CN104610325B - Novel lanthanum coordination polymer and preparation method thereof - Google Patents
Novel lanthanum coordination polymer and preparation method thereof Download PDFInfo
- Publication number
- CN104610325B CN104610325B CN201410841910.2A CN201410841910A CN104610325B CN 104610325 B CN104610325 B CN 104610325B CN 201410841910 A CN201410841910 A CN 201410841910A CN 104610325 B CN104610325 B CN 104610325B
- Authority
- CN
- China
- Prior art keywords
- coordination polymer
- lanthanum
- stirring
- preparation
- lanthanum coordination
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 229910052746 lanthanum Inorganic materials 0.000 title claims abstract description 94
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 239000013256 coordination polymer Substances 0.000 title claims abstract description 81
- 229920001795 coordination polymer Polymers 0.000 title claims abstract description 81
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- MMEDJBFVJUFIDD-UHFFFAOYSA-N 2-[2-(carboxymethyl)phenyl]acetic acid Chemical compound OC(=O)CC1=CC=CC=C1CC(O)=O MMEDJBFVJUFIDD-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000003446 ligand Substances 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 239000012153 distilled water Substances 0.000 claims description 21
- 239000000706 filtrate Substances 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 20
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 19
- 239000002253 acid Substances 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 150000007513 acids Chemical class 0.000 claims description 14
- 229950000845 politef Drugs 0.000 claims description 14
- 229910001220 stainless steel Inorganic materials 0.000 claims description 12
- 239000010935 stainless steel Substances 0.000 claims description 12
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 229910000831 Steel Inorganic materials 0.000 claims description 2
- 239000010959 steel Substances 0.000 claims description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 24
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- -1 rare earth ion Chemical class 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- 238000013329 compounding Methods 0.000 description 2
- 238000012718 coordination polymerization Methods 0.000 description 2
- 238000002050 diffraction method Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000005408 paramagnetism Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/003—Compounds containing elements of Groups 3 or 13 of the Periodic Table without C-Metal linkages
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/18—Metal complexes
- C09K2211/182—Metal complexes of the rare earth metals, i.e. Sc, Y or lanthanide
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
Abstract
The invention discloses a novel lanthanum coordination polymer and a preparation method thereof. The chemical formula of the novel lanthanum coordination polymer is [La(PDAA)1.5(H2O)](H2O), wherein PDAA is a 1, 2-phenylenediacetic acid anion ligand. The novel lanthanum coordination polymer belongs to a C2/c space group in a monoclinic system. The cell parameter is shown in the Specification, wherein beta=92.677(3) degrees, and V=3348.2(7), and the value of V is also shown in the Specification. The invention further provides the novel lanthanum coordination polymer and the preparation method thereof. The preparation method is simple to operate and good in repeatability, and the novel lanthanum coordination polymer obtained is high in purity.
Description
Technical field
The present invention relates to coordination polymer technical field, more particularly to a kind of new lanthanum coordination polymer and its preparation side
Method.
Background technology
Rare earth compounding has a characteristics such as unique light, electricity, the magnetic of rare earth ion, and with its unique fluorescent characteristic and excellent
Good paramagnetism is widely used in the fields such as luminous and display.Substantial amounts of rare earth compounding is reported so far.1,2- benzene two
, used as half firm semiflexible part, the polymer network structure that its assembling is formed is wayward and predicts for acetic acid, it is difficult to control anti-
The condition synthesis target coordination polymer answered.The coordination polymer formed using 1,2- phenylenediacetic Acids and lanthanum is not also reported at present
Road.
The content of the invention
The present invention proposes a kind of new lanthanum coordination polymer, and its is stable in properties, and with fluorescence；The present invention is also proposed
A kind of preparation method of new lanthanum coordination polymer, the method is simple to operate, yield is high, the new lanthanum coordination polymer for preparing
Purity is high, reproducibility is good.
The present invention proposes a kind of new lanthanum coordination polymer, and its chemical formula is [La (PDAA)1.5(H2O)]·(H2O), its
In, PDAA is 1,2- phenylenediacetic Acid anion ligands, and the structural formula of PDAA is as follows：
Preferably, the new lanthanum coordination polymer belongs to monoclinic system, and C2/c space groups, cell parameter is as follows：β=92.677 (3) °,
Preferably, in the new lanthanum coordination polymer, 1,2- phenylenediacetic Acid anion ligand takes as follows
Two kinds of coordination modes：
The invention allows for a kind of preparation method of the new lanthanum coordination polymer, comprises the following steps：By nitric acid
Distilled water is added after lanthanum and the mixing of 1,2- phenylenediacetic Acid, the pH value of regulation system is 2-7 after stirring, is filtered after stirring, so
Filtrate is placed in autoclave afterwards, hydro-thermal reaction 40-60h is carried out at 150-180 DEG C, reaction is cooled to room after terminating
Temperature, filters, and is dried to obtain the new lanthanum coordination polymer.
Preferably, the preparation method of the new lanthanum coordination polymer, comprises the following steps：By Lanthanum (III) nitrate and 1,2- benzene two
Distilled water is added after acetic acid mixing, the pH value of regulation system is 3-6 after stirring, filtered after stirring, be then placed in filtrate
In autoclave, hydro-thermal reaction 48-55h is carried out at 160-170 DEG C, reaction is cooled to room temperature after terminating, and filters, dry
To the new lanthanum coordination polymer.
Preferably, the preparation method of the new lanthanum coordination polymer, comprises the following steps：By Lanthanum (III) nitrate and 1,2- benzene two
Distilled water is added after acetic acid mixing, the pH value of regulation system is 4 after stirring, filtered after stirring, then filtrate is placed in into height
In pressure reactor, hydro-thermal reaction 50h is carried out at 165 DEG C, reaction is cooled to room temperature after terminating, and filters, be dried to obtain described new
Type lanthanum coordination polymer.
Preferably, the preparation method of the new lanthanum coordination polymer, comprises the following steps：By molar part by 0.05-0.1
Part Lanthanum (III) nitrate and 0.1-0.15 parts 1, after the mixing of 2- phenylenediacetic Acids, add 200-500 part distilled water, after stirring, adjust body
The pH value of system is 3-6, is filtered after stirring, and filtrate is placed in and is made in the stainless steel cauldron of lining with politef,
155-175 DEG C carries out hydro-thermal reaction 50-55h, and reaction is cooled to room temperature after terminating, and filters, and is dried to obtain the new lanthanum coordination
Polymer.
Preferably, the preparation method of the new lanthanum coordination polymer, comprises the following steps：By molar part by 0.06-
0.075 part of Lanthanum (III) nitrate and 0.11-0.12 parts 1, after the mixing of 2- phenylenediacetic Acids, add 350-430 part distilled water, after stirring,
The pH value of regulation system is 5-5.5, is filtered after stirring, and filtrate is placed in the stainless steel reaction for making lining with politef
In kettle, hydro-thermal reaction 53-54h is carried out at 160-163 DEG C, reaction is cooled to room temperature after terminating, and filters, and is dried to obtain described new
Lanthanum coordination polymer.
Preferably, the preparation method of the new lanthanum coordination polymer, comprises the following steps：By molar part by 0.08-
0.095 part of Lanthanum (III) nitrate and 0.13-0.14 parts 1, after the mixing of 2- phenylenediacetic Acids, add 250-320 part distilled water, after stirring,
The pH value of regulation system is 3.5-4.5, is filtered after stirring, and filtrate is placed in the rustless steel for making lining with politef anti-
In answering kettle, hydro-thermal reaction 51-52h is carried out at 170-174 DEG C, reaction is cooled to room temperature after terminating, and filters, be dried to obtain described new
Type lanthanum coordination polymer.
Preferably, the preparation method of the new lanthanum coordination polymer, comprises the following steps：By molar part by 0.07 part of nitre
After sour lanthanum and 0.13 part of 1,2- phenylenediacetic Acids mixing, 250 parts of distilled water are added, after stirring, the pH value of regulation system is 4,
Filter after stirring, filtrate is placed in and is made in the stainless steel cauldron of lining with politef, carry out hydro-thermal at 165 DEG C anti-
Answer 50h, reaction to be cooled to room temperature after terminating, filter, be dried to obtain the new lanthanum coordination polymer.
In the present invention, there is provided a kind of new lanthanum coordination polymer, its is stable in properties, can stablize the several months at room temperature, such as
Shown in Fig. 4, it just starts to decompose at 350 DEG C or so, is that its application provides the foundation；As shown in fig. 6, it has fluorescence, can
As potential fluorescent material；The preparation method of new lanthanum coordination polymer of the present invention, it is simple to operate, have adjusted and prepared
Parameters in journey, make the preparation method yield height of the new lanthanum coordination polymer, and reproducibility is good.
Description of the drawings
The minimum asymmetric cell figure of Fig. 1 new lanthanum coordination polymers of the present invention；
Two-dimension plane structure figure in Fig. 2 new lanthanum coordination polymers of the present invention；
Tridimensional network figure in Fig. 3 new lanthanum coordination polymers of the present invention；
The thermogravimetric collection of illustrative plates of new lanthanum coordination polymer prepared by Fig. 4 embodiment of the present invention 5；
The infared spectrum of new lanthanum coordination polymer prepared by Fig. 5 embodiment of the present invention 5；
The fluorescence pattern of new lanthanum coordination polymer prepared by Fig. 6 embodiment of the present invention 5.
Specific embodiment
The present invention is described in detail with reference to specific embodiment, it should be appreciated that embodiment is served only for illustrating this
It is bright, rather than for limiting the invention, any modification made on the basis of the present invention, equivalent etc. are at this
In bright protection domain.
New its chemical formula of lanthanum coordination polymer of the present invention is [La (PDAA)1.5(H2O)]·(H2O), wherein, PDAA
For 1,2- phenylenediacetic Acid anion ligands, the coordination polymer belongs to monoclinic system, C2/c space groups, the following institute of cell parameter
Show：β=92.677 (3) °,
New La (III) ion center of the lanthanum coordination polymer minimum asymmetric cell comprising a crystallography independence, one and half 1,
2- phenylenediacetic Acid anion ligands, a water of coordination molecule and a lattice hydrone, and La (III) is nine coordinations, is taken
It is the anti-prism geometric configuration in the single cap four directions of distortion；In the new lanthanum coordination polymer, 1,2- phenylenediacetic Acid anion ligand
Take the following two kinds coordination mode：
And 1,2- phenylenediacetic Acid anion ligand is connected to form three-dimensional netted by above two coordination mode with La (III)
Structure.
Embodiment 1
The preparation method of new lanthanum coordination polymer of the present invention, comprises the following steps：By molar part by 0.05 part of nitre
After sour lanthanum and 0.1 part of 1,2- phenylenediacetic Acids mixing, 200 parts of distilled water are added, after stirring 50min, adjusted using sodium hydroxide solution
Section pH value is 3, stirs under room temperature and filtered after 50min, and filtrate is transferred to the stainless steel cauldron for making lining with politef
In, hydro-thermal reaction 55h is carried out at 155 DEG C, room temperature is then naturally cooled to, filter, it is dried to obtain the new lanthanum coordination polymerization
Thing；Yield is 69%.
Embodiment 2
The preparation method of new lanthanum coordination polymer of the present invention, comprises the following steps：By molar part by 0.1 part of nitric acid
After lanthanum and 0.15 part of 1,2- phenylenediacetic Acids mixing, 500 parts of distilled water are added, after stirring 20min, adjusted using sodium hydroxide solution
PH value is 6, stirs under room temperature and filtered after 20min, filtrate is transferred to and is made in the stainless steel cauldron of lining with politef,
Hydro-thermal reaction 50h is carried out at 175 DEG C, room temperature is then naturally cooled to, is filtered, be dried to obtain the new lanthanum coordination polymer,
Yield is 71%.
Embodiment 3
The preparation method of new lanthanum coordination polymer of the present invention, comprises the following steps：By molar part by 0.06 part of nitre
After sour lanthanum and 0.12 part of 1,2- phenylenediacetic Acids mixing, 350 parts of distilled water are added, after stirring 35min, adjusted using sodium hydroxide solution
Section pH value is 5, stirs under room temperature and filtered after 45min, and filtrate is transferred to the stainless steel cauldron for making lining with politef
In, hydro-thermal reaction 54h is carried out at 160 DEG C, room temperature is then naturally cooled to, filter, it is dried to obtain the new lanthanum coordination polymerization
Thing；Yield is 72.3%.
Embodiment 4
The preparation method of new lanthanum coordination polymer of the present invention, comprises the following steps：By molar part by 0.075 part of nitre
After sour lanthanum and 0.11 part of 1,2- phenylenediacetic Acids mixing, 430 parts of distilled water are added, after stirring 20min, adjusted using sodium hydroxide solution
Section pH value is 5.5, stirs under room temperature and filtered after 40min, and filtrate is transferred to the stainless steel reaction for making lining with politef
In kettle, hydro-thermal reaction 53h is carried out at 163 DEG C, then naturally cool to room temperature, filtered, be dried to obtain the new lanthanum polycomplexation
Compound；Yield is 71.5%.
Embodiment 5
The preparation method of new lanthanum coordination polymer of the present invention, comprises the following steps：By molar part by 0.08 part of nitre
After sour lanthanum and 0.14 part of 1,2- phenylenediacetic Acids mixing, 250 parts of distilled water are added, after stirring 48min, adjusted using sodium hydroxide solution
Section pH value is 3.5, stirs under room temperature and filtered after 48min, and filtrate is transferred to the stainless steel reaction for making lining with politef
In kettle, hydro-thermal reaction 52h is carried out at 170 DEG C, then naturally cool to room temperature, filtered, be dried to obtain the new lanthanum polycomplexation
Compound；Yield is 70.8%.
Embodiment 6
The preparation method of new lanthanum coordination polymer of the present invention, comprises the following steps：By molar part by 0.095 part of nitre
After sour lanthanum and 0.13 part of 1,2- phenylenediacetic Acids mixing, 320 parts of distilled water are added, after stirring 38min, adjusted using sodium hydroxide solution
Section pH value is 4.5, stirs under room temperature and filtered after 25min, and filtrate is transferred to the stainless steel reaction for making lining with politef
In kettle, hydro-thermal reaction 51h is carried out at 174 DEG C, then naturally cool to room temperature, filtered, be dried to obtain the new lanthanum polycomplexation
Compound；Yield is 72.3%.
Embodiment 7
The preparation method of new lanthanum coordination polymer of the present invention, comprises the following steps：0.03mmol Lanthanum (III) nitrates with
After the mixing of 0.07mmol 1,2- phenylenediacetic Acid, 5ml distilled water is added, after stirring 25min, using sodium hydroxide solution pH is adjusted
It is worth for 2, stirs under room temperature and filtered after 35min, filtrate is transferred to and is made in the stainless steel cauldron of lining with politef,
150 DEG C carry out hydro-thermal reaction 40h, then naturally cool to room temperature, filter, and spontaneously dry at room temperature and obtain the new lanthanum and match somebody with somebody
Position polymer；Yield is 67.3%.
Embodiment 8
The preparation method of new lanthanum coordination polymer of the present invention, comprises the following steps：By 0.07mmol Lanthanum (III) nitrates with
After the mixing of 0.13mmol 1,2- phenylenediacetic Acid, 15ml distilled water is added, after stirring 40min, using sodium hydroxide solution pH is adjusted
It is worth for 7, stirs under room temperature and filtered after 43min, filtrate is transferred to and is made in the stainless steel cauldron of lining with politef,
180 DEG C carry out hydro-thermal reaction 40h, then naturally cool to room temperature, filter, with dry under field conditions (factors) after distilled water wash
To the new lanthanum coordination polymer；Yield is 67%.
New lanthanum coordination polymer to preparing in embodiment 5 carries out crystal structure test, and its predominant crystal data is such as
Shown in table 1：
The predominant crystal data of new lanthanum coordination polymer described in table 1
As known from Table 1, the new lanthanum coordination polymer belongs to monoclinic system, C2/c space groups, the following institute of cell parameter
Show：β=92.677 (3) °,
As shown in Figure 1, in new La (III) ion of the lanthanum coordination polymer minimum asymmetric cell comprising a crystallography independence
The heart, one and half 1,2- phenylenediacetic Acid anion ligands, a water of coordination molecule and a lattice hydrone, wherein La (III) is nine
Coordination, what is taken is the anti-prism geometric configuration in the single cap four directions of distortion, O1, O2 therein and O5, O6 come from two it is different
It is cloudy that 1,2- phenylenediacetic Acid anion ligand, O2#3, O3#2, O4#4 and O5#3 are respectively from four different 1,2- phenylenediacetic Acids
Ion ligand, O1W carrys out water of coordination molecule.As shown in Figure 2, in the new lanthanum coordination polymer, 1,2- phenylenediacetic Acid it is cloudy from
There are two kinds of different coordination modes in sub- part, wherein, one kind is hexa-coordinate, and one kind is pentacoordinate, as follows：
In the new lanthanum coordination polymer, 1, the 2- phenylenediacetic Acids anion ligand and La of two kinds of different coordination modes
(III) tridimensional network as shown in Figure 3 is constituted.
New lanthanum coordination polymer to implementing to be prepared in 5 carries out examination of infrared spectrum, its infrared spectrum spectrogram such as Fig. 5 institutes
Show, as shown in Figure 5, its main absworption peak is 3440cm-1、2927cm-1、1557cm-1、1384cm-1、1271cm-1、1210cm-1、731cm-1、646cm-1。
To in embodiment 5 prepare new lanthanum coordination polymer carry out thermogravimetric analysiss, its thermogravimetric collection of illustrative plates as shown in figure 4, by
Fig. 4 understands that its is stable in properties for the new lanthanum coordination polymer, just starts to decompose at 350 DEG C or so.
New lanthanum coordination polymer and 1,2- phenylenediacetic Acid part to preparing in embodiment 5 carries out solid fluorescence test,
As shown in figure 5, as shown in Figure 5, the new lanthanum coordination polymer and 1,2- phenylenediacetic Acid all have fluorescence to its fluorescence pattern
Matter.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any those familiar with the art the invention discloses technical scope in, technology according to the present invention scheme and its
Inventive concept equivalent or change in addition, all should be included within the scope of the present invention.
Claims (7)
1. a kind of preparation method of lanthanum coordination polymer, it is characterised in that the chemical formula of the lanthanum coordination polymer is [La
(PDAA)1.5(H2O)]·(H2O), wherein, PDAA is 1,2- phenylenediacetic Acid anion ligands, and the structural formula of PDAA is as follows：
The preparation method of the lanthanum coordination polymer is comprised the following steps：By molar part by 0.05-0.1 parts Lanthanum (III) nitrate and 0.1-
After 0.15 part of 1,2- phenylenediacetic Acids mixing, 200-500 part distilled water is added, after stirring, the pH value of regulation system is 2-4,
Filter after stirring, then filtrate is placed in autoclave, hydro-thermal reaction 40-50h is carried out at 150-165 DEG C, instead
Room temperature is cooled to after should terminating, is filtered, be dried to obtain the lanthanum coordination polymer.
2. the preparation method of lanthanum coordination polymer according to claim 1, it is characterised in that the lanthanum coordination polymer belongs to single
Oblique system, C2/c space groups, cell parameter is as follows：
β=92.677 (3) °,
3. the preparation method of lanthanum coordination polymer according to claim 1 or claim 2, it is characterised in that the lanthanum coordination polymer
In, 1,2- phenylenediacetic Acid anion ligand takes as follows two kind coordination mode：
4. the preparation method of lanthanum coordination polymer according to claim 1, it is characterised in that comprise the following steps：By nitric acid
Distilled water is added after lanthanum and the mixing of 1,2- phenylenediacetic Acid, the pH value of regulation system is 3-4 after stirring, is filtered after stirring, so
Filtrate is placed in autoclave afterwards, hydro-thermal reaction 48-50h is carried out at 160-165 DEG C, reaction is cooled to room after terminating
Temperature, filters, and is dried to obtain the lanthanum coordination polymer.
5. the preparation method of lanthanum coordination polymer according to claim 4, it is characterised in that comprise the following steps：By nitric acid
Distilled water is added after lanthanum and the mixing of 1,2- phenylenediacetic Acid, the pH value of regulation system is 4 after stirring, is filtered after stirring, then
Filtrate is placed in autoclave, hydro-thermal reaction 50h is carried out at 165 DEG C, reaction is cooled to room temperature after terminating, and filters, and does
It is dry to obtain the lanthanum coordination polymer.
6. the preparation method of lanthanum coordination polymer according to claim 4, it is characterised in that comprise the following steps：By mole
0.05-0.1 parts Lanthanum (III) nitrate and 0.1-0.15 parts 1 after the mixing of 2- phenylenediacetic Acids, are added 200-500 part distilled water by part, and stirring is
After even, the pH value of regulation system is 3-4, is filtered after stirring, and filtrate is placed in the rustless steel for making lining with politef
In reactor, hydro-thermal reaction 50h is carried out at 160-165 DEG C, reaction is cooled to room temperature after terminating, and filters, and is dried to obtain the lanthanum
Coordination polymer.
7. the preparation method of lanthanum coordination polymer according to claim 6, it is characterised in that comprise the following steps：By mole
After part is by 0.07 part of Lanthanum (III) nitrate and 0.13 part of 1,2- phenylenediacetic Acids mixing, 250 parts of distilled water are added, after stirring, adjust body
The pH value of system is 4, is filtered after stirring, and filtrate is placed in and is made in the stainless steel cauldron of lining with politef, 165
Hydro-thermal reaction 50h DEG C is carried out, reaction is cooled to room temperature after terminating, and filters, and is dried to obtain the lanthanum coordination polymer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410841910.2A CN104610325B (en) | 2014-12-30 | 2014-12-30 | Novel lanthanum coordination polymer and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410841910.2A CN104610325B (en) | 2014-12-30 | 2014-12-30 | Novel lanthanum coordination polymer and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104610325A CN104610325A (en) | 2015-05-13 |
| CN104610325B true CN104610325B (en) | 2017-04-26 |
Family
ID=53145003
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410841910.2A Expired - Fee Related CN104610325B (en) | 2014-12-30 | 2014-12-30 | Novel lanthanum coordination polymer and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104610325B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106675330A (en) * | 2016-12-15 | 2017-05-17 | 天长市金陵电子有限责任公司 | Electrostatic spraying coating of epoxy resin |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004000213A (en) * | 2002-04-26 | 2004-01-08 | Banyu Pharmaceut Co Ltd | Detection method of enzyme activity, and screening process using it |
| CN103007889B (en) * | 2012-12-31 | 2014-08-13 | 湖南大学 | Preparation method of metal-organic frame material La-BDC adsorbing CO2 and modified product of metal-organic frame material La-BDC |
-
2014
- 2014-12-30 CN CN201410841910.2A patent/CN104610325B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN104610325A (en) | 2015-05-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110358109B (en) | Luminous Zr-MOG metal organogel and synthesis method thereof | |
| CN104105664B (en) | Prepare the method for aluminosilicate zeolite SSZ-56 | |
| EP1641808B1 (en) | Method for producing chlorotris(triphenylphosphine) rhodium (i) | |
| CN104610325B (en) | Novel lanthanum coordination polymer and preparation method thereof | |
| CN106563437A (en) | Dy-containing nano lamellar structure complex photocatalyst and preparation method thereof | |
| CN110467641A (en) | A kind of more molybdic acid alcoxyl derivatives of Anderson type and one pot hydrothermal preparing process | |
| CN105884805B (en) | A kind of Cd (II) mixture coordination polymer and preparation method thereof | |
| CN109354695A (en) | A method of coordination adjusts preparation sheet metal-organic framework materials | |
| CN107043390A (en) | L phenylalanine Schiff base metal copper complex monocrystalline and preparation method thereof | |
| CN108341970B (en) | Coordination polymer based on 2, 5-thiophenedicarboxylic acid and gadolinium and preparation method thereof | |
| CN104130292B (en) | Three dimensional coordination polymer with double core structure and preparation method thereof | |
| CN108570143B (en) | Method for catalyzing polymerization of glycolide by using aluminum compound containing chiral cyclohexanediamine | |
| CN113617391B (en) | Uranium polyacid crystal and preparation method and application thereof | |
| CN102040572A (en) | Production method of benzofuranone | |
| CN105481812B (en) | Preparation method of 5-benzyloxy-4-oxo-4H-pyran-2-carboxylic acid | |
| CN106832315B (en) | A kind of two-dimentional lead coordination polymer with fluorescence property and preparation method thereof | |
| CN105481912B (en) | A kind of novel barium metal organic coordination polymer and its preparation method and application | |
| CN112645813A (en) | Preparation method of (R) -3-cyclohexenecarboxylic acid | |
| CN109369728A (en) | A kind of nickel complex and preparation method thereof based on phenylenediacetic Acid and double pyridinylmethylene hydrazine ligands | |
| CN108341969B (en) | Coordination polymer based on 2, 5-thiophenedicarboxylic acid and lanthanum and preparation method thereof | |
| CN106800659B (en) | A kind of three-dimensional lead coordination polymer with fluorescence property and preparation method thereof | |
| CN104130290B (en) | A kind of three-dimensional coordination polymer of two core clustering architectures and preparation method thereof | |
| CN110294694A (en) | A kind of improved preparation method of intermediate DAS of paratonere 177 | |
| Chen et al. | Molecular and Low‐dimensional Coordination Compounds of Copper (II) and 3, 5‐Dimethylpyrazole—Synthesis, Crystal Structure, and Properties | |
| CN105330703B (en) | A kind of ten core terbiums substitution arsenic tungsten oxygen silicate nanometer cluster compound and its preparation method and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170426 Termination date: 20171230 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |