CN104774219A - Trimethylaluminium preparation method - Google Patents
Trimethylaluminium preparation method Download PDFInfo
- Publication number
- CN104774219A CN104774219A CN201510206842.7A CN201510206842A CN104774219A CN 104774219 A CN104774219 A CN 104774219A CN 201510206842 A CN201510206842 A CN 201510206842A CN 104774219 A CN104774219 A CN 104774219A
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- China
- Prior art keywords
- aluminium
- ethers
- hours
- keep
- preparation
- 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.)
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- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 150000002170 ethers Chemical class 0.000 claims abstract description 50
- 150000001350 alkyl halides Chemical class 0.000 claims abstract description 29
- 229910000861 Mg alloy Inorganic materials 0.000 claims abstract description 26
- GANNOFFDYMSBSZ-UHFFFAOYSA-N [AlH3].[Mg] Chemical compound [AlH3].[Mg] GANNOFFDYMSBSZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 12
- XTAZYLNFDRKIHJ-UHFFFAOYSA-N n,n-dioctyloctan-1-amine Chemical compound CCCCCCCCN(CCCCCCCC)CCCCCCCC XTAZYLNFDRKIHJ-UHFFFAOYSA-N 0.000 claims abstract description 11
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 23
- 239000004411 aluminium Substances 0.000 claims description 23
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 23
- 238000010992 reflux Methods 0.000 claims description 13
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 12
- 238000013019 agitation Methods 0.000 claims description 10
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 5
- 229910052749 magnesium Inorganic materials 0.000 claims description 5
- 239000011777 magnesium Substances 0.000 claims description 5
- JWUJQDFVADABEY-UHFFFAOYSA-N 2-methyltetrahydrofuran Chemical compound CC1CCCO1 JWUJQDFVADABEY-UHFFFAOYSA-N 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 238000001704 evaporation Methods 0.000 abstract 4
- 230000001105 regulatory effect Effects 0.000 abstract 3
- 238000003756 stirring Methods 0.000 abstract 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- VOITXYVAKOUIBA-UHFFFAOYSA-N triethylaluminium Chemical compound CC[Al](CC)CC VOITXYVAKOUIBA-UHFFFAOYSA-N 0.000 description 4
- 238000004871 chemical beam epitaxy Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000002269 spontaneous effect Effects 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 229910018134 Al-Mg Inorganic materials 0.000 description 1
- 229910018467 Al—Mg Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010555 transalkylation reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- C07F5/06—Aluminium compounds
- C07F5/061—Aluminium compounds with C-aluminium linkage
- C07F5/062—Al linked exclusively to C
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A trimethylaluminium preparation method includes the steps of adding aluminium-magnesium alloy powder and ethers into a reactor under the protection of inert gas, dropwise adding alkyl halide under the stirring condition, keeping ether backflow in the dropwise alkyl halide adding process, continuing to keep the ether backflow for 4 hours to 5 hours after alkyl halide is dropwise added, regulating the temperature of the reactor to 45 DEG C to 100 DEG C, keeping the temperature for 1 hour to 4 hours, evaporating the ethers, regulating the temperature of the reactor to 45 DEG C to 70 DEG C, keeping the temperature, evaporating the coordination compound of trimethylaluminium and the ethers under the vacuum condition, moving the coordination compound of the trimethylaluminium and the ethers to a deolation kettle, adding tri-n-octylamine, conducting heating and backflow under the stirring condition, keeping for 2 hours to 3 hours, regulating the temperature of the deolation kettle to 85 DEG C to 89 DEG C again, keeping the temperature for 8 hours to 10 hours under the vacuum degree of 1 mmHg to 50 mmHg, evaporating the ethers, raising the temperature of the deolation kettle to 90 DEG C to 160 DEG C, keeping the temperature for 30 hours to 35 hours under the vacuum condition, and evaporating the trimethylaluminium.
Description
Technical field
The invention belongs to organometallic compound synthesis technical field, be specifically related to a kind of trimethyl aluminium preparation method.
Background technology
The organometallicss such as high-purity trimethyl aluminium, metal organic chemical vapor deposition technology (MOCVD), in chemical beam epitaxy (CBE) process grow light electronic material most important, be also the maximum raw material of current consumption, be widely used in compound semiconductor film material.Pure trimethyl aluminium is at room temperature liquid, when being encapsulated in steel cylinder for needing during MOCVD, then steel cylinder temperature is controlled, its vapour pressure is made to reach certain value, again by continuing the carrier gas of flowing, bring the trimethyl aluminium in solid vapor equilibrium state gas phase at service temperatures into MOCVD or CBE growing system.
The preparation method of trimethyl aluminium is more, but it is little to apply to industrialized method, and namely common method adopts industrial triethyl aluminum and haloalkane to carry out transalkylation reaction, but there is following shortcoming: 1) reaction transformation efficiency is not high, has a large amount of by product to produce; 2) material cost is high, and as preparation of industrialization route, triethyl aluminum price is higher, and production cost is high; 3) raw material is inflammable, there is potential safety hazard, and triethyl aluminum is very responsive to air, steam, meets air spontaneous combustion, meets water blast, and the processes such as filling during use, transfer, reaction exist potential safety hazard.
Summary of the invention
The object of this invention is to provide that a kind of technique is simple, reacting balance, be easy to the trimethyl aluminium preparation method of suitability for industrialized production.
For achieving the above object, the technical solution used in the present invention is, a kind of trimethyl aluminium preparation method, comprise the following steps: under protection of inert gas, in reactor, add aluminium-magnesium alloy powder and ethers, drip haloalkane under agitation, in haloalkane dropping process, keep ethers to reflux; After haloalkane is added dropwise to complete, continues to keep ethers backflow 4 ~ 5 hours, then reactor still temperature be adjusted to 45 ~ 100 DEG C and keep 1 ~ 4 hour, ethers is steamed; Again reactor still temperature adjusted to 45 ~ 70 DEG C and kept, under vacuum tightness 1 ~ 100mmHg, the title complex of trimethyl aluminium and ethers being steamed; The title complex of trimethyl aluminium and ethers is transferred to solution joins in still, then adds tri-n-octyl amine, under agitation reflux, keeps 2 ~ 3 hours; Adjust again solution join still still temperature be 85 ~ 89 DEG C and keep, under vacuum tightness 1 ~ 50mmHg keep 8 ~ 10 hours, steam ethers; Solution is joined still still temperature rise to 90 ~ 160 DEG C again, and keep 30 ~ 35 hours under vacuum tightness 1 ~ 30mmHg, steam trimethyl aluminium.
Preferably, in described aluminium-magnesium alloy powder, the mass content of aluminium is 30 ~ 42%, and surplus is magnesium.
Preferably, in described haloalkane and aluminium-magnesium alloy powder, the mol ratio of aluminium is 3.5 ~ 4.5:1.
Preferably, in tri-n-octyl amine and aluminium-magnesium alloy powder, the mol ratio of aluminium is 1 ~ 1.3:1.
Preferably, in described ethers and aluminium-magnesium alloy powder, the mol ratio of aluminium is 4 ~ 8:1.
Preferably, described ethers is any one of ether, tetrahydrofuran (THF) or 2-methyltetrahydrofuran.
Preferably, described haloalkane is CH
3br, CH
3i or CH
3any one in Cl.
The reaction preparing trimethyl aluminium of the present invention is as follows:
Al-Mg (alloy)+CH
3x → Al (CH
3)
3+ MgX
2(X is Br, I or Cl).
The beneficial effect that the present invention produces is that, compared with triethyl aluminum substitution method, material is cheap, owing to adopting reactor to join being separated of still with solution, unreacted alloy still in a kettle., continues reaction, overall yield is higher, and by product can be recycled, and does not almost have waste material; Security is better, and because the raw material adopted in reaction process does not have spontaneous combustible substance, reaction process safety, is particularly suitable for large-scale industrial production.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, but protection scope of the present invention is not limited thereto.
Embodiment 1
A kind of trimethyl aluminium preparation method, comprise the following steps: under nitrogen protection, add aluminium-magnesium alloy powder and ethers in reactor, in described ethers and aluminium-magnesium alloy powder, the mol ratio of aluminium is 6:1, drip haloalkane under agitation, in haloalkane dropping process, keep ethers to reflux; After haloalkane is added dropwise to complete, continues to keep ethers to reflux 4.5 hours, then reactor still temperature be adjusted to 80 DEG C and keep 2.5 hours, ethers is steamed; Again reactor still temperature adjusted to 65 DEG C and kept, under vacuum tightness 50mmHg, the title complex of trimethyl aluminium and ethers being steamed; The title complex of trimethyl aluminium and ethers is transferred to solution joins in still, then adds tri-n-octyl amine, and in tri-n-octyl amine and aluminium-magnesium alloy powder, the mol ratio of aluminium is 1.2:1, under agitation reflux, keeps 2.5 hours; Adjust again solution join still still temperature be 87 DEG C and keep, under vacuum tightness 25mmHg keep 9 hours, steam ethers; Solution is joined the temperature rise to 120 DEG C of still still again, and keep 32 hours under vacuum tightness 15mmHg, steam trimethyl aluminium.
In described aluminium-magnesium alloy powder, the mass content of aluminium is 30%, and surplus is magnesium.In described haloalkane and aluminium-magnesium alloy powder, the mol ratio of aluminium is 4:1.Described ethers is tetrahydrofuran (THF), and described haloalkane is CH
3cl.In the present embodiment, the yield of trimethyl aluminium is 90% (calculating by metallic aluminium).
Embodiment 2
A kind of trimethyl aluminium preparation method, comprise the following steps: under nitrogen protection, add aluminium-magnesium alloy powder and ethers in reactor, in described ethers and aluminium-magnesium alloy powder, the mol ratio of aluminium is 4:1, drip haloalkane under agitation, in haloalkane dropping process, keep ethers to reflux; After haloalkane is added dropwise to complete, continues to keep ethers to reflux 5 hours, then reactor still temperature be adjusted to 45 DEG C and keep 4 hours, ethers is steamed; Again reactor still temperature adjusted to 45 DEG C and kept, under vacuum tightness 1mmHg, the title complex of trimethyl aluminium and ethers being steamed; The title complex of trimethyl aluminium and ethers is transferred to solution joins in still, then adds tri-n-octyl amine, and in tri-n-octyl amine and aluminium-magnesium alloy powder, the mol ratio of aluminium is 1:1, under agitation reflux, keeps 2 hours; Adjust again solution join still still temperature be 85 DEG C and keep, under vacuum tightness 1mmHg keep 8 hours, steam ethers; Solution is joined the temperature rise to 90 DEG C of still still again, and keep 30 hours under vacuum tightness 1mmHg, steam trimethyl aluminium.
In described aluminium-magnesium alloy powder, the mass content of aluminium is 35%, and surplus is magnesium.In described haloalkane and aluminium-magnesium alloy powder, the mol ratio of aluminium is 3.5:1.Described ethers is ether, and described haloalkane is CH
3br.The yield of the trimethyl aluminium in the present embodiment is that 83%(calculates by metallic aluminium).
Embodiment 3
A kind of trimethyl aluminium preparation method, comprise the following steps: under nitrogen protection, add aluminium-magnesium alloy powder and ethers in reactor, in described ethers and aluminium-magnesium alloy powder, the mol ratio of aluminium is 8:1, drip haloalkane under agitation, in haloalkane dropping process, keep ethers to reflux; After haloalkane is added dropwise to complete, continues to keep ethers to reflux 4 hours, then reactor still temperature be adjusted to 100 DEG C and keep 1 hour, ethers is steamed; Again reactor still temperature adjusted to 70 DEG C and kept, under vacuum tightness 100mmHg, the title complex of trimethyl aluminium and ethers being steamed; The title complex of trimethyl aluminium and ethers is transferred to solution joins in still, then adds tri-n-octyl amine, and in tri-n-octyl amine and aluminium-magnesium alloy powder, the mol ratio of aluminium is 1.3:1, under agitation reflux, keeps 3 hours; Adjust again solution join still still temperature be 89 DEG C and keep, under vacuum tightness 50mmHg keep 10 hours, steam ethers; Solution is joined the temperature rise to 160 DEG C of still still again, and keep 35 hours under vacuum tightness 30mmHg, steam trimethyl aluminium.
In described aluminium-magnesium alloy powder, the mass content of aluminium is 42%, and surplus is magnesium.In described haloalkane and aluminium-magnesium alloy powder, the mol ratio of aluminium is 4.5:1.Described ethers is 2-methyltetrahydrofuran, and described haloalkane is CH
3i.The yield of the trimethyl aluminium in the present embodiment is that 83%(calculates by metallic aluminium).
Claims (7)
1. a trimethyl aluminium preparation method, is characterized in that, comprises the following steps: under protection of inert gas, adds aluminium-magnesium alloy powder and ethers, drip haloalkane under agitation in reactor, in haloalkane dropping process, keep ethers to reflux; After haloalkane is added dropwise to complete, continues to keep ethers backflow 4 ~ 5 hours, then reactor still temperature be adjusted to 45 ~ 100 DEG C and keep 1 ~ 4 hour, ethers is steamed; Again reactor still temperature adjusted to 45 ~ 70 DEG C and kept, under vacuum tightness 1 ~ 100mmHg, the title complex of trimethyl aluminium and ethers being steamed; The title complex of trimethyl aluminium and ethers is transferred to solution joins in still, then adds tri-n-octyl amine, under agitation reflux, keeps 2 ~ 3 hours; Adjust again solution join still still temperature be 85 ~ 89 DEG C and keep, under vacuum tightness 1 ~ 50mmHg keep 8 ~ 10 hours, steam ethers; Solution is joined still still temperature rise to 90 ~ 160 DEG C again, and keep 30 ~ 35 hours under vacuum tightness 1 ~ 30mmHg, steam trimethyl aluminium.
2. trimethyl aluminium preparation method as claimed in claim 1, it is characterized in that: in described aluminium-magnesium alloy powder, the mass content of aluminium is 30 ~ 42%, surplus is magnesium.
3. trimethyl aluminium preparation method as claimed in claim 1, is characterized in that: in described haloalkane and aluminium-magnesium alloy powder, the mol ratio of aluminium is 3.5 ~ 4.5:1.
4. trimethyl aluminium preparation method as claimed in claim 1, is characterized in that: in tri-n-octyl amine and aluminium-magnesium alloy powder, the mol ratio of aluminium is 1 ~ 1.3:1.
5. trimethyl aluminium preparation method as claimed in claim 1, is characterized in that: in described ethers and aluminium-magnesium alloy powder, the mol ratio of aluminium is 4 ~ 8:1.
6. trimethyl aluminium preparation method as claimed in claim 1, is characterized in that: described ethers is any one of ether, tetrahydrofuran (THF) or 2-methyltetrahydrofuran.
7. trimethyl aluminium preparation method as claimed in claim 1, is characterized in that: described haloalkane is CH
3br, CH
3i or CH
3any one in Cl.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510206842.7A CN104774219A (en) | 2015-04-28 | 2015-04-28 | Trimethylaluminium preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510206842.7A CN104774219A (en) | 2015-04-28 | 2015-04-28 | Trimethylaluminium preparation method |
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|---|---|
| CN104774219A true CN104774219A (en) | 2015-07-15 |
Family
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| CN201510206842.7A Pending CN104774219A (en) | 2015-04-28 | 2015-04-28 | Trimethylaluminium preparation method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105175440A (en) * | 2015-09-30 | 2015-12-23 | 江西佳因光电材料有限公司 | Preparation method of trimethylaluminium |
| CN106831844A (en) * | 2017-02-10 | 2017-06-13 | 安徽博泰电子材料有限公司 | A kind of preparation method of trimethyl aluminium |
| WO2018074231A1 (en) * | 2016-10-20 | 2018-04-26 | 東ソー・ファインケム株式会社 | Aluminum alloy-containing composition, production method therefor, and trialkyl aluminum production method |
| CN109879900A (en) * | 2018-12-18 | 2019-06-14 | 安徽亚格盛电子新材料有限公司 | A method of trimethyl aluminium is effectively purified using inorganic salts |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6305622B1 (en) * | 1997-07-18 | 2001-10-23 | Nippon Aluminum Alkyls, Ltd. | Process for producing trihydrocarbyl aluminums |
| JP2008024617A (en) * | 2006-07-19 | 2008-02-07 | Ube Ind Ltd | High-purity trialkylaluminum and method for producing the same |
-
2015
- 2015-04-28 CN CN201510206842.7A patent/CN104774219A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6305622B1 (en) * | 1997-07-18 | 2001-10-23 | Nippon Aluminum Alkyls, Ltd. | Process for producing trihydrocarbyl aluminums |
| JP2008024617A (en) * | 2006-07-19 | 2008-02-07 | Ube Ind Ltd | High-purity trialkylaluminum and method for producing the same |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105175440A (en) * | 2015-09-30 | 2015-12-23 | 江西佳因光电材料有限公司 | Preparation method of trimethylaluminium |
| WO2018074231A1 (en) * | 2016-10-20 | 2018-04-26 | 東ソー・ファインケム株式会社 | Aluminum alloy-containing composition, production method therefor, and trialkyl aluminum production method |
| CN109843895A (en) * | 2016-10-20 | 2019-06-04 | 东曹精细化工株式会社 | The preparation method of composition containing aluminium alloy and preparation method thereof and trialkylaluminium |
| US10870666B2 (en) | 2016-10-20 | 2020-12-22 | Tosoh Finechem Corporation | Aluminum alloy-containing composition, production method therefor, and trialkyl aluminum production method |
| KR20210123412A (en) * | 2016-10-20 | 2021-10-13 | 토소 화인켐 가부시키가이샤 | Aluminum alloy containing composition, production method therefor, and trialkyl aluminum production method |
| CN109843895B (en) * | 2016-10-20 | 2022-02-22 | 东曹精细化工株式会社 | Composition containing aluminum alloy, method for producing same, and method for producing trialkylaluminum |
| KR102418924B1 (en) * | 2016-10-20 | 2022-07-08 | 토소 화인켐 가부시키가이샤 | Aluminum alloy containing composition, production method therefor, and trialkyl aluminum production method |
| US11591349B2 (en) | 2016-10-20 | 2023-02-28 | Tosoh Finechem Corporation | Aluminum alloy-containing composition, production method therefor, and trialkyl aluminum production method |
| CN106831844A (en) * | 2017-02-10 | 2017-06-13 | 安徽博泰电子材料有限公司 | A kind of preparation method of trimethyl aluminium |
| CN106831844B (en) * | 2017-02-10 | 2019-07-02 | 安徽博泰电子材料有限公司 | A kind of preparation method of trimethyl aluminium |
| CN109879900A (en) * | 2018-12-18 | 2019-06-14 | 安徽亚格盛电子新材料有限公司 | A method of trimethyl aluminium is effectively purified using inorganic salts |
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