CN108821350A - A kind of preparation method of transition metal salt amine complex - Google Patents
A kind of preparation method of transition metal salt amine complex Download PDFInfo
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- CN108821350A CN108821350A CN201810526368.XA CN201810526368A CN108821350A CN 108821350 A CN108821350 A CN 108821350A CN 201810526368 A CN201810526368 A CN 201810526368A CN 108821350 A CN108821350 A CN 108821350A
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- -1 transition metal salt amine Chemical class 0.000 title claims abstract description 29
- 229910052723 transition metal Inorganic materials 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000004202 carbamide Substances 0.000 claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910021381 transition metal chloride Inorganic materials 0.000 claims abstract description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 11
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 10
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 8
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 7
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 6
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 5
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 5
- 150000001298 alcohols Chemical class 0.000 claims description 5
- 238000005660 chlorination reaction Methods 0.000 claims description 5
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 5
- 235000002867 manganese chloride Nutrition 0.000 claims description 5
- 239000011565 manganese chloride Substances 0.000 claims description 5
- 229940099607 manganese chloride Drugs 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 235000005074 zinc chloride Nutrition 0.000 claims description 5
- 239000011592 zinc chloride Substances 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 150000003624 transition metals Chemical class 0.000 claims description 3
- 229960004756 ethanol Drugs 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims 1
- 238000000527 sonication Methods 0.000 claims 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 27
- 229910021529 ammonia Inorganic materials 0.000 abstract description 10
- 238000010438 heat treatment Methods 0.000 abstract description 7
- 238000005406 washing Methods 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract description 2
- 238000005119 centrifugation Methods 0.000 abstract 1
- 239000007787 solid Substances 0.000 description 29
- 239000000243 solution Substances 0.000 description 17
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 14
- 239000004810 polytetrafluoroethylene Substances 0.000 description 14
- 239000000460 chlorine Substances 0.000 description 10
- 238000010586 diagram Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 7
- 229910001220 stainless steel Inorganic materials 0.000 description 7
- 239000010935 stainless steel Substances 0.000 description 7
- 238000002425 crystallisation Methods 0.000 description 6
- 230000008025 crystallization Effects 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 238000001291 vacuum drying Methods 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 5
- 229910052793 cadmium Inorganic materials 0.000 description 5
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 5
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 5
- 238000002604 ultrasonography Methods 0.000 description 5
- 239000010949 copper Substances 0.000 description 4
- 239000011572 manganese Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 230000000840 anti-viral effect Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 2
- 239000004312 hexamethylene tetramine Substances 0.000 description 2
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 229910007337 Zn(NH3)2Cl2 Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 235000017168 chlorine Nutrition 0.000 description 1
- 239000011365 complex material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/12—Complexes with ammonia
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/006—Compounds containing, besides cobalt, two or more other elements, with the exception of oxygen or hydrogen
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention discloses a kind of preparation method of transition metal salt amine complex, it is sufficiently mixed urea and transition metal chloride are sonicated in alcohol, at a certain temperature heating reaction prepare transition metal salt amine complex, by centrifugation, washing, again be centrifuged and drying and other steps acquisition target product.With the transition metal salt amine complex sample purity height of this method synthesis, better crystallinity degree, and the method is simple with synthesis technology and equipment, low in cost and navigability is good, it is only necessary to the target product of specific ligancy ammonia can be obtained by factors such as molar ratio, reaction temperature or the reaction time of control reaction mass.
Description
Technical field
The present invention relates to a kind of preparation methods of transition metal salt amine complex, belong to the preparation field of nano material.
Background technique
Transition metal salt amine complex is the product after metal and ammonia coordination, in the separation and storage of vehicle-mounted hydrogen storage, refrigeration, ammonia
It deposits, antiviral and medicine or even catalytic field etc. have important application.The coordination mode of transition metal salt amine complex
Multiplicity makes the cooperation species of transition metal and ammonia variation multiplicity, and the difference of coordination mode is to transition metal salt amine complex
Color, crystalline form and property all have an impact, and the quality of dispersibility, homogeneity is to transition metal salt amine complex material application performance
Also there is large effect.The preparation method of transition metal salt amine complex is mainly passed through ammonia in corresponding metal salt solution
Or ammonium chloride is added in the aqueous solution of metal oxide.It is passed through ammonia into metal salt solution and prepares the cooperation of transition metal salt ammonia
Ammonia plays the role of precipitating reagent when object, and ammonia will lead to ammonia local over-concentration in the solution when being passed through solution, leads to gained
Product particles bad dispersibility is reunited serious, and pattern control is difficult；The salt containing ammonium is added in metal oxide solution and needs solution
It can just be crystallized after system is cooling and corresponding transition metal salt amine complex is precipitated, or needed under expensive catalyst action
Corresponding target product can be obtained.
Summary of the invention
In order to overcome the shortcomings of the prior art, the present invention provides one kind and simply prepares transition metal salt amine complex
Method, cheap, quick and easy, navigability is strong, can substantially reduce the preparation of transition metal salt amine complex fund cost and
Time cost, transition metal salt amine complex obtained purity is high, better crystallinity degree, coordination mode is controllable, in vehicle-mounted hydrogen storage, system
Cold, ammonia separation and storage, antiviral and medicine or even catalytic field etc. have corresponding application.
The technical solution adopted by the present invention is as follows：
A kind of preparation method of transition metal salt amine complex, includes the following steps：
（1）It weighs urea and Anhydrous transition metal chloride at room temperature, alcohols solvent is added, stir after 2 ~ 6h at 20 ~ 40 DEG C
It is ultrasonically treated 10 ~ 35min, the stainless steel hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE) material is then injected by miillpore filter
In, in 100 ~ 200 DEG C of 3 ~ 30h of reaction, generate transition metal salt amine complex；
（2）It is cooled to room temperature to reaction kettle, by step（1）Transition metal salt amine complex obtained is 2000 ~ 5000r/min's
It is centrifuged 10 ~ 15min under revolving speed, then washes away unreacted transition metal chloride with anhydrous methanol or dehydrated alcohol, again
Under the revolving speed of 6000 ~ 10000r/min be centrifuged 5 ~ 15min after, 40 ~ 60 DEG C be dried in vacuo 2 ~ can be obtained for 24 hours target produce
Object.
Preferably, step（1）The molar ratio of middle urea and Anhydrous transition metal chloride is 1:1~1:12.
Preferably, step（1）Middle transition metal chloride is caddy, nickel chloride, cobalt chloride, zinc chloride, manganese chloride, chlorine
Change one of copper, they are all the transition metal chlorides that chemical valence is divalent.
Preferably, step（1）Middle alcohols solvent and urea mol ratio are 25:1~45:1.
Preferably, step（1）Middle alcohol organic solvent is one of methanol, ethyl alcohol, n-butanol, ethylene glycol.
Preferably, step（1）The aperture of middle miillpore filter is 0.45 μm.
Advantages of the present invention is as follows：（1）Reaction can be facilitated using urea as precipitating reagent using sluggish precipitation
Ground controls entire precipitation process, is allowed in equilibrium state and slowly carry out, products therefrom purity is high, better crystallinity degree, particle
Intergranular good dispersion and size is more uniform；（2）Transition metal salt amine complex synthesis technology and equipment are simple, raw material is easy to get, at
This cheap and navigability is good, it is only necessary to can by factors such as molar ratio, reaction temperature, the reaction time of control reaction mass
Obtain the target product of specific ligancy ammonia.
Detailed description of the invention
Fig. 1 is six cobaltammine Co (NH of dichloride made from embodiment 13)6Cl2XRD diagram and its standard diagram；
Fig. 2 is that diamminodichloro made from embodiment 6 closes cadmium Cd (NH3)2Cl2XRD diagram and its standard diagram；
Fig. 3 is six cobaltammine Co (NH of dichloride made from embodiment 13)6Cl2SEM figure；
Fig. 4 is that diamminodichloro made from embodiment 6 closes cadmium Cd (NH3)2Cl2SEM figure.
Specific embodiment
The present invention is described in further details below with reference to embodiment, but protection scope of the present invention is not limited in described
Hold.
Embodiment 1：Six cobaltammine of dichloride（Co(NH3)6Cl2）Preparation method
Weighing molar ratio at room temperature is 1:6 urea and cobalt chloride is placed in the small beaker of 50mL, and addition is with urea mol ratio
45:1 anhydrous methanol stirs and gained clarified solution is transferred to after 4h to pre-set temperature be to surpass in 40 DEG C of ultrasonic washing instrument
Sound 30min is to promote cobalt chloride sufficiently to dissolve.Clarified solution is set to be injected into appearance by the filtering head in 0.45 μm of aperture with syringe
Amount is that heating crystallization reaction is stood at 180 DEG C in the stainless steel hydrothermal reaction kettle that 50mL liner is polytetrafluoroethylene (PTFE) material
10h is cooled to room temperature to reaction kettle after completion of the reaction, and products therefrom is centrifuged under the revolving speed of 5000r/min with centrifuge
10min collects solids；Obtained solid object is washed away into unreacted cobalt chloride with anhydrous methanol, operating 2 ~ 5 times repeatedly makes not instead
The cobalt chloride answered thoroughly is cleaned；The solids centrifuge washed is centrifuged to 10min to collect admittedly under the revolving speed of 8000r/min
Body object；Obtained solid object is placed in a vacuum drying oven and obtains six cobaltammine of product dichloride for 24 hours in 60 DEG C of dryings.Its XRD diagram and
Its standard diagram as shown in Figure 1, product XRD spectrum and joint committee（ICDD）The PDF2-2003 of publication
No.77-0222MH standard spectrogram is consistent, and lattice constant a=10.122, b=10.122, c=10.122, α=β=γ=90 ° belong to
Fm-3m space lattice respectively corresponds 111,220,400 crystal faces in 2 θ=15.148 °, 24.859 °, 35.444 °, and peak type is more sharp
Sharp and free from admixture peak illustrates that the six cobaltammine crystallinity of dichloride of this method preparation is high, purity is good, and SEM figure is as shown in Figure 3.
Embodiment 2：Eight ammino manganese of dichloride（Mn(NH3)8Cl2）Preparation method
Weighing molar ratio at room temperature is 1:12 urea and manganese chloride is placed in the small beaker of 50mL, and addition is with urea mol ratio
25:1 n-butanol stirs and gained clarified solution is transferred to after 6h to pre-set temperature be ultrasound in 30 DEG C of ultrasonic washing instrument
20min is to promote manganese chloride sufficiently to dissolve.Clarified solution is set to be injected into capacity by the filtering head in 0.45 μm of aperture with syringe
To stand heating crystallization at 140 DEG C and reacting 15h in stainless steel hydrothermal reaction kettle that 50mL liner is polytetrafluoroethylene (PTFE) material,
It is cooled to room temperature after completion of the reaction to reaction kettle, products therefrom centrifuge is centrifuged to 15min receipts under the revolving speed of 2000r/min
Collect solids；Obtained solid object is washed away into unreacted manganese chloride with dehydrated alcohol, operating 2 ~ 5 times repeatedly makes unreacted chlorination
Manganese is thoroughly cleaned；The solids centrifuge washed is centrifuged to 10min under the revolving speed of 10000r/min and collects solids；It will
Obtained solid object is placed in a vacuum drying oven obtains eight ammino manganese of product dichloride in 40 DEG C of dryings for 24 hours.
Embodiment 3：Dichloride hexamine nickel（Ni(NH3)6Cl2）Preparation method
Weighing molar ratio at room temperature is 1:6 urea and nickel chloride is placed in the small beaker of 50mL, and addition is with urea mol ratio
35:1 dehydrated alcohol, stirs after 3h for gained clarified solution to be transferred to and pre-sets ultrasound in the ultrasonic washing instrument that temperature is 40 DEG C
10min is to promote nickel chloride sufficiently to dissolve.Clarified solution is set to be injected into capacity by the filtering head in 0.45 μm of aperture with syringe
To stand heating crystallization at 120 DEG C and reacting 6h, instead in stainless steel hydrothermal reaction kettle that 50mL liner is polytetrafluoroethylene (PTFE) material
It is cooled to room temperature after answering to reaction kettle, products therefrom centrifuge is centrifuged to 13min collection under the revolving speed of 3500r/min
Solids；Obtained solid object is washed away into unreacted nickel chloride with dehydrated alcohol, operating 2 ~ 5 times repeatedly makes unreacted nickel chloride
Thoroughly clean；The solids centrifuge washed is centrifuged to 15min under the revolving speed of 6000r/min and collects solids；By institute
Solids is placed in a vacuum drying oven and obtains product dichloride hexamine nickel in 50 DEG C of dry 12h.
Embodiment 4：Diamminodichloro closes zinc（Zn(NH3)2Cl2）Preparation method it is as follows：
Weighing molar ratio at room temperature is 1:8 urea and zinc chloride is placed in the small beaker of 50mL, and addition is with urea mol ratio
30:1 ethylene glycol stirs and gained clarified solution is transferred to after 6h to pre-set temperature be ultrasound in 20 DEG C of ultrasonic washing instrument
35min is to promote zinc chloride sufficiently to dissolve.Clarified solution is set to be injected into capacity by the filtering head in 0.45 μm of aperture with syringe
To stand heating crystallization reaction at 160 DEG C for 24 hours in stainless steel hydrothermal reaction kettle that 50mL liner is polytetrafluoroethylene (PTFE) material,
It is cooled to room temperature after completion of the reaction to reaction kettle, products therefrom centrifuge is centrifuged to 10min receipts under the revolving speed of 4000r/min
Collect solids；Obtained solid object is washed away into unreacted zinc chloride with dehydrated alcohol, operating 2 ~ 5 times repeatedly makes unreacted chlorination
Zinc is thoroughly cleaned；The solids centrifuge washed is centrifuged to 15min under the revolving speed of 8000r/min and collects solids；It will
Obtained solid object, which is placed in a vacuum drying oven, obtains product diamminodichloro conjunction zinc in 60 DEG C of dry 18h.
Embodiment 5：Diamminodichloro closes copper（Cu(NH3)2Cl2）Preparation method
Weighing molar ratio at room temperature is 1:1 urea and copper chloride is placed in the small beaker of 50mL, and addition is with urea mol ratio
25:1 n-butanol stirs and gained clarified solution is transferred to after 2h to pre-set temperature be ultrasound in 35 DEG C of ultrasonic washing instrument
15min is to promote copper chloride sufficiently to dissolve.Clarified solution is set to be injected into capacity by the filtering head in 0.45 μm of aperture with syringe
To stand heating crystallization at 200 DEG C and reacting 3h, instead in stainless steel hydrothermal reaction kettle that 50mL liner is polytetrafluoroethylene (PTFE) material
It is cooled to room temperature after answering to reaction kettle, products therefrom centrifuge is centrifuged to 15min collection under the revolving speed of 3000r/min
Solids；Obtained solid object is washed away into unreacted copper chloride with dehydrated alcohol, operating 2 ~ 5 times repeatedly makes unreacted copper chloride
Thoroughly clean；The solids centrifuge washed is centrifuged to 10min under the revolving speed of 8000r/min and collects solids；By institute
Solids be placed in a vacuum drying oven in 60 DEG C of dry 2h obtain product diamminodichloro conjunction copper.
Embodiment 6：Diamminodichloro closes cadmium（Cd(NH3)2Cl2）Preparation method
Weighing molar ratio at room temperature is 1:6 urea and caddy is placed in the small beaker of 50mL, and addition is with urea mol ratio
30:1 ethylene glycol stirs and gained clarified solution is transferred to after 6h to pre-set temperature be ultrasound in 25 DEG C of ultrasonic washing instrument
20min is to promote caddy sufficiently to dissolve.Clarified solution is set to be injected into capacity by the filtering head in 0.45 μm of aperture with syringe
To stand heating crystallization at 100 DEG C and reacting 30h in stainless steel hydrothermal reaction kettle that 50mL liner is polytetrafluoroethylene (PTFE) material,
It is cooled to room temperature after completion of the reaction to reaction kettle, products therefrom centrifuge is centrifuged to 10min receipts under the revolving speed of 5000r/min
Collect solids；Obtained solid object is washed away into unreacted caddy with dehydrated alcohol, operating 2 ~ 5 times repeatedly makes unreacted chlorination
Cadmium is thoroughly cleaned；The solids centrifuge washed is centrifuged to 5min under the revolving speed of 10000r/min and collects solids；It will
Obtained solid object, which is placed in a vacuum drying oven, obtains product diamminodichloro conjunction cadmium in 60 DEG C of dry 12h.Its XRD diagram and its standard drawing
Compose XRD spectrum and joint committee as shown in figure 3, product（ICDD）The PDF#72-0574 standard spectrogram one of publication
Cause, lattice constant a=8.180, b=8.290, c=3.960, α=β=γ=90 ° belong to Cmmm space lattice, 2 θ=15.204 °,
21.419 ° and 31.418 ° respectively correspond 110,020,201 crystal faces, and peak type is relatively sharp and free from admixture peak illustrates product crystallinity
Height, purity are good.Its SEM figure is as shown in Figure 4.
Claims (6)
1. a kind of preparation method of transition metal salt amine complex, includes the following steps：
（1）Urea and Anhydrous transition metal chloride are taken at room temperature, alcohols solvent is added, and are surpassed after stirring 2 ~ 6h at 20 ~ 40 DEG C
Then 10 ~ 35min of sonication is injected in hydrothermal reaction kettle by miillpore filter, in 100 ~ 200 DEG C of 3 ~ 30h of reaction, generate transition
Metal salt amine complex；
（2）It is cooled to room temperature to reaction kettle, by step（1）Transition metal salt amine complex obtained is 2000 ~ 5000r/min's
It is centrifuged 10 ~ 15min under revolving speed, then washes away unreacted transition metal chloride with anhydrous methanol or dehydrated alcohol, again
Under the revolving speed of 6000 ~ 10000r/min be centrifuged 5 ~ 15min after, 40 ~ 60 DEG C be dried in vacuo 2 ~ can be obtained for 24 hours target produce
Object.
2. preparation method according to claim 1, which is characterized in that step（1）Middle urea and Anhydrous transition metal chlorination
The molar ratio of object is 1:1~1:12.
3. preparation method according to claim 1 or 2, which is characterized in that transition metal chloride is caddy, chlorination
One of nickel, cobalt chloride, zinc chloride, manganese chloride, copper chloride.
4. preparation method according to claim 1, which is characterized in that step（1）Middle alcohols solvent is with urea mol ratio
25:1~45:1。
5. preparation method according to claim 1 or 4, which is characterized in that alcohols solvent is methanol, ethyl alcohol, n-butanol, second
One of glycol.
6. preparation method according to claim 1, which is characterized in that step（1）The aperture of middle miillpore filter is 0.45 μm.
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