CN111871464A - Synthesis method of MIL-53(Cr) photocatalyst - Google Patents
Synthesis method of MIL-53(Cr) photocatalyst Download PDFInfo
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- CN111871464A CN111871464A CN202010780733.7A CN202010780733A CN111871464A CN 111871464 A CN111871464 A CN 111871464A CN 202010780733 A CN202010780733 A CN 202010780733A CN 111871464 A CN111871464 A CN 111871464A
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 57
- 239000013206 MIL-53 Substances 0.000 title claims abstract description 47
- 238000001308 synthesis method Methods 0.000 title claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 35
- 239000002994 raw material Substances 0.000 claims abstract description 32
- 238000010438 heat treatment Methods 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 239000000126 substance Substances 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 11
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 10
- 238000000227 grinding Methods 0.000 claims abstract description 9
- 239000010453 quartz Substances 0.000 claims abstract description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 239000011651 chromium Substances 0.000 claims description 46
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 16
- 230000002194 synthesizing effect Effects 0.000 claims description 16
- 238000005485 electric heating Methods 0.000 claims description 13
- GVHCUJZTWMCYJM-UHFFFAOYSA-N chromium(3+);trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GVHCUJZTWMCYJM-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 230000035484 reaction time Effects 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 9
- 230000015572 biosynthetic process Effects 0.000 abstract description 8
- 238000007789 sealing Methods 0.000 description 24
- 239000000463 material Substances 0.000 description 10
- 230000006835 compression Effects 0.000 description 5
- 238000007906 compression Methods 0.000 description 5
- 238000013016 damping Methods 0.000 description 5
- 239000004519 grease Substances 0.000 description 4
- 229920001296 polysiloxane Polymers 0.000 description 4
- 239000000565 sealant Substances 0.000 description 4
- 241000894006 Bacteria Species 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000013087 chromium-based metal-organic framework Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 241000233866 Fungi Species 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/22—Organic complexes
- B01J31/2204—Organic complexes the ligands containing oxygen or sulfur as complexing atoms
- B01J31/2208—Oxygen, e.g. acetylacetonates
- B01J31/2226—Anionic ligands, i.e. the overall ligand carries at least one formal negative charge
- B01J31/223—At least two oxygen atoms present in one at least bidentate or bridging ligand
- B01J31/2239—Bridging ligands, e.g. OAc in Cr2(OAc)4, Pt4(OAc)8 or dicarboxylate ligands
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/1691—Coordination polymers, e.g. metal-organic frameworks [MOF]
-
- B01J35/39—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/04—Mixing
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
-
- 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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/02—Compositional aspects of complexes used, e.g. polynuclearity
- B01J2531/0213—Complexes without C-metal linkages
-
- 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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/60—Complexes comprising metals of Group VI (VIA or VIB) as the central metal
- B01J2531/62—Chromium
Abstract
The invention relates to the technical field of synthesis, in particular to a synthesis method of an MIL-53(Cr) photocatalyst, which comprises the following steps: s1, taking a proper amount of raw materials according to the mixture ratio. S2, placing the raw materials in a synthesizer, and stirring by a stirring paddle; then, an appropriate amount of hydrofluoric acid (40% HF) was added and the stirring was continued. S3, the synthesizer is heated by the heating wire. And S4, cooling the substance obtained after the reaction in the synthesizer, and drying and grinding the substance. S5, placing the obtained substance in a quartz tube for calcination.
Description
Technical Field
The invention relates to the technical field of synthesis of photocatalysts, in particular to a synthesis method of an MIL-53(Cr) photocatalyst.
Background
The photocatalyst is a generic name for a material having a photocatalytic function. Substances which are capable of generating strong oxidizing properties under irradiation with light (e.g., hydroxyl radicals, oxygen, etc.) and are useful for decomposing organic compounds, partially inorganic compounds, bacteria, viruses, etc. The photocatalyst can effectively degrade toxic and harmful gases in the air, such as formaldehyde and the like, and efficiently purify the air; meanwhile, various bacteria can be effectively killed, and toxin released by the bacteria or fungi can be decomposed and harmlessly treated.
Based on the characteristics of the photocatalyst, in the field of environmental management, a photocatalytic technology is commonly adopted to degrade organic pollutants by utilizing light energy so as to better degrade hazardous organic matters, and the organic pollutants are degraded into inorganic micromolecular water and carbon dioxide.
The MIL-53(Cr) photocatalyst is used as one of Cr-based metal-organic framework materials, and compared with other metal-organic framework materials, the Cr-based metal-organic framework material has the advantages of economy, greenness, low toxicity and the like.
Based on the advantages of the MIL-53(Cr) photocatalyst, the invention discloses a synthesis method of the MIL-53(Cr) photocatalyst, so as to better prepare the MIL-53(Cr) photocatalyst.
Disclosure of Invention
The invention aims to provide a synthesis method of an MIL-53(Cr) photocatalyst, which aims to improve the yield and the crystallinity of the MIL-53(Cr) photocatalyst and improve the quality of the synthesized MIL-53(Cr) photocatalyst.
In order to achieve the purpose, the invention provides the following technical scheme:
a synthesis method of an MIL-53(Cr) photocatalyst comprises the following steps:
s1, taking a proper amount of raw materials according to the mixture ratio.
S2, placing the raw materials in the step S1 in a synthesizer, and stirring the raw materials by a stirring paddle for T1; then, a proper amount of hydrofluoric acid (40% HF) is added and stirring is continued for T2.
S3, heating the mixture in a synthesizer by an electric heating wire at the heating temperature of t 1; the reaction time was T3.
And S4, cooling the substance obtained after the reaction in the synthesizer, performing suction filtration through a vacuum pump, drying, and grinding.
S5, placing the substance obtained after grinding in the step S4 in a quartz tube to be calcined for a plurality of hours, and obtaining the MIL-53(Cr) photocatalyst.
Preferably, in the step S1, the raw materials and their mixture ratio are: 4-6 parts of chromium nitrate nonahydrate, 8-12 parts of terephthalic acid and 1600 parts of deionized water.
Preferably, in the step S1, the raw materials and their mixture ratio are: 5 parts of chromium nitrate nonahydrate, 10 parts of terephthalic acid and 1400 parts of deionized water.
Preferably, in the step S3, the heating temperature t1 is 206-231 ℃, particularly 219.85 ℃.
Preferably, in the step S3, the vibration conduction is performed by a vibration motor while heating, so as to accelerate the reaction of the raw material.
Preferably, in the step S2, the stirring time T1 is 0.6 to 1.2 hours, in particular 1 hour.
Preferably, in the step S2, the stirring time T2 is 0.8 to 1.2 hours, in particular 1 hour.
Preferably, in step S3, the reaction time T3 is 68 to 76 hours, in particular 72 hours.
Preferably, in the step S4, the temperature t2 of drying is 90-110 ℃, especially 100 ℃; the drying time is 22-26 hours, especially 24 hours.
Preferably, in the step S5, the quartz tube is placed into a tube furnace to be calcined in an air atmosphere, and the calcination temperature t3 is 259-305 ℃, especially 299.85 ℃; the calcination time may be 3 to 8 hours.
Preferably, in order to better synthesize the MIL-53(Cr) photocatalyst, the invention also discloses a device for synthesizing the MIL- (Cr) photocatalyst, which comprises a synthesizing mechanism and a vibrating mechanism, wherein the synthesizing mechanism comprises a base, a first disc is placed and installed in a groove at the top end of the base, a first connecting rod is arranged on one side of the first disc, a second disc is arranged at the top end of the first connecting rod, a first servo motor is arranged inside the first connecting rod, a synthesizer is arranged on one side of the first connecting rod through a rotating shaft, the rotating shaft on one side of the first connecting rod is connected with a first rotating rod, the first rotating rod is inserted into the synthesizer, stirring paddles are sleeved on the outer side of the synthesizer, the number of the stirring paddles is three, the vibrating mechanism comprises a vertical plate, and the vertical plate is arranged on one side of the top end of the base, and a second motor is arranged at the top end of one side of the base.
Preferably, a polytetrafluoroethylene lining layer is arranged in the synthesizer.
Preferably, the second motor is a vibration motor; a damping table is arranged between the second motor and the base; the damping table is made of flexible materials, particularly rubber; the Shore hardness Y of the rubber is 45-65, and the tensile strength Q is 30-35 MPa; in particular, the Shore hardness Y and the tensile strength Q satisfy the following condition: Y.Q is 1450 or more and 2685 or less.
Preferably, a sealing gasket is arranged between the synthesizer and the first rotating rod, and the sealing gasket plays a role in shock absorption while ensuring sealing. The thickness h of the sealing gasket is 1.5-2.8mm, and the sealing compression amount is 10-17%.
Preferably, in order to increase the reaction rate between the raw materials and further increase the synthesis efficiency of the MIL-53(Cr) photocatalyst, the vibration frequency f of the vibration motor is 38-66; particularly, the vibration frequency f, the sealing compression amount of the sealing gasket and the tensile strength Q satisfy the following empirical formula:
＝α·(Q/f)；
wherein alpha is a relation coefficient and has a value range of 0.54-0.78.
Preferably, cavities are formed in the first rotating rod and the stirring paddle, and electric heating wires are arranged in the cavities; the electric heating wire and the cavity are filled up through one of heat-conducting insulating pouring sealant, heat-conducting silicone grease and the like.
Preferably, a cavity is arranged in the wall of the synthesizer, and an electric heating wire is arranged in the cavity; the electric heating wire and the cavity are filled up through one of heat-conducting insulating pouring sealant, heat-conducting silicone grease and the like.
Preferably, the sliding grooves are formed in the two sides of the first disc, sliding blocks are arranged inside the sliding grooves in a sliding mode, and one side of each sliding block is connected with the inner wall of the corresponding groove of the base.
Preferably, transparent glass window is installed in the top and the embedding of one side of synthesizer, the bottom of second disc evenly is provided with the heating lamp, just the quantity of heating lamp is six. The heating lamp is a ceramic heating lamp.
Preferably, both sides of the synthesizer are provided with second connecting rods, two sides, away from each other, of the second connecting rods are provided with connecting blocks through rotating shafts, one end of each connecting block is provided with a third connecting rod through a rotating shaft, the third connecting rod is connected with the vertical plate, and the other end of each connecting block is connected with a rotating shaft on one side of the second motor.
Preferably, the bottom of synthesizer one side is inserted and is installed sealed piece, the outside of sealed piece is cup jointed and is provided with the sealing washer, just inside the sealing washer inserts the synthesizer, one side at base top is placed and is installed and is collected the box.
Preferably, the connecting blocks are all L-shaped.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the synthesis method of the MIL-53(Cr) photocatalyst, the MIL-53(Cr) photocatalyst is synthesized by chromium nitrate nonahydrate, terephthalic acid and deionized water, and the MIL-53(Cr) photocatalyst is easy to obtain raw materials, low in price and easy to produce on a large scale.
2. According to the synthesis method of the MIL-53(Cr) photocatalyst, the raw materials are fully mixed by stirring through the stirring of the stirring paddle, so that the reaction is facilitated, and the reaction rate is further improved.
3. According to the synthesis method of the MIL-53(Cr) photocatalyst, vibration conduction is carried out through the vibration motor, so that the MIL-53(Cr) photocatalyst reaction reagent in the synthesizer fully reacts, the reaction rate is accelerated, and the MIL-53(Cr) photocatalyst is rapidly synthesized.
4. According to the synthesis method of the MIL-53(Cr) photocatalyst, the cavities are formed in the first rotating rod and the stirring paddle, and the electric heating wires are arranged in the cavities, so that reagents in each position in the synthesizer can uniformly keep a proper reaction temperature, the reaction rate is accelerated, and the MIL-53(Cr) photocatalyst is rapidly synthesized.
5. The synthesis method of the MIL-53(Cr) photocatalyst comprises the steps of limiting a damping table to be made of a flexible material, particularly rubber; and the ranges of Shore hardness Y and tensile strength Q of the photocatalyst and the satisfied relation, so that the vibration generated by the vibration motor can better match with the reagent reaction in the synthesizer to promote the fusion, so as to accelerate the reaction rate and quickly synthesize the MIL-53(Cr) photocatalyst.
6. According to the synthesis method of the MIL-53(Cr) photocatalyst, the relation among the vibration frequency f, the sealing compression amount of the sealing gasket and the tensile strength Q is set, and the reaction rate among raw materials is increased, so that the synthesis efficiency of the MIL-53(Cr) photocatalyst is improved.
Drawings
FIG. 1 is a molecular structure diagram of a MIL-53(Cr) photocatalyst.
FIG. 2 is a spatial structure diagram of the MIL-53(Cr) photocatalyst.
FIG. 3 is a flow chart of the synthesis method of the MIL-53(Cr) photocatalyst of the present invention.
FIG. 4 is a schematic view of a photocatalyst synthesizing apparatus according to the present invention.
Figure 5 is a side cross-sectional view of the first disk and synthesizer structure of the present invention.
Fig. 6 is an enlarged view of a portion of a structure shown in fig. 4 according to the present invention.
Fig. 7 is an enlarged view of a portion of the structure at B in fig. 4 according to the present invention.
In the figure: 100. a synthesizing mechanism; 110. a base; 111. a first disc; 112. a first connecting rod; 113. a first servo motor; 114. a heating lamp; 115. a synthesizer; 116. a first rotating lever; 117. a stirring paddle; 118. a chute; 119. a slider; 120. a transparent glass window; 121. a second disc; 200. a vibration mechanism; 210. a vertical plate; 211. a second motor; 212. a second connecting rod; 213. connecting blocks; 214. a third connecting rod; 215. a sealing block; 216. a seal ring; 217. and (4) collecting the box.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Referring to fig. 1-3, a method for synthesizing MIL-53(Cr) photocatalyst includes the following steps:
s1, taking a proper amount of raw materials according to the mixture ratio.
S2, placing the raw materials in the step S1 in a synthesizer, and stirring the raw materials by a stirring paddle for T1; then, a proper amount of hydrofluoric acid (40% HF) is added and stirring is continued for T2.
S3, heating the mixture in a synthesizer by an electric heating wire at the heating temperature of t 1; the reaction time was T3.
And S4, cooling the substance obtained after the reaction in the synthesizer, performing suction filtration through a vacuum pump, drying, and grinding.
S5, placing the substance obtained after grinding in the step S4 in a quartz tube to be calcined for a plurality of hours, and obtaining the MIL-53(Cr) photocatalyst.
In the step S1, the raw materials and their mixture ratio are: 4-6 parts of chromium nitrate nonahydrate, 8-12 parts of terephthalic acid and 1600 parts of deionized water.
In the step S3, the heating temperature t1 is 206-231 ℃, particularly 219.85 ℃. While heating, the vibration motor is used for vibration conduction to promote the reaction of the raw materials. The reaction time T3 is 68 to 76 hours, in particular 72 hours.
In step S2, the stirring time T1 is 0.6 to 1.2 hours, in particular 1 hour. The stirring time T2 is from 0.8 to 1.2 hours, in particular 1 hour.
In the step S4, the temperature t2 of drying is 90-110 ℃, in particular 100 ℃; the drying time is 22-26 hours, especially 24 hours.
In the step S5, the quartz tube is placed into a tube furnace to be calcined in an air atmosphere, wherein the calcination temperature t3 is 259-305 ℃, in particular 299.85 ℃; the calcination time may be 3 to 8 hours.
In order to further increase the reaction rate of the chromium nitrate nonahydrate, the terephthalic acid and the like to synthesize MIL-53(Cr) more rapidly, the following empirical formula is satisfied between the heating temperature t1 and the calcination temperature t 3:
t1/t3＝β·ζ；
wherein, zeta is the part ratio of chromium nitrate nonahydrate and terephthalic acid; beta is a relation factor, and the value range is 2.5-21.4.
Example 2
Referring to fig. 3, a method for synthesizing MIL-53(Cr) photocatalyst includes the following steps:
s1, taking a proper amount of raw materials according to the mixture ratio.
S2, placing the raw materials in the step S1 in a synthesizer, and stirring the raw materials by a stirring paddle for T1; then, a proper amount of hydrofluoric acid (40% HF) is added and stirring is continued for T2.
S3, heating the mixture in a synthesizer by an electric heating wire at the heating temperature of t 1; the reaction time was T3.
And S4, cooling the substance obtained after the reaction in the synthesizer, performing suction filtration through a vacuum pump, drying, and grinding.
S5, placing the substance obtained after grinding in the step S4 in a quartz tube to be calcined for a plurality of hours, and obtaining the MIL-53(Cr) photocatalyst.
In the step S1, the raw materials and their mixture ratio are: 5 parts of chromium nitrate nonahydrate, 10 parts of terephthalic acid and 1400 parts of deionized water.
In the step S3, the heating temperature t1 is 206-231 ℃, particularly 219.85 ℃. While heating, the vibration motor is used for vibration conduction to promote the reaction of the raw materials. The reaction time T3 is 68 to 76 hours, in particular 72 hours.
In step S2, the stirring time T1 is 0.6 to 1.2 hours, in particular 1 hour. The stirring time T2 is from 0.8 to 1.2 hours, in particular 1 hour.
In the step S4, the temperature t2 of drying is 90-110 ℃, in particular 100 ℃; the drying time is 22-26 hours, especially 24 hours.
In the step S5, the quartz tube is placed into a tube furnace to be calcined in an air atmosphere, wherein the calcination temperature t3 is 259-305 ℃, in particular 299.85 ℃; the calcination time may be 3 to 8 hours.
Example 3
Referring to fig. 4-7, the present invention further discloses a device for synthesizing MIL-53(Cr) photocatalyst, comprising a synthesizing mechanism 100 and a vibrating mechanism 200, wherein the synthesizing mechanism 100 includes a base 110, a first disc 111 is disposed in a groove at the top end of the base 110, a first connecting rod 112 is disposed at one side of the first disc 111, a second disc 121 is disposed at the top end of the first connecting rod 112, a first servo motor 113 is disposed inside the first connecting rod 112, a synthesizer 115 is disposed at one side of the first connecting rod 112 through a rotating shaft, the rotating shaft at one side of the first connecting rod 112 is connected to a first rotating rod 116, the first rotating rod 116 is inserted into the synthesizer 115, three stirring paddles 117 are sleeved outside the synthesizer 115, the vibrating mechanism 200 includes a vertical plate 210, the vertical plate 210 is disposed at one side of the top end of the base 110, a second motor 211 is disposed at the top end of one side of the base 110, chemical raw materials and the photocatalyst in the synthesizer 115 can be fully mixed, and the reaction efficiency is improved.
The two sides of the first disc 111 are both provided with sliding grooves 118, the sliding blocks 119 are slidably mounted inside the sliding grooves 118, one side of each sliding block 119 is connected with the inner wall of the groove of the base 110, the two sides of the synthesizer 115 are both provided with second connecting rods 212, the sides, away from each other, of the two second connecting rods 212 are both provided with connecting blocks 213 through rotating shafts, one end of one connecting block 213 is provided with a third connecting rod 214 through rotating shaft, the third connecting rod 214 is connected with the vertical plate 210, one end of the other connecting block 213 is connected with the rotating shaft on one side of the second motor 211, the connecting blocks 213 are all in L shape, the L shape of the connecting block 213 enables the connecting block 213 to rotate to drive the first disc 111 to reciprocate, therefore, the synthesizer 115 can be driven by the rotation of the connection block 213 to shake up and down, so that the chemical raw materials and the photocatalyst in the synthesizer 115 can be fully stirred and mixed, and the stirring efficiency is improved.
The synthesizer is a container with closed periphery, and is provided with a material inlet and a material outlet.
Example 4
A synthesis device of MIL-53(Cr) photocatalyst comprises a synthesis mechanism 100 and a vibration mechanism 200, wherein the synthesis mechanism 100 comprises a base 110, a first disc 111 is placed and installed in a groove at the top end of the base 110, one side of the first disc 111 is provided with a first connecting rod 112, the top end of the first connecting rod 112 is provided with a second disc 121, a first servo motor 113 is arranged inside the first connecting rod 112, one side of the first connecting rod 112 is provided with a synthesizer 115 through a rotating shaft, the rotating shaft at one side of the first connecting rod 112 is connected with a first rotating rod 116, the first rotating rod 116 is inserted into the synthesizer 115, the outer side of the synthesizer 115 is sleeved with three stirring paddles 117, the vibration mechanism 200 comprises a vertical plate 210, the vertical plate 210 is arranged at one side of the top end of the base 110, the top end at one side of the base 110 is provided with a second motor 211, so that chemical raw materials and photocatalyst inside the synthesizer 115 can be fully mixed, the reaction efficiency is improved.
The two sides of the first disc 111 are both provided with sliding grooves 118, the sliding blocks 119 are slidably mounted inside the sliding grooves 118, one side of each sliding block 119 is connected with the inner wall of the groove of the base 110, the two sides of the synthesizer 115 are both provided with second connecting rods 212, the sides, away from each other, of the two second connecting rods 212 are both provided with connecting blocks 213 through rotating shafts, one end of one connecting block 213 is provided with a third connecting rod 214 through rotating shaft, the third connecting rod 214 is connected with the vertical plate 210, one end of the other connecting block 213 is connected with the rotating shaft on one side of the second motor 211, the connecting blocks 213 are all in L shape, the L shape of the connecting block 213 enables the connecting block 213 to rotate to drive the first disc 111 to reciprocate, therefore, the synthesizer 115 can be driven by the rotation of the connection block 213 to shake up and down, so that the chemical raw materials and the photocatalyst in the synthesizer 115 can be fully stirred and mixed, and the stirring efficiency is improved.
A polytetrafluoroethylene lining layer is arranged in the synthesizer. The second motor is a vibration motor; a damping table is arranged between the second motor and the base; the damping table is made of flexible materials, particularly rubber; the Shore hardness Y of the rubber is 45-65, and the tensile strength Q is 30-35 MPa; in particular, the Shore hardness Y and the tensile strength Q satisfy the following condition: Y.Q is 1450 or more and 2685 or less.
A sealing gasket is arranged between the synthesizer and the first rotating rod, and the sealing gasket can play a role in shock absorption while ensuring sealing. The thickness h of the sealing gasket is 1.5-2.8mm, and the sealing compression amount is 10-17%.
In order to improve the reaction rate between raw materials and further improve the synthesis efficiency of the MIL-53(Cr) photocatalyst, the vibration frequency f of the vibration motor is 38-66; particularly, the vibration frequency f, the sealing compression amount of the sealing gasket and the tensile strength Q satisfy the following empirical formula:
＝α·(Q/f)；
wherein alpha is a relation coefficient and has a value range of 0.54-0.78.
Cavities are formed in the first rotating rod and the stirring paddle, and electric heating wires are arranged in the cavities; the electric heating wire and the cavity are filled up through one of heat-conducting insulating pouring sealant, heat-conducting silicone grease and the like.
A cavity is arranged in the wall of the synthesizer, and an electric heating wire is arranged in the cavity; the electric heating wire and the cavity are filled up through one of heat-conducting insulating pouring sealant, heat-conducting silicone grease and the like.
The top end and one side of the combiner 115 are embedded with a transparent glass window 120, the bottom end of the second disk 121 is uniformly provided with six heating lamps 114, and the heating lamps 114 can adjust the appropriate illumination intensity. The heating lamp is a ceramic heating lamp.
The bottom end of one side of the synthesizer 115 is inserted with a sealing block 215, the outer side of the sealing block 215 is sleeved with a sealing ring 216, and the sealing ring 216 is inserted into the synthesizer 115, so that the discharge port of the synthesizer 115 is in a sealing state, and reactants cannot leak out. A collection box 217 is disposed on one side of the top end of the base 110, and the discharged material of the synthesizer 115 is allowed to fall into the collection box 217 for collection after the synthesis reaction is completed.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (7)
1. A synthesis method of an MIL-53(Cr) photocatalyst is characterized by comprising the following steps: the synthesis method comprises the following steps:
s1, taking a proper amount of raw materials according to the proportion;
s2, placing the raw materials in the step S1 in a synthesizer, and stirring the raw materials by a stirring paddle for T1; then adding a proper amount of hydrofluoric acid (40% HF) and continuing stirring for T2;
s3, heating the mixture in a synthesizer by an electric heating wire at the heating temperature of t 1; the reaction time is T3;
s4, cooling the substance obtained after the reaction in the synthesizer, performing suction filtration through a vacuum pump, drying, and grinding;
s5, placing the substance obtained after grinding in the step S4 in a quartz tube to be calcined for a plurality of hours, and obtaining the MIL-53(Cr) photocatalyst.
2. The method for synthesizing an MIL-53(Cr) photocatalyst as claimed in claim 1, wherein: in the step S1, the raw materials and the mixture ratio thereof are as follows: 4-6 parts of chromium nitrate nonahydrate, 8-12 parts of terephthalic acid and 1600 parts of deionized water.
3. The method for synthesizing MIL-53(Cr) photocatalyst as claimed in claims 1 and 2, wherein: in the step S3, the heating temperature t1 is 206-231 ℃, particularly 219.85 ℃.
4. The method for synthesizing an MIL-53(Cr) photocatalyst as claimed in claim 1, wherein: in step S3, vibration conduction is performed by the vibration motor while heating, so as to accelerate the reaction of the raw material.
5. The method for synthesizing an MIL-53(Cr) photocatalyst as claimed in claim 1, wherein: in the step S2, the stirring time T1 is 0.6 to 1.2 hours.
6. The method for synthesizing an MIL-53(Cr) photocatalyst as claimed in claim 1, wherein: in the step S3, the reaction time T3 is 68 to 76 hours.
7. The method for synthesizing an MIL-53(Cr) photocatalyst as claimed in claim 1, wherein: in the step S5, the quartz tube is placed into a tube furnace to be calcined in an air atmosphere, wherein the calcination temperature t3 is 259-305 ℃, in particular 299.85 ℃; the calcination time may be 3 to 8 hours.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012144758A2 (en) * | 2011-04-18 | 2012-10-26 | 한국화학연구원 | Method for functionalizing porous metal-organic framework materials, solid acid catalyst using same, and method for evaporating alcohol using the solid acid catalyst |
| CN107556488A (en) * | 2017-09-30 | 2018-01-09 | 哈尔滨工业大学 | A kind of simple, green syt metal machine framework material MIL 53 (Cr) method |
-
2020
- 2020-08-05 CN CN202010780733.7A patent/CN111871464A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012144758A2 (en) * | 2011-04-18 | 2012-10-26 | 한국화학연구원 | Method for functionalizing porous metal-organic framework materials, solid acid catalyst using same, and method for evaporating alcohol using the solid acid catalyst |
| CN107556488A (en) * | 2017-09-30 | 2018-01-09 | 哈尔滨工业大学 | A kind of simple, green syt metal machine framework material MIL 53 (Cr) method |
Non-Patent Citations (2)
| Title |
|---|
| 刘澳琦等: "MIL-53材料的制备及其光催化性能的研究", 《化工科技》 * |
| 杨琰: "金属有机骨架材料MIL-53（Cr）的改性及其吸附CO2和CH4的性能", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑 (月刊)》 * |
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