comprehensible, preferred embodiments accompanied with figures are described in detail below.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without inventive efforts based on the embodiments of the present invention, are within the scope of protection of the present invention. Thus, the following detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention.
The terms "first", "second", and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
Example 1
The embodiment of the invention provides a preparation method of a full-silicon micro-dielectric composite molecular sieve VOCs adsorbent, which mainly comprises the following steps:
step S10: 5g of hexadecyl trimethyl ammonium bromide is dissolved in 50mL of water, 2.4g of sodium hydroxide is added, 10mL of ethyl orthosilicate is gradually added at 50 ℃, then ultrasonic crystallization is carried out for 1h, and MCM-41 crystal cluster is obtained by filtration.
Step S20: dissolving 5g of tetrapropylammonium bromide in 50mL of water, adding the MCM-41 crystal cluster obtained in the step S10, adding 0.4g of sodium hydroxide, gradually adding 10mL of tetraethoxysilane at the temperature of 20 ℃, and then carrying out ultrasonic crystallization for 30 min.
Step S30: and (3) putting the crystallized liquid into a crystallization kettle, continuously crystallizing for 24 hours at 160 ℃, and filtering, washing, drying and roasting for 5 hours at 550 ℃ to obtain the all-silicon micro-mesoporous composite molecular sieve VOCs adsorbent.
Example 2
The preparation method of the all-silicon micro-dielectric composite molecular sieve VOCs adsorbent provided by the embodiment of the invention mainly comprises the following steps:
step S10: 5g of hexadecyl trimethyl ammonium bromide is dissolved in 20mL of water, 2.4g of sodium hydroxide is added, 30g of silica sol is gradually added at 50 ℃, then ultrasonic crystallization is carried out for 1h, and MCM-41 crystal clusters are obtained by filtration.
Step S20: dissolving 5g of tetrapropylammonium bromide in 20mL of water, adding the MCM-41 crystal cluster obtained in the first step, adding 0.4g of sodium hydroxide, gradually adding 30g of tetraethoxysilane at the temperature of 20 ℃, and then carrying out ultrasonic crystallization for 30 min.
Step S30: and (3) putting the crystallized liquid into a crystallization kettle, continuously crystallizing for 24 hours at 160 ℃, and filtering, washing, drying and roasting for 5 hours at 550 ℃ to obtain the all-silicon micro-mesoporous composite molecular sieve VOCs adsorbent.
Example 3
The embodiment of the invention provides a preparation method of a full-silicon micro-dielectric composite molecular sieve VOCs adsorbent, which mainly comprises the following steps:
step S10: 5g of hexadecyl trimethyl ammonium bromide is dissolved in 20mL of water, 2g of sodium hydroxide is added, 10mL of tetraethoxysilane is gradually added at 70 ℃, then ultrasonic crystallization is carried out for 0.5h, and MCM-41 crystal cluster is obtained by filtration.
Step S20: dissolving 5g of tetrapropylammonium bromide in 50mL of water, adding the MCM-41 crystal cluster obtained in the first step, adding 0.5g of sodium hydroxide, gradually adding 10mL of tetraethoxysilane at 50 ℃, and then carrying out ultrasonic crystallization for 30 min.
Step S30: and (3) putting the crystallized liquid into a crystallization kettle, continuously crystallizing for 12 hours at 160 ℃, and filtering, washing, drying and roasting for 5 hours at 550 ℃ to obtain the all-silicon micro-mesoporous composite molecular sieve VOCs adsorbent.
Comparative example
The microporous molecular sieve S-1 adsorbent and the composite molecular sieve adsorbent prepared in examples 1-3 above were subjected to organic matter adsorption performance tests. Each sample was crushed after being tableted, and 60 to 80 mesh powder was charged into a fixed bed reaction tube to test the dynamic adsorption performance.
The raw material gas is air with the concentration of organic matters of 300ppm, the organic matters are a mixture of ethyl acetate (50%) and dimethylbenzene (50%), and the test space velocity is 50000h-1The pressure is normal pressure, and the test is stopped when the purification efficiency is reduced to 90%.
The results of the adsorption performance test are shown in table 1.
TABLE 1
| Adsorbent and method of making same | Adsorption time | Adsorption capacity |
| Example 1 | 97min | 167mg/g |
| Example 2 | 81min | 140mg/g |
| Example 3 | 88min | 152mg/g |
| S-1 | 52min | 95mg/g |
As can be seen from the above table, the all-silicon micro-mesoporous composite molecular sieve VOCs adsorbent prepared in the embodiment of the present invention has a better adsorption capacity for macromolecular organic substances.
In summary, according to the preparation method of the all-silicon micro-dielectric composite molecular sieve VOCs adsorbent provided by the embodiment of the invention, the MCM-41 crystal cluster is prepared firstly, then the MCM-41 crystal cluster is added in the process of synthesizing the composite molecular sieve VOCs adsorbent, and the silicon source is added for ultrasonic crystallization, so that the pore size distribution range of the molecular sieve is expanded, and the molecular sieve has good adsorption capacity on macromolecular organic matters.
In addition, the embodiment of the invention utilizes the cavitation and mechanical effect of the ultrasonic to ensure that the molecular sieve nano-crystalline clusters are more uniform, and can effectively reduce the crystallization time.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A preparation method of an all-silicon micro-mesoporous composite molecular sieve VOCs adsorbent is characterized by comprising the following steps:
s10: dissolving hexadecyl trimethyl ammonium bromide in water, adding sodium hydroxide to adjust the pH value, gradually adding a silicon source at a certain temperature, then carrying out ultrasonic crystallization for a certain time, and filtering to obtain an MCM-41 crystal cluster;
s20: dissolving tetrapropylammonium bromide in water, adding the MCM-41 crystal cluster, adding sodium hydroxide to adjust the pH value, gradually adding a silicon source at a certain temperature, and then carrying out ultrasonic crystallization for a certain time;
s30: and (3) putting the crystallized liquid into a crystallization kettle, continuously crystallizing for a certain time at a certain temperature, and filtering, washing, drying and roasting to obtain the all-silicon micro-mesoporous composite molecular sieve VOCs adsorbent.
2. The method for preparing all-silicon micro-mesoporous composite molecular sieve VOCs adsorbents according to claim 1, wherein a silicon source is added into S10 at a temperature of 40-70 ℃ for an ultrasonic crystallization time of 0.5-2 h.
3. The method for preparing all-silicon micro-mesoporous composite molecular sieve VOCs adsorbents according to claim 1, wherein a silicon source is added into S20 at a temperature of 20-50 ℃ for 10-30min by ultrasonic crystallization.
4. The method for preparing all-silicon micro-mesoporous composite molecular sieve VOCs adsorbent according to claim 1, wherein the pH is adjusted to 10-12 in both S10 and S20.
5. The method as claimed in claim 1, wherein the crystallization temperature of S30 is 150-180 ℃ and the crystallization time is 12-36 h.
6. The method according to claim 1, wherein the silicon source is one of normal ethyl acetate, silica sol, sodium silicate, and silica.
7. The method of claim 1, wherein the molar ratio of the silicon source to cetyltrimethylammonium bromide to tetrapropylammonium bromide is (1: 0.1) - (0.2: 0.15) - (0.25), respectively.
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| CN202210429473.8A CN114768748A (en) | 2022-04-22 | 2022-04-22 | Preparation method of all-silicon micro-mesoporous composite molecular sieve VOCs adsorbent |
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