CN116040673B - Synthetic method of samarium diiodide - Google Patents
Synthetic method of samarium diiodide Download PDFInfo
- Publication number
- CN116040673B CN116040673B CN202310336266.2A CN202310336266A CN116040673B CN 116040673 B CN116040673 B CN 116040673B CN 202310336266 A CN202310336266 A CN 202310336266A CN 116040673 B CN116040673 B CN 116040673B
- Authority
- CN
- China
- Prior art keywords
- iodine
- reactor
- samarium
- sublimation
- pipeline
- 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.)
- Active
Links
- UAWABSHMGXMCRK-UHFFFAOYSA-L samarium(ii) iodide Chemical compound I[Sm]I UAWABSHMGXMCRK-UHFFFAOYSA-L 0.000 title claims abstract description 45
- 238000010189 synthetic method Methods 0.000 title claims abstract description 6
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims abstract description 66
- 229910052740 iodine Inorganic materials 0.000 claims abstract description 65
- 239000011630 iodine Substances 0.000 claims abstract description 65
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 22
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 11
- 238000001308 synthesis method Methods 0.000 claims abstract description 4
- 238000000859 sublimation Methods 0.000 claims description 33
- 230000008022 sublimation Effects 0.000 claims description 33
- 238000011084 recovery Methods 0.000 claims description 24
- 239000011261 inert gas Substances 0.000 claims description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000010453 quartz Substances 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000012159 carrier gas Substances 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 230000008569 process Effects 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 3
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 18
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 6
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 230000002194 synthesizing effect Effects 0.000 description 3
- 229910052772 Samarium Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- XQKBFQXWZCFNFF-UHFFFAOYSA-K triiodosamarium Chemical compound I[Sm](I)I XQKBFQXWZCFNFF-UHFFFAOYSA-K 0.000 description 2
- GBBZLMLLFVFKJM-UHFFFAOYSA-N 1,2-diiodoethane Chemical compound ICCI GBBZLMLLFVFKJM-UHFFFAOYSA-N 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- YZCKVEUIGOORGS-NJFSPNSNSA-N Tritium Chemical compound [3H] YZCKVEUIGOORGS-NJFSPNSNSA-N 0.000 description 1
- 150000001299 aldehydes Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000001906 cholesterol absorption Effects 0.000 description 1
- 238000003926 complexometric titration Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- -1 dicyclopentadienyl samarium (II) Chemical compound 0.000 description 1
- 150000002148 esters Chemical group 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 150000002576 ketones Chemical group 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- NRVRMANRRKBYEK-UHFFFAOYSA-N methane;dihydroiodide Chemical compound C.I.I NRVRMANRRKBYEK-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920001610 polycaprolactone Polymers 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000007151 ring opening polymerisation reaction Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- ORZHVTYKPFFVMG-UHFFFAOYSA-N xylenol orange Chemical compound OC(=O)CN(CC(O)=O)CC1=C(O)C(C)=CC(C2(C3=CC=CC=C3S(=O)(=O)O2)C=2C=C(CN(CC(O)=O)CC(O)=O)C(O)=C(C)C=2)=C1 ORZHVTYKPFFVMG-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/253—Halides
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a synthetic method of samarium diiodide, and belongs to the technical field of organic synthesis. The samarium powder and the iodine simple substance are used as raw materials, the pure samarium diiodide is directly synthesized by a solvent-free method, and the pure samarium diiodide can be prepared in high yield by optimizing the process conditions such as the reaction temperature, and the yield can reach more than 80 percent; the synthesis method disclosed by the invention is simple in process, easy to realize industrialization and beneficial to reducing the cost; the prepared samarium diiodide can be conveniently prepared into different concentrations in different solvents, so that various use requirements are met.
Description
Technical Field
The invention belongs to the technical field of organic synthesis, and particularly relates to a method for synthesizing samarium diiodide.
Background
In 1906, matignon and Cazes heated SmI at high temperature in hydrogen 3 Preparation of SmI 2 . However, for a long time thereafter, the preparation method is limited to high temperature technology and solid phase chemical method; until 1977, kagan et al improved the preparation process and used samarium powder and 1, 2-diiodoethane in tetrahydrofuran to obtain SmI 2 So that it is widely used.
Samarium diiodide is a very widely applied reducing reagent, and the reducing capability of the samarium diiodide can be regulated and controlled by adding different auxiliary reagents, so that functional groups such as aldehyde, ketone, ester, double bond and the like can be selectively reduced. In 1980, kagan first established SmI 2 Applied to organic synthesis reaction due to SmI 2 The ether solubility is excellent, the reduction potential and the oxygen affinity are high, the chemical selectivity and diastereoselectivity of the reaction can be promoted, and the ether solubility is rapidly changed into widely used single electron transfer reducing agent and coupling agent. Krief called samarium diiodide as Kagan reagent.
Journal literature ("The reaction of samarium (III) iodide with samarium metal in tetrahydrofuran, a new method for the preparation of samarium (II) iodide", T Imamoto, M Ono, "Chemistry Letters", 1987) used samarium triiodide and samarium metal reacted in tetrahydrofuran to give samarium diiodide solutions.
Journal literature ("research of ring-opening polymerization mechanism of poly epsilon-caprolactone by alpha, alpha' -o-xylyl bridged dicyclopentadienyl samarium (II) complex",kang Yong, rubber and plastic technology and equipment (plastics), volume 45, discloses a preparation method of samarium diiodide solution: cutting 14g Sm into strips of N 2 Into a reaction flask with a stirrer under protection, THF was added, and then 12.9g of I was introduced into a glass tube after treatment 2 After weighing, at N 2 Adding the mixture into a reaction bottle under the protection, stirring at room temperature for reaction 24 h to obtain blue-green SmI 2 THF. Transferring the above solution into a centrifuge bottle, centrifuging at 2200 r/min for 10 min, transferring supernatant into a reaction bottle to obtain 0.1260 mol/L SmI 2 395mL, 97.9% yield.
Journal literature ("modification of the process for preparing samarium diiodide reagents", ruan Mingde, chemical reagents, volume 16, stage 5) uses a slight excess of samarium powder to react with diiodide methane in tetrahydrofuran to prepare samarium diiodide reagents.
Studies ("design and Synthesis of novel cholesterol absorption inhibitors", he Xinglian) disclose samarium diiodide (Smi) 2 ) The preparation method comprises the following specific processes: a condensing tube is arranged on a dry 1000mL three-neck flask, nitrogen is used for removing air in the reaction flask, iodine (5 g,40 mmol) is added, 600mL of newly distilled tetrahydrofuran which is refluxed by sodium is added, samarium powder (3 g,20 mmol) is added after the elemental iodine is dissolved, nitrogen is used for protecting, and heating reflux reaction is carried out.
It can be seen that the prior art synthesizes SmI 2 The route of (2) is as follows:
in the prior art, samarium diiodide products of 0.1M/L tetrahydrofuran solution are mainly obtained by the reaction of samarium powder and iodine or diiodine in tetrahydrofuran, the concentration of the products is very low, and the large-scale production of the pure samarium diiodide products is not easy.
Therefore, it is necessary to provide a method for synthesizing samarium diiodide, which uses samarium powder and iodine simple substance as raw materials, and directly synthesizes the pure samarium diiodide by a solvent-free method, so that the cost is lower and the industrialization is easier to realize.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides a method for synthesizing samarium diiodide, which takes samarium powder and iodine simple substance as raw materials, directly synthesizes the pure samarium diiodide by a solvent-free method, and can prepare the pure samarium diiodide with high yield by optimizing the process conditions such as reaction temperature and the like, wherein the yield can reach more than 90 percent; the synthesis method disclosed by the invention is simple in process, easy to realize industrialization and beneficial to reducing the cost; the prepared samarium diiodide can be conveniently prepared into different concentrations in different solvents, so that various use requirements are met.
In order to achieve the above purpose, the invention provides a synthetic method of samarium diiodide, comprising the following steps:
transferring samarium powder into a reactor, setting the reaction temperature to be 200-500 ℃, taking iodine into a sublimation device, introducing sublimated iodine steam into the reactor, and reacting with the samarium powder to generate samarium diiodide.
In a preferred embodiment, the reaction temperature is 300 to 500 ℃.
In a preferred embodiment, the reactor is a quartz tube reactor.
In a preferred embodiment, the temperature of the iodine sublimation apparatus is controlled between 45-70 ℃, more preferably between 50-60 ℃.
In a preferred embodiment, the molar ratio of samarium powder to elemental iodine is 1 (1-2).
In a preferred embodiment, the reaction apparatus employed comprises: the device comprises a reactor, a sublimation device and an iodine vapor recovery device, wherein the reactor is connected with the sublimation device through a first pipeline, the sublimation device is heated through a pipeline, the reactor is connected with the iodine vapor recovery device through a second pipeline, a heating device is arranged in the reactor, a carrier gas inlet is formed in the upper portion of the sublimation device, an air outlet is formed in the iodine vapor recovery device, and a condensing device is arranged on the iodine vapor recovery device.
In a preferred embodiment, the heating device is started to heat samarium powder in the reactor, elemental iodine at the bottom of the sublimation device is heated by adopting a pipeline, the elemental iodine sublimates to generate iodine steam, the iodine steam enters the reactor through a first pipeline to react with the samarium powder in the reactor under the heating condition, and excessive iodine steam enters an iodine steam recovery device with a condensing device through a second pipeline to be condensed into iodine solid for recovery.
In a preferred embodiment, inert gas is introduced through the carrier gas inlet before the reaction starts, and the inert gas is discharged from the gas outlet after flowing through the sublimation device, the reactor and the iodine vapor recovery device.
In a preferred embodiment, the inert gas is selected from argon, helium, nitrogen.
In a preferred embodiment, the inert gas flow is 20-100mL/min, preferably 30-60mL/min.
Compared with the prior art, the invention has the beneficial effects that:
1. the method takes samarium powder and iodine simple substance as raw materials, directly synthesizes the pure samarium diiodide by a solvent-free method, and can prepare the pure samarium diiodide with high yield by optimizing the process conditions such as reaction temperature and the like, wherein the yield can reach more than 80 percent.
2. The synthesis method disclosed by the invention is simple in process, easy to realize industrialization and beneficial to reducing the cost; the prepared samarium diiodide can be conveniently prepared into different concentrations in different solvents, so that various use requirements are met.
Drawings
FIG. 1 shows a samarium diiodide reaction apparatus.
In the figure, 1, a reactor, 2, samarium powder, 3, a second pipeline, 4, a first pipeline, 5, a sublimation device, 6, a carrier gas inlet, 7, elemental iodine, 8, an iodine vapor recovery device, 9 and an air outlet.
Detailed Description
It is to be noted that the raw materials used in the present invention are all common commercial products, and the sources thereof are not particularly limited.
A reaction device adopted by the synthetic method of the samarium diiodide is shown in figure 1, and comprises: reactor 1, sublimation device 5, iodine vapor recovery unit 8, reactor 1 is connected with sublimation device 5 through first pipeline 4, sublimation device 5 adopts the pipeline area to heat, reactor 1 is connected with iodine vapor recovery unit 8 through second pipeline 3, be provided with heating device in the reactor 1, sublimation device 5 top is equipped with carrier gas inlet 6, iodine vapor recovery unit 8 is equipped with gas outlet 9, is equipped with condensing equipment on the iodine vapor recovery unit 8.
In the samarium diiodide synthesis process, a heating device is started to heat samarium powder 2 in a reactor 1, elemental iodine 7 at the bottom of a heating sublimation device 5 is arranged on a pipeline, the elemental iodine 7 sublimates to generate iodine steam, the iodine steam enters the reactor 1 through a first pipeline 4 and reacts with samarium powder 2 in the reactor 1 under the heating condition, and excessive iodine steam enters an iodine steam recovery device 8 with a condensing device through a second pipeline 3 and is condensed into iodine solids for recovery.
Before the reaction starts, inert gas is introduced through the carrier gas inlet 6, and the inert gas flows through the sublimation device, the reactor and the iodine vapor recovery device and is discharged from the gas outlet 9. The inert gas is selected from argon, helium and nitrogen. The inert gas is introduced to provide an inert environment and promote iodine vapor to enter the reactor 1 and the iodine vapor recovery device 8 from the sublimation device 5 along with the inert gas to participate in the reaction and recovery.
Next, the technical scheme of the present invention will be described with reference to examples. Before samarium diiodide synthesis reaction is carried out in all the examples, nitrogen is introduced, and the flow rate of inert gas is 30-60mL/min until the reaction is finished. The samarium diiodide content was determined by EDTA complexometric titration using xylenol orange indicator.
Example 1
Transferring 50g of samarium powder into a quartz tube reactor, reacting at 200 ℃, transferring 85g of iodine into a sublimation device, keeping the temperature of the sublimation device to be raised to 50 ℃, enabling the flow rate of inert gas to be 30mL/min, introducing sublimated iodine steam into the quartz tube reactor, and reacting with samarium powder to generate 5g of samarium diiodide (4% yield).
Example 2
50g of samarium powder is transferred into a quartz tube reactor, the reaction temperature is 300 ℃, 101.5g of iodine (1.2 eq) is taken in a sublimation device, the temperature of the sublimation device is kept to be raised to 50 ℃, the flow rate of inert gas is 30mL/min, sublimated iodine steam is introduced into a samarium powder glass reactor, and 75g of samarium diiodide is generated by reaction with samarium powder (56% yield).
Example 3
50g of samarium powder is transferred into a quartz tube reactor, the reaction temperature is 350 ℃, 101.5g of iodine (1.2 eq) is taken in a sublimation device, the temperature of the sublimation device is kept to be raised to 50 ℃, the flow rate of inert gas is 30mL/min, sublimated iodine steam is introduced into the quartz tube reactor, and the sublimated iodine steam reacts with samarium powder to generate 115g of samarium diiodide (85 percent yield).
Example 4
Transferring 50g of samarium powder into a quartz tube reactor, reacting at 400 ℃, transferring 85g of iodine into a sublimation device, keeping the temperature of the sublimation device to be raised to 55 ℃, enabling the flow rate of inert gas to be 40mL/min, introducing sublimated iodine steam into the quartz tube reactor, and reacting with samarium powder to generate 113g of samarium diiodide (84% yield).
According to the examples 1-4, samarium powder and elemental iodine are adopted as raw materials, samarium diiodide can be prepared under the solvent-free condition, and along with the increase of the reaction temperature (200 ℃. Fwdarw.400 ℃), the yield of the samarium diiodide is obviously improved, especially the temperature reaches more than 350 ℃, and the yield is more than 80%.
Finally, it should be noted that the above description is only for illustrating the technical solution of the present invention, and not for limiting the scope of the present invention, and that the simple modification and equivalent substitution of the technical solution of the present invention can be made by those skilled in the art without departing from the spirit and scope of the technical solution of the present invention.
Claims (7)
1. The synthetic method of the samarium diiodide is characterized by comprising the following steps of:
transferring samarium powder into a reactor, setting the reaction temperature to be 350-500 ℃, taking iodine into a sublimation device, introducing sublimated iodine steam into the reactor, and reacting with the samarium powder to generate samarium diiodide;
the reaction device used comprises: the device comprises a reactor (1), a sublimation device (5) and an iodine vapor recovery device (8), wherein the reactor (1) is connected with the sublimation device (5) through a first pipeline (4), the sublimation device (5) is heated by adopting a pipeline, the reactor (1) is connected with the iodine vapor recovery device (8) through a second pipeline (3), a heating device is arranged in the reactor (1), a carrier gas inlet (6) is arranged above the sublimation device (5), an air outlet (9) is arranged on the iodine vapor recovery device (8), and a condensing device is arranged on the iodine vapor recovery device (8);
before the samarium diiodide synthesis reaction is carried out, inert gas is introduced until the reaction is finished; inert gas is introduced through the carrier gas inlet (6), and is discharged from the gas outlet (9) after flowing through the sublimation device, the reactor and the iodine vapor recovery device; the flow rate of the inert gas is 20-100mL/min; the mole ratio of samarium powder to elemental iodine is 1 (1-2).
2. The synthesis according to claim 1, wherein the reactor is a quartz tube reactor.
3. The method of synthesis according to claim 1, wherein the temperature of the iodine sublimation device is controlled between 45 ℃ and 70 ℃.
4. A method of synthesis according to claim 3, wherein the temperature of the iodine sublimation apparatus is controlled between 50 ℃ and 60 ℃.
5. The synthesis method according to claim 1, wherein the samarium powder (2) in the reactor (1) is heated by starting a heating device, elemental iodine (7) at the bottom of the heating sublimation device (5) is heated by adopting a pipeline, the elemental iodine (7) sublimates to generate iodine steam, the iodine steam enters the reactor (1) through a first pipeline (4) and reacts with the samarium powder (2) in the reactor (1) under the heating condition, and excessive iodine steam enters an iodine steam recovery device (8) with a condensing device through a second pipeline (3) and is condensed into iodine solid for recovery.
6. The method of synthesis according to claim 1, wherein the inert gas is selected from the group consisting of argon, helium, and nitrogen.
7. The method of claim 1, wherein the inert gas flow is 30-60mL/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310336266.2A CN116040673B (en) | 2023-03-31 | 2023-03-31 | Synthetic method of samarium diiodide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310336266.2A CN116040673B (en) | 2023-03-31 | 2023-03-31 | Synthetic method of samarium diiodide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116040673A CN116040673A (en) | 2023-05-02 |
| CN116040673B true CN116040673B (en) | 2023-06-09 |
Family
ID=86131755
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310336266.2A Active CN116040673B (en) | 2023-03-31 | 2023-03-31 | Synthetic method of samarium diiodide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116040673B (en) |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3305184B2 (en) * | 1996-02-09 | 2002-07-22 | 信越化学工業株式会社 | Method for producing anhydrous samarium diiodide |
| CN2253341Y (en) * | 1996-07-12 | 1997-04-30 | 中国原子能科学研究院 | Anhydrous thorium iodide synthetic device |
| CN104451317A (en) * | 2013-09-22 | 2015-03-25 | 北京有色金属研究总院 | Hafnium-base mixed metal material and iodination preparation method thereof |
| CN108101096A (en) * | 2016-11-25 | 2018-06-01 | 山东高洁环保科技有限公司 | Solvent removes water the preparation of samarium triiodide |
| CN208583345U (en) * | 2018-08-16 | 2019-03-08 | 泰安汉威集团有限公司 | A kind of high-purity potassium iodide production charging device |
-
2023
- 2023-03-31 CN CN202310336266.2A patent/CN116040673B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN116040673A (en) | 2023-05-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108997504B (en) | Preparation method of ionic liquid functionalized cellulose carbamate material | |
| CN114957193B (en) | Method for green synthesis of vinylene carbonate | |
| CN113698325A (en) | Method for preparing alkyl sulfonyl fluoride | |
| CN116040673B (en) | Synthetic method of samarium diiodide | |
| CN116096699A (en) | Formate production method, formic acid production method, formate production catalyst, and ruthenium complex | |
| CN111440207B (en) | Cuprous complex, preparation method thereof and application thereof in synthesis of 3-indolyl thioether | |
| CN111362974A (en) | Preparation method of fubitavir impurity | |
| CN111747923B (en) | Crown ether carboxylic acid compound-containing BPDC-12-C-4 and preparation method and application thereof | |
| CN113214306B (en) | Preparation method of double-amino-silicon ether compound and double-amino-silicon ether compound | |
| CN115350724A (en) | Preparation method of bifunctional polyion liquid catalyst for synthesizing oxazolidinone | |
| CN112299952B (en) | Method for producing 3-chloro-1, 2-propanediol by using acetic anhydride modified graphene oxide | |
| CN114591148A (en) | Method for synthesizing bisphenol fluorene based on microreactor | |
| CN112552318B (en) | Preparation method of perylene diimide derivative | |
| CN112625160B (en) | End group functionalized polymer and method for carrying out Glaser coupling polymerization reaction by utilizing copper acetylide | |
| JPS59190210A (en) | Dismutation of silane | |
| CN111790452B (en) | Methanol carbonylation catalyst, preparation method and application thereof | |
| CN109761947B (en) | Synthesis method of functionalized benzo chromene compound | |
| CN113214256A (en) | Synthesis method of 1, 7-diazaspiro [3.5] nonane-7-tert-butyl formate | |
| CN112079765A (en) | Synthesis method of 1- [60] fullerene pyrrolidine derivative | |
| CN115745761B (en) | Preparation method of high-quality 9-fluorenone | |
| CN114031773B (en) | Hyperbranched polyimidazoline compound and preparation method and application thereof | |
| CN111499548B (en) | Method for efficiently introducing acetoxyl group into beta position of fatty amine and fatty alcohol | |
| CN113105492B (en) | Preparation method of trifluoromethyl trimethylsilane | |
| CN114773377B (en) | Synthesis method of gamma- (2, 3-glycidoxy) propyl trimethoxy silane | |
| CN102516547B (en) | Benzocyclobutene silicone oil resin and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: Building 8, Yard 1, Zhongguancun East Road, Haidian District, Beijing, 100081, CG05-223 Patentee after: Yanfeng Technology (Beijing) Co.,Ltd. Address before: 18E, Unit 4, Building C, Yingdu Building, No. A48 Zhichun Road, Haidian District, Beijing, 100086 Patentee before: Yanfeng Technology (Beijing) Co.,Ltd. |