CN107417921B - A chemical formula of [ C18H12N6Nd2O15]nSynthesis and application of metal organic framework compound - Google Patents
A chemical formula of [ C18H12N6Nd2O15]nSynthesis and application of metal organic framework compound Download PDFInfo
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- 150000001875 compounds Chemical class 0.000 title claims abstract description 39
- 239000012621 metal-organic framework Substances 0.000 title claims abstract description 39
- 239000000126 substance Substances 0.000 title claims abstract description 29
- 239000013078 crystal Substances 0.000 claims abstract description 12
- ZUCRGHABDDWQPY-UHFFFAOYSA-N pyrazine-2,3-dicarboxylic acid Chemical compound OC(=O)C1=NC=CN=C1C(O)=O ZUCRGHABDDWQPY-UHFFFAOYSA-N 0.000 claims abstract description 7
- -1 rare earth salt Chemical class 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 4
- MWVTWFVJZLCBMC-UHFFFAOYSA-N 4,4'-bipyridine Chemical compound C1=NC=CC(C=2C=CN=CC=2)=C1 MWVTWFVJZLCBMC-UHFFFAOYSA-N 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000002447 crystallographic data Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 2
- 239000011259 mixed solution Substances 0.000 claims 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims 1
- 239000004810 polytetrafluoroethylene Substances 0.000 claims 1
- 239000000758 substrate Substances 0.000 claims 1
- 238000005260 corrosion Methods 0.000 abstract description 18
- 230000007797 corrosion Effects 0.000 abstract description 18
- 229910052751 metal Inorganic materials 0.000 abstract description 17
- 239000002184 metal Substances 0.000 abstract description 17
- 239000003112 inhibitor Substances 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 5
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000001308 synthesis method Methods 0.000 abstract description 2
- 230000002194 synthesizing effect Effects 0.000 abstract description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 15
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 10
- 229910052802 copper Inorganic materials 0.000 description 10
- 239000010949 copper Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 8
- 238000010586 diagram Methods 0.000 description 6
- 230000005764 inhibitory process Effects 0.000 description 5
- 125000004430 oxygen atom Chemical group O* 0.000 description 5
- 239000011148 porous material Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 3
- 229910052779 Neodymium Inorganic materials 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- ZHUXMBYIONRQQX-UHFFFAOYSA-N hydroxidodioxidocarbon(.) Chemical group [O]C(O)=O ZHUXMBYIONRQQX-UHFFFAOYSA-N 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229940125782 compound 2 Drugs 0.000 description 1
- 239000013256 coordination polymer Substances 0.000 description 1
- 229920001795 coordination polymer Polymers 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 150000002391 heterocyclic compounds Chemical class 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
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- 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
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
- C23F11/10—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
- C23F11/14—Nitrogen-containing compounds
Abstract
The invention discloses a chemical formula of [ C ]18H12N6Nd2O15]nA method for synthesizing a metal organic framework compound. Has a chemical formula of [ C18H12N6Nd2O15]nThe metal-organic framework compound crystal belongs to a monoclinic system, P21Space group/c, unit cell parameter a 5.4573nm, b 10.900nm, c 10.410nm, beta 98.172 deg. and unit cell volume V612.9 nm3The face-centered cell F (000) is 350, GOOF is 1.042, the number of molecules in the cell Z is 4, and the chemical formula is [ C18H12N6Nd2O15]nThe metal organic framework compound takes pyrazine-2, 3-dicarboxylic acid, 4' -bipyridine and rare earth salt as raw materials, reacts for 72 hours at 140 ℃, and is slowly cooled to room temperature to obtain a target product. The synthesis method is simple to operate and environment-friendly. Has a chemical formula of [ C18H12N6Nd2O15]nThe metal organic framework compound can be used as a corrosion inhibitor to be applied to the field of metal corrosion and protection.
Description
Technical Field
The invention relates to a chemical formula of [ C ]18H12N6Nd2O15]nSynthesis and application of metal organic frame compound.
Background
Metal-organic frameworks (MOFs) are a new type of porous material formed by self-assembling organic ligands and metal ions into a zeolite-like structure with a repeating network structure, and MOFs is one of coordination polymers. MOFs are a new type of material that has developed rapidly in the field of coordination chemistry in the last decade. The MOFs material has a series of characteristics of high porosity, various topological structures, larger specific surface area, simple and easy operation of a synthesis method, adjustable framework scale and space structure and the like, and a series of MOFs materials with rich structures and complete functions can be obtained by adjusting an experimental scheme and synthesis conditions according to target requirements, so that the research on the MOFs materials is paid more and more attention. Heterocyclic compounds are a very bulky class of organic compounds commonly used as ligands for the preparation of MOFs. The carboxylic acid heterocyclic compound has strong coordination capacity and extremely flexible coordination mode, and MOFs materials obtained by coordination of the carboxylic acid heterocyclic compound and metal ions often have novel and changeable structures and are widely applied to many fields, such as adsorption and separation of gas, catalysis, electrochemical properties, molecular magnets, ion exchange, slow release of drugs and the like, so that the carboxylic acid heterocyclic compound has a good development prospect. The MOFs are one of the hot topics in the field of porous materials.
Metals and alloys thereof are important components of modern materials, but the metal materials are damaged by the environmental effects of gas, water, soil and the like in the using process to cause the metal materials to be corroded or aged, the corrosion of the metals is seriously harmful in the industrial department, and the corrosion is more serious especially in acidic media. The metal organic framework material has larger specific surface area and strong adsorption capacity on the metal surface, and is expected to become a good metal corrosion inhibitor. At present, the MOFs material is applied to the field of metal corrosion and protection, and documents report a few.
The patent provides a method for synthesizing a compound with a chemical formula of [ C ] by using pyrazine-2, 3-dicarboxylic acid, 4' -bipyridine and rare earth salt as raw materials through a hydrothermal method18H12N6Nd2O15]nThe metal organic frame compounds (MOFs) and the corrosion inhibitor for metal copper in dilute hydrochloric acid is provided by utilizing the strong corrosion inhibition performance of the MOFs.
Disclosure of Invention
The invention aims to provide a chemical formula of [ C ]18H12N6Nd2O15]nSynthesis and application of metal organic frame compound.
Has a chemical formula of [ C18H12N6Nd2O15]nThe metal organic framework compound crystal belongs to a monoclinic system, P21/c space group and has the unit cell parameter of
Beta is 101.244(2) ° and unit cell volume is
The face center unit cell F (000) ═ 1608.0, GOOF ═ 1.042, and the number of molecules in the unit cell Z ═ 4, the crystallographic data are shown in table 1. Has a chemical formula of [ C18H12N6Nd2O15]nThe metal organic framework compound has stronger corrosion inhibition performance and can be used as a corrosion inhibitor for metal copper in dilute hydrochloric acid.
TABLE 1 chemical formula is [ C18H12N6Nd2O15]nCrystallographic parameters of metal-organic framework compounds
The chemical formula is [ C18H12N6Nd2O15]nThe metal organic framework compound is synthesized by the following specific steps:
(1) 15mL of a solution containing 0.5mmol (0.165g) of Nd (NO)3)3·nH2O, 0.5mmol (0.084g) of pyrazine-2, 3-dicarboxylic acid (2,3-Hpyza) and 0.5mmol (0.0781g) of distilled water solution of 4,4 '-bipyridine (4, 4' -pydc) were magnetically stirred at room temperature for 30min, the pH was adjusted to 5-6 with ammonia water, and stirring was continued for 30 min.
(2) The mixture in the beaker was transferred to a 25mL hydrothermal reaction vessel equipped with a Teflon liner. And (3) putting the reaction kettle into an oven, heating to 140 ℃, and crystallizing for 72 hours. Cooling by program after 72h, cooling to 10-100 deg.C per hour, maintaining for 10h, cooling to room temperature in natural state, taking out the reaction kettle, generating white needle crystal, filtering, drying at room temperature, and collecting sample to obtain product with chemical formula [ C [ ]18H12N6Nd2O15]nA metal organic framework compound.
Has a chemical formula of [ C18H12N6Nd2O15]nThe metal organic framework compound is used as a corrosion inhibitor to be applied to dilute hydrochloric acid to slow down the corrosion of hydrochloric acid to metal copper.
Drawings
FIG. 1 shows a chemical formula of [ C ] according to the present invention18H12N6Nd2O15]nA metal organic framework compound structural unit diagram.
FIG. 2 shows a chemical formula of [ C ] according to the present invention18H12N6Nd2O15]nMetal organic framework compound coordination polyhedral diagram.
FIG. 3 shows a chemical formula of [ C ] according to the present invention18H12N6Nd2O15]nThe three-dimensional stacking diagram (a direction) of the metal-organic framework compound crystals.
FIG. 4 shows a chemical formula of [ C ] according to the present invention18H12N6Nd2O15]nScanning electron microscope photo of metal organic frame compound to dilute hydrochloric acid metal copper corrosion inhibition effect.
Detailed Description
Example (b):
(1) 15mL of a solution containing 0.5mmol (0.165g) of Nd (NO)3)3·nH2O, 0.5mmol (0.084g) of pyrazine-2, 3-dicarboxylic acid (2,3-Hpyza) and 0.5mmol (0.0781g) of distilled water solution of 4,4 '-bipyridine (4, 4' -pydc) were magnetically stirred at room temperature for 30min, the pH was adjusted to 5-6 with ammonia water, and stirring was continued for 30 min.
(2) The mixture in the beaker was transferred to a 25mL hydrothermal reaction vessel equipped with a Teflon liner. And (3) putting the reaction kettle into an oven, heating to 140 ℃, and crystallizing for 72 hours. Cooling by program after 72h, cooling to 10-100 deg.C per hour, maintaining for 10h, cooling to room temperature in natural state, taking out the reaction kettle, generating white needle crystal, filtering, drying at room temperature, and collecting sample to obtain product with chemical formula [ C [ ]18H12N6Nd2O15]nA metal organic framework compound. Yield 79%, theoretical value (%) of elemental analysis: c, 25.76; h, 1.19; test values (%): c, 25.16; h, 1.06.
Has a chemical formula of [ C18H12N6Nd2O15]nMetal organic frameThe rack compound is used as a corrosion inhibitor applied to dilute hydrochloric acid to slow down the corrosion of hydrochloric acid to metal copper.
The obtained chemical formula is [ C ]18H12N6Nd2O15]nAnalysis of the crystal structure of the metal-organic framework compound: appropriately sized crystals (0.34X 0.38X 0.15mm) were selected and 5 crystal data were collected sequentially using a Bruker SMART APEX CCD single crystal diffractometer. Using Mo-Kalpha rays (gamma. 0.071073nm) monochromatized with graphite
Scanning mode, diffraction points were collected at 293(2) K in the range of 3.36 ° to 25.0 °. The diffracted intensity data were empirically absorption corrected using the SADABS program. The structure of the crystal is resolved by a direct method by using a SHELXS-97 program, and coordinates of all non-hydrogen atoms and anisotropic parameters thereof are corrected by a full matrix least square method by using the SHELXS-97 program. All hydrogen atoms are theoretically hydrogenated. The data on the crystallographic and structural modifications are shown in Table 1.
TABLE 1 chemical formula is [ C18H12N6Nd2O15]nCrystallographic parameters of metal-organic framework compounds
As can be seen from Table 1, the chemical formula is [ C ]18H12N6Nd2O15]nThe metal-organic framework compound belongs to a monoclinic system and is P21/c space group with unit cell parameters
Beta is 101.244(2) ° and unit cell volume is
The face center unit cell F (000) ═ 1608.0, GOOF ═ 1.042, the number of molecules Z in the unit cell is 4, and the bond angle of partial bond length is shown in table 2. FIG. 1 is a structural unit diagram of a compound, FIG. 2 is a coordination polyhedron diagram of a central metal neodymium ion, and FIG. 3 is a stacking diagram of the compound in the direction a. As can be seen from Table 1, the empirical formula of the metal-organic framework compound is C18H10N6Nd2O15Two neodymium ions have different coordination modes (as shown in figure 2), Nd1 is combined with five oxygen atoms, O3 and O4 are derived from carboxyl oxygen atoms in the same pyrazine-2, 3-dicarboxylic acid molecule, O6 and O9 are derived from carboxyl oxygen atoms in two different pyrazine-2, 3-dicarboxylic acid molecules, oxygen atoms in solvent water, and O13 is derived from oxygen atoms in solvent water, and the coordination number of the coordination number is 5; nd2 is bonded to one nitrogen atom and seven oxygen atoms, has a coordination number of 8, and forms a polyhedral configuration of binuclear neodymium by the bonded oxygen atoms and nitrogen atoms. As can be seen from FIG. 3, Compound 2 had 3D pores in the a-axis direction, and the pore size was 1.067X 1.066nm2。
In order to observe the corrosion inhibition effect of the compound more intuitively, a scanning electron microscope is adopted to study the surface morphology of the copper sheet after being soaked in hydrochloric acid without the compound and hydrochloric acid with the compound for 72 hours (as shown in figure 4). As can be seen from FIG. 4, the copper sheet in the hydrochloric acid solution without the compound is corroded very severely, the surface of the copper sheet is uneven, and more pitting pits with different depths appear. After the compound is added, the corrosion degree of the surface of the copper sheet is greatly reduced, and the surface is relatively flat, which shows that the compound can be adsorbed on the surface of the copper sheet to form a film and play a corrosion inhibition role.
Claims (1)
1. A chemical formula of [ C18H12N6Nd2O15]nA metal-organic framework compound characterized by the chemical formula [ C18H12N6Nd2O15]nThe metal organic framework compound crystal belongs to a monoclinic system, P21/c space group and has the unit cell parameter of
β＝101.244(2)DEG, unit cell volume of
The face center unit cell F (000) ═ 1608.0, GOOF ═ 1.042, the number of molecules in the unit cell Z ═ 4, and the crystallographic data are shown in table 1;
TABLE 1 chemical formula is [ C18H12N6Nd2O15]nCrystallographic parameters of metal-organic framework compounds
The chemical formula is [ C18H12N6Nd2O15]nThe preparation method of the metal organic framework compound is characterized by comprising the following specific steps:
(1) 15mL of a solution containing 0.5mmol (0.165g) of Nd (NO)3)30.5mmol (0.084g) of pyrazine-2, 3-dicarboxylic acid (2,3-Hpyza) and 0.5mmol (0.0781g) of distilled water solution of 4,4 '-bipyridine (4, 4' -pydc) are magnetically stirred at room temperature for 30min, the pH is adjusted to be between 5 and 6 by ammonia water, and stirring is continued for 30 min;
(2) transferring the mixed solution in the beaker to a 25mL hydrothermal reaction kettle with a polytetrafluoroethylene substrate, putting the reaction kettle into an oven, heating to 140 ℃, crystallizing for 72h, carrying out programmed cooling after 72h, cooling to 10-100 ℃ per hour, preserving heat for 10h, turning off the oven, cooling to room temperature in a natural state, taking out the reaction kettle, generating white needle crystals, filtering, drying at room temperature, collecting a sample to obtain the chemical formula [ C ]18H12N6Nd2O15]nA metal organic framework compound.
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| CN108671893B (en) * | 2018-04-24 | 2021-03-30 | 浙江大学 | Metal organic framework material for separating ethylene and acetylene and method for separating ethylene and acetylene |
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| CN110218332A (en) * | 2019-06-17 | 2019-09-10 | 北京石油化工学院 | A kind of Zn complex nano container and the preparation method and application thereof loading corrosion inhibiter |
| CN112457696B (en) * | 2020-10-28 | 2022-03-22 | 桂林理工大学 | Self-repairing coating based on quinoline nano metal-organic framework material and preparation method thereof |
| CN112679749B (en) * | 2020-12-24 | 2022-03-29 | 华南理工大学 | Zeolite-like zinc-based imidazole ester metal organic framework reinforcing steel bar corrosion inhibitor and preparation method and application thereof |
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Application publication date: 20171201 Assignee: GUANGXI YANGSHENG NEW ENERGY CO.,LTD. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2023980045034 Denomination of invention: Synthesis and application of a metal organic framework compound with chemical formula [C18H12N6Nd2O15]n Granted publication date: 20201124 License type: Common License Record date: 20231101 |
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Application publication date: 20171201 Assignee: Guilin Hongshengda Chemical Reagent Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2023980045089 Denomination of invention: Synthesis and application of a metal organic framework compound with chemical formula [C18H12N6Nd2O15]n Granted publication date: 20201124 License type: Common License Record date: 20231103 |
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Application publication date: 20171201 Assignee: Guangxi shimaoda Technology Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2023980045683 Denomination of invention: Synthesis and application of a metal organic framework compound with chemical formula [C18H12N6Nd2O15]n Granted publication date: 20201124 License type: Common License Record date: 20231106 |