CN103449525A - Preparation method of molybdenum hexafluoride - Google Patents
Preparation method of molybdenum hexafluoride Download PDFInfo
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- CN103449525A CN103449525A CN2013103854076A CN201310385407A CN103449525A CN 103449525 A CN103449525 A CN 103449525A CN 2013103854076 A CN2013103854076 A CN 2013103854076A CN 201310385407 A CN201310385407 A CN 201310385407A CN 103449525 A CN103449525 A CN 103449525A
- Authority
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- China
- Prior art keywords
- molybdenum
- molybdenum hexafluoride
- reactor
- fluorine gas
- hexafluoride
- Prior art date
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Links
- WSWMGHRLUYADNA-UHFFFAOYSA-N 7-nitro-1,2,3,4-tetrahydroquinoline Chemical compound C1CCNC2=CC([N+](=O)[O-])=CC=C21 WSWMGHRLUYADNA-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims description 13
- 239000007789 gas Substances 0.000 claims abstract description 42
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 36
- 239000011737 fluorine Substances 0.000 claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 20
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 17
- 239000011733 molybdenum Substances 0.000 claims abstract description 17
- 239000012535 impurity Substances 0.000 claims abstract description 13
- 229910052751 metal Inorganic materials 0.000 claims abstract description 13
- 239000002184 metal Substances 0.000 claims abstract description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 10
- 239000001301 oxygen Substances 0.000 claims abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 10
- 238000000746 purification Methods 0.000 claims abstract description 10
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims abstract description 8
- 230000035484 reaction time Effects 0.000 claims abstract description 4
- 229910000831 Steel Inorganic materials 0.000 claims description 16
- 239000010959 steel Substances 0.000 claims description 16
- 238000010992 reflux Methods 0.000 claims description 9
- 238000009833 condensation Methods 0.000 claims description 6
- 230000005494 condensation Effects 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000001179 sorption measurement Methods 0.000 claims description 4
- 229910000792 Monel Inorganic materials 0.000 claims description 3
- 238000007710 freezing Methods 0.000 claims description 3
- 230000008014 freezing Effects 0.000 claims description 3
- 238000002309 gasification Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 235000013024 sodium fluoride Nutrition 0.000 claims description 2
- 239000011775 sodium fluoride Substances 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 28
- 238000000034 method Methods 0.000 abstract description 5
- 239000012043 crude product Substances 0.000 abstract 2
- 238000003786 synthesis reaction Methods 0.000 abstract 2
- 229910015275 MoF 6 Inorganic materials 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- FQFKTKUFHWNTBN-UHFFFAOYSA-N trifluoro-$l^{3}-bromane Chemical compound FBr(F)F FQFKTKUFHWNTBN-UHFFFAOYSA-N 0.000 description 3
- GICWIDZXWJGTCI-UHFFFAOYSA-I molybdenum pentachloride Chemical compound Cl[Mo](Cl)(Cl)(Cl)Cl GICWIDZXWJGTCI-UHFFFAOYSA-I 0.000 description 2
- YXTPWUNVHCYOSP-UHFFFAOYSA-N bis($l^{2}-silanylidene)molybdenum Chemical compound [Si]=[Mo]=[Si] YXTPWUNVHCYOSP-UHFFFAOYSA-N 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 229910021344 molybdenum silicide Inorganic materials 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a process method for preparing molybdenum hexafluoride, which comprises the following steps: (i) fluorine purification: the hydrogen fluoride gas in the fluorine is removed; (ii) synthesis reaction: the fluorine contacts with metal molybdenum in a reactor to generate a synthesis reaction, wherein the reaction temperature is 200-350 DEG C, the reaction time is 2-4 hours, the pressure is (-0.05)-0MPa, and a crude product of molybdenum hexafluoride is generated by the reaction; (iii) removing light impurities in the crude product of molybdenum hexafluoride such as oxygen and nitrogen; and (iv) purifying the molybdenum hexafluoride to obtain a product with purity over 99%. The method disclosed by the invention has the advantages that the reaction process is simple, the reaction conditions are easy to control, and the product purity is high.
Description
Technical field
The invention belongs to a kind of preparation method of fluorochemical, be specifically related to a kind of preparation method of molybdenum hexafluoride.
Background technology
Molybdenum hexafluoride (MoF
6) be mainly used in the separation of isotopes of molybdenum, can in microelectronics industry, be used as chemical vapor deposition molybdenum silicide or molybdenum film, to make low resistance, dystectic interconnection line.At present, the preparation method of molybdenum hexafluoride has following two kinds:
(i) molybdenum and bromine trifluoride reaction
Logical bromine trifluoride be heated to 350 ℃ and can make molybdenum hexafluoride on molybdenum, reaction equation is as follows:
Mo+2BrF
3→MoF
6+Br
2
, under air exists, molybdenum pentachloride and fluorine gas react (II)
Under air exists, to MoCl
5in logical fluorine gas also can generate molybdenum hexafluoride, reaction equation is as follows:
2MoCl
5+?6F
2→2MoF
6+?5Cl
2
In method (i), the starting material bromine trifluoride is the active liquid of chemical property, and inflammable, reaction conditions is wayward.In method (II), molybdenum pentachloride is the crystal with volatility that water absorbability is very strong, reacts more complicated.
In the preparation process of industrialized molybdenum hexafluoride, a series of problem such as reaction conditions is wayward, reaction process is complicated.
Summary of the invention
The present invention proposes for solving the shortcoming existed in prior art, its objective is a kind of preparation method who reacts simple, is easy to control, obtain the molybdenum hexafluoride that product purity is high is provided.
Technical scheme of the present invention is: a kind of processing method for preparing molybdenum hexafluoride comprises following step
Suddenly:
(i) fluorine gas purifies
Fluorine gas in the fluorine gas surge tank is passed in cooling tower, be cooled to-70～-90 ℃, first remove a large amount of hydrogen fluoride gas in fluorine gas, the fluorine gas that will contain a small amount of hydrogen fluoride gas passes in the absorption tower that Sodium Fluoride is housed again, remaining a small amount of hydrogen fluoride in 100 ℃ of conditions are gone down except fluorine gas;
(II) building-up reactions
Metal molybdenum is placed in to reactor, be preheating to 200 ℃, to reactor be evacuated to-0.1～-0.09MPa, slowly pass into the fluorine gas after purification, fluorine gas contacts in reactor with metal molybdenum building-up reactions occurs, and the temperature of reaction of reactor maintains 200～350 ℃, and the reaction times is 2～4 hours, maintain-0.05～0MPa of pressure, building-up reactions generates the thick product of molybdenum hexafluoride;
(III) removes the light impurity in the thick product of molybdenum hexafluoride
Contain the light impurities such as oxygen, nitrogen from reactor 4 the thick product of gaseous state molybdenum hexafluoride out, by freezing mode, the gaseous state molybdenum hexafluoride is condensed in collector 5, the temperature of collector 5 maintains-50～0 ℃, extract the light impurities such as uncooled oxygen, nitrogen in system, make it after exhaust gas processing device carbonating tower, adsorption tower are processed, emptying by the vacuum unit;
(IV) purification molybdenum hexafluoride
Then improve the distillation temperature to 40 ℃ of collector, the temperature to 35 of reflux column ℃, molybdenum hexafluoride starts gasification, open the valve on the product steel cylinder, receive the molybdenum hexafluoride product, in purification process, the temperature of molybdenum hexafluoride product steel cylinder is controlled at-50～0 ℃, when system pressure obviously descends, stops collecting, and obtains the sterling molybdenum hexafluoride.
The main body of described collector is the cylinder with condensation and heating unit, and upper end is the reflux column with the condensation chuck.
Described reactor, collector and fill steel cylinder and the material of connecting tube is stainless steel or Monel metal.
Reaction process of the present invention is simple, and reaction conditions is easy to control, and product purity is high.
The accompanying drawing explanation
Fig. 1 is the preparation method's of molybdenum hexafluoride of the present invention schema.
Wherein:
1 fluorine gas snubber 2 cooling towers
3 absorption tower 4 reactors
5 collector 6 product steel cylinders
7 carbonating tower 8 adsorption towers
9 vacuum units.
Embodiment
With embodiment, the preparation method of molybdenum hexafluoride of the present invention is elaborated with reference to the accompanying drawings:
As shown in Figure 1, a kind of preparation method of molybdenum hexafluoride comprises the following steps:
(i) fluorine gas purifies
By the fluorine gas (F in fluorine gas surge tank 1
2) pass in cooling tower 2, be cooled to-70～-90 ℃, first remove a large amount of hydrogen fluoride (HF) gas in fluorine gas, will contain a small amount of hydrofluoric fluorine gas and pass into again in the absorption tower 3 that Sodium Fluoride (NaF) is housed, remaining a small amount of hydrogen fluoride in 100 ℃ of conditions are gone down except fluorine gas
(II) building-up reactions
Metal molybdenum is placed in to reactor 4, be preheating to 200 ℃, to reactor 4 be evacuated to-0.1～-0.09MPa, slowly pass into the fluorine gas after purification, fluorine gas is with metal molybdenum in the interior generation building-up reactions that contacts of reactor 4, and the temperature of reaction of reactor 4 maintains 200～350 ℃, reaction times is 2～4 hours, maintain-0.05～0MPa of pressure, building-up reactions generates the thick product of molybdenum hexafluoride, and reaction formula is:
Mo＋3F
2→MoF
6
(III) removes the light impurity in the thick product of molybdenum hexafluoride
Contain the light impurities such as oxygen, nitrogen from reactor 4 the thick product of gaseous state molybdenum hexafluoride out, by freezing mode, the gaseous state molybdenum hexafluoride is condensed in collector 5, the temperature of collector 5 maintains-50～0 ℃, extract the light impurities such as uncooled oxygen, nitrogen in system, make it after exhaust gas processing device carbonating tower 7, adsorption tower 8 are processed, emptying by vacuum unit 9
(IV) purification molybdenum hexafluoride
Then improve the distillation temperature to 40 ℃ of collector 5, the temperature to 35 of reflux column ℃, molybdenum hexafluoride starts gasification, open the valve on product steel cylinder 6, receive the molybdenum hexafluoride product, in purification process, the temperature of molybdenum hexafluoride product steel cylinder 6 is controlled at-50～0 ℃, when system pressure obviously descends, stops collecting, and obtains the sterling molybdenum hexafluoride.
Wherein, the main body of collector 5 is the cylinder with condensation and heating unit, and upper end is the reflux column with the condensation chuck.The material of reactor 4, collector 5 and product steel cylinder 6 and connecting tube thereof is stainless steel or Monel metal.
Embodiment 1
The 50g metal molybdenum is placed in reactor 4, to reactor sealing leak hunting qualified after, it is preheating to 200 ℃, stop heating, to be evacuated to-0.1Mpa of reactor 4.To the interior fluorine gas slowly passed into after purifying of reactor 4, metal molybdenum and fluorine gas building-up reactions generate molybdenum hexafluoride, and reactor 4 temperature are controlled at 200 ℃, maintain-0.05MPa of pressure, and after 2 hours, reaction finishes.
The thick product introduction collector 5 of molybdenum hexafluoride out from reactor 4, collector 5 temperature are-50 ℃, the light constituent impurity such as the oxygen in molybdenum hexafluoride, nitrogen enter exhaust treatment system, the distillation temperature of collector 5 rises to 40 ℃, the temperature to 35 ℃ of reflux column, the temperature of product steel cylinder 6 maintains 0 ℃, product-collecting, in steel cylinder, obtains 90g molybdenum hexafluoride product, and its purity is more than 99%.
The 100g metal molybdenum is placed in reactor 4, to reactor 4 sealing leak hunting qualified after, it is preheating to 200 ℃, stop heating, to be evacuated to-0.05Mpa of reactor 4.To the interior fluorine gas slowly passed into after purifying of reactor 4, metal molybdenum and fluorine gas building-up reactions generate molybdenum hexafluoride, and reactor 4 temperature are controlled at 280 ℃, maintain-0.08MPa of pressure, and after 3 hours, reaction finishes.
The thick product introduction collector 5 of molybdenum hexafluoride out from reactor 4, collector 5 temperature are-25 ℃, the light constituent impurity such as the oxygen in molybdenum hexafluoride, nitrogen enter exhaust treatment system, the distillation temperature of collector 5 rises to 40 ℃, the temperature to 35 of reflux column ℃, the temperature of product steel cylinder 6 maintains-25 ℃, and product-collecting is in steel cylinder, obtain 190g molybdenum hexafluoride product, its purity is more than 99%.
The 200g metal molybdenum is placed in reactor 4, to reactor 4 sealing leak hunting qualified after, it is preheating to 200 ℃, stop heating, to be evacuated to-0.09Mpa of reactor 4.To reactor 4 is interior, slowly pass into through the fluorine gas after purifying, metal molybdenum and fluorine gas building-up reactions generate molybdenum hexafluoride, and reactor 4 temperature are controlled at 350 ℃, pressure and maintain 0MPa, and after 4 hours, reaction finishes.
The thick product introduction collector 5 of molybdenum hexafluoride out from reactor 4, the temperature of collector 5 is 0 ℃, the light constituent impurity such as the oxygen in molybdenum hexafluoride, nitrogen enter exhaust treatment system, the distillation temperature of collector 5 rises to 40 ℃, the temperature to 35 ℃ of reflux column, the temperature of product steel cylinder 6 maintains-50 ℃, product-collecting, in steel cylinder, obtains 410g molybdenum hexafluoride product, and its purity is more than 99%.
Reaction process of the present invention is simple, and reaction conditions is easy to control, and product purity is high.
Claims (3)
1. the preparation method of a molybdenum hexafluoride is characterized in that comprising the following steps:
(i) fluorine gas purifies
Fluorine gas in fluorine gas surge tank (1) is passed in cooling tower (2), be cooled to-70～-90 ℃, first remove a large amount of hydrogen fluoride gas in fluorine gas, the fluorine gas that will contain a small amount of hydrogen fluoride gas passes in the absorption tower (3) that Sodium Fluoride is housed again, a small amount of hydrogen fluoride in 100 ℃ of conditions are gone down except fluorine gas;
(II) building-up reactions
Metal molybdenum is placed in to reactor (4), be preheating to 200 ℃, to reactor (4) be evacuated to-0.1～-0.09MPa, slowly pass into the fluorine gas after purification, fluorine gas contacts in reactor (4) with metal molybdenum building-up reactions occurs, and the temperature of reaction of reactor (4) maintains 200～350 ℃, and the reaction times is 2～4 hours, maintain-0.05～0MPa of pressure, building-up reactions generates the thick product of molybdenum hexafluoride;
(III) removes the light impurity in the thick product of molybdenum hexafluoride
Contain the light impurities such as oxygen, nitrogen from reactor (4) the thick product of gaseous state molybdenum hexafluoride out, by freezing mode, the gaseous state molybdenum hexafluoride is condensed in collector (5), the temperature of collector (5) maintains-50～0 ℃, extract the light impurities such as uncooled oxygen, nitrogen in system, make it after exhaust gas processing device carbonating tower (7), adsorption tower (8) are processed, emptying by vacuum unit (9);
(IV) purification molybdenum hexafluoride
Then improve the distillation temperature to 40 ℃ of collector (5), the temperature to 35 of reflux column ℃, molybdenum hexafluoride starts gasification, open the valve on product steel cylinder (6), receive the molybdenum hexafluoride product, in purification process, the temperature of molybdenum hexafluoride product steel cylinder (6) is controlled at-50～0 ℃, when system pressure obviously descends, stops collecting, and obtains the sterling molybdenum hexafluoride.
2. the preparation method of molybdenum hexafluoride according to claim 1 is characterized in that: the main body of described collector (5) is the cylinder with condensation and heating unit, and upper end is the reflux column with the condensation chuck.
3. the preparation method of molybdenum hexafluoride according to claim 1 is characterized in that: described reactor (4), collector (5) and the material that fills steel cylinder (6) and connecting tube thereof are stainless steel or Monel metal.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104016412A (en) * | 2014-05-14 | 2014-09-03 | 黎明化工研究设计院有限责任公司 | Tungsten hexafluoride freezing trap and using method thereof |
| CN107290437A (en) * | 2016-03-31 | 2017-10-24 | 中核新能核工业工程有限责任公司 | The method for measuring content of fluorine indirectly using chromatograph |
| CN109179341A (en) * | 2018-11-29 | 2019-01-11 | 天津长芦华信化工股份有限公司 | The method for preparing tellurium hexafluoride |
| WO2019189715A1 (en) * | 2018-03-30 | 2019-10-03 | 関東電化工業株式会社 | Method and device for producing molybdenum hexafluoride |
| CN111785407A (en) * | 2020-07-13 | 2020-10-16 | 中国科学院上海应用物理研究所 | A kind of treatment method of molybdenum-containing substance |
| CN114318256A (en) * | 2021-12-28 | 2022-04-12 | 亚芯半导体材料(江苏)有限公司 | Large size molybdenum sputtering target and its preparation process by chemical vapor deposition |
| CN115974157A (en) * | 2023-02-28 | 2023-04-18 | 中船(邯郸)派瑞特种气体股份有限公司 | Preparation and purification method of molybdenum hexafluoride |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU416317A1 (en) * | 1972-03-22 | 1974-02-25 | ||
| CN201089722Y (en) * | 2007-07-20 | 2008-07-23 | 核工业理化工程研究院华核新技术开发公司 | Device for preparing sulfur hexafluoride |
| CN102951684A (en) * | 2012-11-26 | 2013-03-06 | 厦门钨业股份有限公司 | Preparation method for tungsten hexafluoride gas |
-
2013
- 2013-08-30 CN CN201310385407.6A patent/CN103449525B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU416317A1 (en) * | 1972-03-22 | 1974-02-25 | ||
| CN201089722Y (en) * | 2007-07-20 | 2008-07-23 | 核工业理化工程研究院华核新技术开发公司 | Device for preparing sulfur hexafluoride |
| CN102951684A (en) * | 2012-11-26 | 2013-03-06 | 厦门钨业股份有限公司 | Preparation method for tungsten hexafluoride gas |
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| CN104016412B (en) * | 2014-05-14 | 2016-01-20 | 黎明化工研究设计院有限责任公司 | A kind of tungsten hexafluoride freezing trap and using method thereof |
| CN104016412A (en) * | 2014-05-14 | 2014-09-03 | 黎明化工研究设计院有限责任公司 | Tungsten hexafluoride freezing trap and using method thereof |
| CN107290437A (en) * | 2016-03-31 | 2017-10-24 | 中核新能核工业工程有限责任公司 | The method for measuring content of fluorine indirectly using chromatograph |
| JP7186768B2 (en) | 2018-03-30 | 2022-12-09 | 関東電化工業株式会社 | Method and apparatus for producing molybdenum hexafluoride |
| WO2019189715A1 (en) * | 2018-03-30 | 2019-10-03 | 関東電化工業株式会社 | Method and device for producing molybdenum hexafluoride |
| US11878915B2 (en) | 2018-03-30 | 2024-01-23 | Kanto Denka Kogyo Co., Ltd. | Production method and production apparatus for molybdenum hexafluoride |
| CN111918839A (en) * | 2018-03-30 | 2020-11-10 | 关东电化工业株式会社 | Method and apparatus for producing molybdenum hexafluoride |
| KR20200136913A (en) * | 2018-03-30 | 2020-12-08 | 칸토 덴카 코교 가부시키가이샤 | Molybdenum hexafluoride manufacturing method and manufacturing apparatus |
| JPWO2019189715A1 (en) * | 2018-03-30 | 2021-04-22 | 関東電化工業株式会社 | Manufacturing method and equipment for molybdenum hexafluoride |
| KR102586310B1 (en) * | 2018-03-30 | 2023-10-06 | 칸토 덴카 코교 가부시키가이샤 | Manufacturing method and manufacturing device of molybdenum hexafluoride |
| CN111918839B (en) * | 2018-03-30 | 2022-09-13 | 关东电化工业株式会社 | Method and apparatus for producing molybdenum hexafluoride |
| CN109179341A (en) * | 2018-11-29 | 2019-01-11 | 天津长芦华信化工股份有限公司 | The method for preparing tellurium hexafluoride |
| CN111785407A (en) * | 2020-07-13 | 2020-10-16 | 中国科学院上海应用物理研究所 | A kind of treatment method of molybdenum-containing substance |
| CN114318256A (en) * | 2021-12-28 | 2022-04-12 | 亚芯半导体材料(江苏)有限公司 | Large size molybdenum sputtering target and its preparation process by chemical vapor deposition |
| CN115974157A (en) * | 2023-02-28 | 2023-04-18 | 中船(邯郸)派瑞特种气体股份有限公司 | Preparation and purification method of molybdenum hexafluoride |
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