CN106279217B - Cadmium organic supermolecular solid [Cd (ppa) (bpe)]nAnd preparation method - Google Patents
Cadmium organic supermolecular solid [Cd (ppa) (bpe)]nAnd preparation method Download PDFInfo
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- CN106279217B CN106279217B CN201610565442.XA CN201610565442A CN106279217B CN 106279217 B CN106279217 B CN 106279217B CN 201610565442 A CN201610565442 A CN 201610565442A CN 106279217 B CN106279217 B CN 106279217B
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- 229910052793 cadmium Inorganic materials 0.000 title claims abstract description 23
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000007787 solid Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 8
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- 239000002253 acid Substances 0.000 claims abstract description 5
- 239000003049 inorganic solvent Substances 0.000 claims abstract description 5
- 239000003960 organic solvent Substances 0.000 claims abstract description 5
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000010276 construction Methods 0.000 claims abstract description 4
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims abstract description 4
- 230000001413 cellular effect Effects 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract 4
- 239000013078 crystal Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 229910002651 NO3 Inorganic materials 0.000 claims description 7
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical class CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 7
- JUJWROOIHBZHMG-UHFFFAOYSA-N pyridine Substances C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 3
- 125000005504 styryl group Chemical group 0.000 claims description 3
- 125000004429 atom Chemical group 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 239000012046 mixed solvent Substances 0.000 claims description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 claims description 2
- 238000010189 synthetic method Methods 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims 1
- ZHUXMBYIONRQQX-UHFFFAOYSA-N hydroxidodioxidocarbon(.) Chemical compound [O]C(O)=O ZHUXMBYIONRQQX-UHFFFAOYSA-N 0.000 claims 1
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 9
- 238000009825 accumulation Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 14
- 239000000126 substance Substances 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 4
- 238000000634 powder X-ray diffraction Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000012452 mother liquor Substances 0.000 description 3
- 239000002689 soil Substances 0.000 description 3
- 239000003381 stabilizer Substances 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 238000002050 diffraction method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 238000003911 water pollution Methods 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 206010023126 Jaundice Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006388 chemical passivation reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000010537 deprotonation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000035558 fertility Effects 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 230000008635 plant growth Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000005588 protonation Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
Classifications
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- 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
- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic Table
- C07F3/003—Compounds containing elements of Groups 2 or 12 of the Periodic Table without C-Metal linkages
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
Abstract
The invention belongs to heavy metal accumulation Solid-state Chemistry technical field, and in particular to cadmium organic supermolecular solid [Cd (ppa) (bpe)]n, its cellular construction is as follows:Present invention also offers the preparation method of the supermolecule solid of cadmium, using solvent process for thermosynthesizing by cadmium nitrate, organic carboxyl acid H2Ppa and nitrogen component bpe set out and are prepared.The supermolecule solid matter of the present invention is insoluble in inorganic or organic solvent, has higher heat endurance, is a kind of supramolecular system of new cadmium.
Description
Technical field
The invention belongs to heavy metal accumulation Solid-state Chemistry technical field, and in particular to cadmium-organic supermolecular solid [Cd
(ppa)(bpe)]nAnd preparation method.
Background technology
In water pollution caused by human production activity, water pollution most serious caused by industry, it is more containing pollutant, into
Divide complexity, not only be not easy to purify in water, and handle also relatively difficult.In production, heavy metal is usually used, it is untreated useless
Water discharges, and causes in environment content of beary metal apparently higher than background value, causes the phenomenon of the deterioration of the ecological environment.Wherein cadmium is to make agriculture
The contaminated heavy metal element most universal, bio-toxicity is most strong in field, its chemism in the environment is strong, and existing forms are more, shifting
Dynamic property is big, toxicity is lasting, jeopardizes human health easily by the enrichment of food chain.
For Heavy-Metal-Contaminated Environments reparation be mainly using physics, chemistry or biology method transfer, absorb, degraded or
The heavy metal in waste water is converted, the concentration of heavy metal in waste water is reduced to level of security.At present, the place of heavy metal cadmium waste water
Reason method has phytoremediation, biological prosthetic and chemical passivation reparation etc..
Phytoremediation technology typically cost is low, can reduce heavy metal ion content, can also improve soil organic content and
Soil fertility, but plant is limited to the patience of cadmium, is unsuitable for the processing of large amount of sewage, and super enrichment cadmium plant growth is slow, leads to
Normal repairing efficiency is longer, it is difficult to meets quick restoring cadmium polluted requirement.Therefore, new and effective, inexpensive cadmium enrichment is sought
Chemical system receives the extensive concern in each field.
For cadmium ion to O, N has stronger affinity, and solubility is big in water, therefore be relatively insoluble in water contains O, N groups
Chemical stabilizer can adjust and change the physics of cadmium, chemical property, so as to reduce its concentration in soil environment and can move
Shifting property.
The content of the invention
It is an object of the invention to provide a kind of cadmium-organic supermolecular solid [Cd (ppa) (bpe)]n, there is higher thermostabilization
Property, it can will effectively be hydrated cadmium ion and be converted into stable complex compound, be a kind of chemical system of new cadmium, be used in
The enrichment of cadmium Cd ions in sewage.
Technical scheme is as follows:
Proposed by the present invention is cadmium-organic supermolecular solid [Cd (ppa) (bpe)]n, its cellular construction is as follows:
Wherein ppa2-It is organic carboxyl acid H2Ppa sloughs the component after 2 carboxyl hydrogen atoms, H2Ppa structural formula isDescribed bpe structural formula is
Specifically, described supermolecule is by component H2Ppa and bpe is prepared with cadmium nitrate, the H2Ppa is that one kind contains
The flexible multiple tooth organic carboxyl acid of styryl, the bpe are a kind of bidentate components of vinyl containing pyridine, in part carboxyl O and
Stable metal-organic supermolecular solid is formed between pyridine N and central atom Cd, is insoluble in inorganic or organic solvent.
Present invention also offers supermolecule [Cd (ppa) (bpe)]nPreparation method, comprise the following steps:Using solvent heat
Synthetic method, raw material is weighed by following mol ratio:H2Ppa ︰ bpe ︰ Cd (NO3)2︰ DMA ︰ H2The mol ratio of O ︰ triethylamines is 12
~18:4~8:12~18:1866~3732:8000~116000:7~11, DMA are solvent DMA.
In DMA and water mixed solvent, raw material is mixed into 0.5~1.5h, at 110~130 DEG C in closed container
Lower reaction 2~4 days;After natural cooling, filter, washing, it is target product to obtain faint yellow bulk crystals.
Preferably, H2Ppa ︰ bpe ︰ Cd (NO3)2︰ DMA ︰ H2The mol ratio of O ︰ triethylamines is 15:6:15:3732:6000:7.
Preferably, described closed container is reactor.
Preferably, the described reaction time is 3 days.
Preferably, described reaction temperature is 120 DEG C.
Preferably, described faint yellow bulk crystals spontaneously dry successively with DMA, water washing.
Beneficial effects of the present invention:
H selected by chemical stabilizer of the present invention2Ppa and bpe, chromophoric group is conjugated containing styryl, easily by
Conventional ultraviolet instrumentation detection;They are insoluble in the protic bonding solvents such as water, alcohol-water, gradually increase with the rise solubility of temperature
Greatly, there is preferable concentration effect for hydration cadmium ion.From source of the cadmium nitrate as cadmium ion, be advantageous to center cadmium from
The release of son, and then advantageously form a kind of supermolecule solid of the cadmium of stabilization.Gained cadmium-organic supermolecular solid, it is difficult
Inorganic or organic solvent is dissolved in, can be easily separated;With relatively good heat endurance, 290 DEG C of skeletons start to decompose (see Fig. 5), this
Property is laid a good foundation for the separation of cadmium and enriching and recovering.In addition, the preparation method of the present invention is simple to operate, yield can reach
53.8%~68.0%.
The present invention have is easy to implement, treatment cost it is cheap and administer speed it is fast the advantages that, be adapted in, slight heavy metal cadmium
The purified treatment of contaminant water.
Brief description of the drawings
Fig. 1 H2Ppa structural formula;
Fig. 2 bpe structural formula;
Fig. 3 [Cd (ppa) (bpe)]nCellular construction;
Fig. 4 crystal jaundice green fluorescence photo (under 365 ultra violet lamps);
Thermogravimetric curve (the air atmosphere of Fig. 5 complexs;Abscissa-temperature;Ordinate-residual percentage);
Fig. 6 X-ray powder diffractions style (abscissa-angle;Ordinate-diffracted intensity).
Embodiment
In the dissymmetrical structure unit of complex, include the ppa of complete deprotonation2-Part and the bpe of protonation match somebody with somebody
Body.Each cadmium ion and two ppa2-Carboxyl oxygen bidentate chelating on part, with another ppa2-Combined with monodentate, with
And the nitrogen-atoms connection on two bpe.The solid finds that yield is up to 65% after experiment, turns into a kind of new enrichment weight cadmium
Supramolecular system.
Part H selected by the present invention2Ppa structural formulas are shown in Fig. 1, and part bpe structural formulas are shown in Fig. 2, part H2Ppa and part
Bpe conjugated degree is larger.H during the course of the reaction2Ppa has sloughed 2 H atoms, becomes ppa2-, and combined with cadmium ion.
The product arrived is with H2Ppa is according to calculating yield, i.e., according to H in reactant2Ppa and [Cd (ppa) (bpe)]nMol ratio, calculate
Go out [Cd (ppa) (bpe)] that should be obtained in theorynQuality, further according to [Cd (ppa) (bpe)] actually obtainednQuality, the latter
The ratio for accounting for the former is yield.
X-ray single crystal diffraction analysis is carried out to final product in the present invention, obtains its crystal structure;And to final product
A series of signs are carried out, such as elementary analysis, infrared, thermogravimetric, X-ray powder diffraction.
The preparation of 1 complex of the present invention of embodiment
Raw material is weighed by following mol ratio:H2Ppa ︰ bpe ︰ Cd (NO3)2︰ DMA ︰ H2The mol ratio of O ︰ triethylamines is 12:
4:12:1866:8000:7.
It is placed in 50mL glass beakers, raw material is mixed into 0.5 hour (h), is then transferred in 25mL reactors,
Reacted at 100 DEG C two days later, naturally cool to room temperature, it was observed that light yellow crystal, as target product [Cd (ppa)
(bpe)]n.Target product is filtered out from mother liquor, successively with DMA, water washing, spontaneously dried after complete.
Product [Cd (ppa) (bpe)]nIn C, H, N element carry out elementary analysis, calculated value (%):C,59.90;H,
4.23;N,4.25.Actually measured (%):C,59.81;H,4.51;N,4.22.FT-IR (KBr, cm-1):,3038(w),2964
(w), 1632 (m), 1609 (vs), 1494 (m), 1398 (vs), 1245 (s), 1221 (s), 1121 (m), 889 (m), 836 (m).
Explanation:Elemental analysis value is measured by Perkin-Elmer2400 elemental analysers;Infrared spectrum is by Nicolet Impact
410FTIR spectrometers are bottom in 400-4000cm using KBr-1In the range of measure.
X-ray single crystal diffraction analysis is carried out to obtained target product, obtains its crystal structure (see Fig. 3).Demonstrate this
The each cadmium ion of complex uses seven coordination modes, four ppa2-Two on five oxygen atoms and two bpe on carboxylate radical
Nitrogen-atoms is connected with cadmium ion respectively.
Yellow green is shown as to target product fluorescence photo (see Fig. 4).Entered with Shimadzu XRD-6100 type x-ray diffractometers
Row powder diffraction is tested, and the peak energy for testing collection of illustrative plates of the peak of collection of illustrative plates with being simulated through mercury softwares matches well, illustrates that this is brilliant
Body is target product, and sample purity is higher (see Fig. 6).
By the present embodiment repeatedly, actual production obtains [Cd (ppa) (bpe)]nQuality be maintained at 54.8~
60.4mg, it is calculated as yield 56.7%~68%.
The preparation of 2 complex of the present invention of embodiment
Raw material is weighed by following mol ratio:H2Ppa ︰ bpe ︰ Cd (NO3)2︰ DMA ︰ H2The mol ratio of O ︰ triethylamines is 15:
6:15:2799:9800:9.
It is placed in 50mL glass beakers, raw material is mixed into 1 hour (h), is then transferred in 25mL reactors,
After being reacted three days at 110 DEG C, room temperature is naturally cooled to, it was observed that light yellow crystal, i.e. target product, it is filtered from mother liquor
Out, spontaneously dried successively with DMA, water washing after complete.
Elementary analysis, infrared, fluorescence, X-ray powder diffraction sign are carried out to product, obtains data and the phase of embodiment 1
Seemingly.Crystal structure does not change explanation made from embodiment 2 and product is purer, and performance does not also change (see Fig. 6).
By the present embodiment repeatedly, obtained [Cd (ppa) (bpe)] according to actual productionn52.4~61.3mg of quality,
Calculated yield is 55.4%~65.2%.
The preparation of 3 complex of the present invention of embodiment
Raw material H is weighed by following mol ratio2Ppa ︰ bpe ︰ Cd (NO3)2︰ DMA ︰ H2The mol ratio of O ︰ triethylamines is 18:8:
18:3732:116000:11.It is placed in 50mL glass beakers, raw material is mixed into 1.5h, is then transferred to 25mL reactors
In, after being reacted four days under 120 degree, room temperature is naturally cooled to, it was observed that light yellow crystal, i.e. target product, by it from mother liquor
In filter out, successively with DMA, water washing, spontaneously dried after complete.
Elementary analysis, infrared, fluorescence, X-ray powder diffraction sign are carried out to product, obtains data and the phase of embodiment 1
Seemingly.Explanation crystal structure made from embodiment 3 does not change and product is purer (see Fig. 6).
By the present embodiment repeatedly, obtained [Cd (ppa) (bpe)] according to actual productionn53.7~59.6mg of quality,
Calculated yield is 53.8%~62.8%.
As shown in Figure 5, cadmium complex [Cd (ppa) (bpe)] is madenWeighed feed molar proportioning is H2Ppa ︰ bpe ︰ Cd
(NO3)2︰ DMA ︰ H2The mol ratio of O ︰ triethylamines is 12~18:4~8:12~18:1866~3732:8000~116000:7~
11, it is more suitable to be placed at 100 DEG C~120 DEG C, and the reaction time is 2~4 days more suitable:Cadmium complex [the Cd of gained
(ppa)(bpe)]nPurer, cadmium effectively can be converted into stable complex state from hydrated ion state by yield up to 68%.
As seen from the above-described embodiment, the chemical stabilizer used in the present invention is organic component h2ppa, and bpe is difficult at normal temperatures
It is dissolved in water, temperature rise solubility increase;Cadmium ion can be enriched with the conditions of solvent heat, the supermolecule solid of gained compared with
Also inorganic or organic solvent is insoluble under high-temperature, is separated and enriching and recovering cadmium.
Claims (7)
1. cadmium-organic supermolecular solid [Cd (ppa) (bpe)]n, its cellular construction is as follows:
Wherein, a cadmium ion and two ppa2-Match somebody with somebody
Carboxyl oxygen bidentate chelating on body, with another ppa2-Connected with the nitrogen-atoms on monodentate combination and two bpe, it is described
Ppa is organic carboxyl acid H2Ppa sloughs the component after 2 carboxyl hydrogen atoms, carboxylic acid H2Ppa structural formula isThe nitrogen component bpe structures are
2. cadmium as claimed in claim 1-organic supermolecular solid [Cd (ppa) (bpe)]n, it is characterised in that:By H2ppa、bpe
It is prepared with cadmium nitrate, the H2Ppa is a kind of flexible multiple tooth organic carboxyl acid containing styryl, and the bpe is that one kind contains
The bidentate component of pyridine vinyl, it is solid that stable metal-organic supermolecular is formed between carboxyl O and pyridine N and central atom Cd
Body, it is insoluble in inorganic or organic solvent.
3. cadmium-organic supermolecular solid [Cd (ppa) (bpe)] described in claim 1 or 2nSynthetic method, it is characterised in that
Comprise the following steps:
Using solvent process for thermosynthesizing, raw material is weighed by following mol ratio:H2Ppa ︰ bpe ︰ Cd (NO3)2︰ DMA ︰ H2O ︰ triethylamines
Mol ratio be 12~18:4~8:12~18:1866~3732:8000~116000:7~11, DMA are solvent N, N- diformazan
Yl acetamide;In DMA and water mixed solvent, raw material is mixed into 0.5~1.5h, at 110~130 DEG C in closed container
Lower reaction 2~4 days;After natural cooling, faint yellow bulk crystals are filtrated to get, wash this crystal, it is target production to spontaneously dry
Thing.
4. method as claimed in claim 3, it is characterised in that:Described closed container is reactor.
5. method as claimed in claim 3, it is characterised in that:The described reaction time is 3 days.
6. method as claimed in claim 3, it is characterised in that:Described reaction temperature is 120 DEG C.
7. method as claimed in claim 3, it is characterised in that:Described faint yellow bulk crystals use DMA, water washing successively,
Spontaneously dry.
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