CN103449525B - Preparation method of molybdenum hexafluoride - Google Patents
Preparation method of molybdenum hexafluoride Download PDFInfo
- Publication number
- CN103449525B CN103449525B CN201310385407.6A CN201310385407A CN103449525B CN 103449525 B CN103449525 B CN 103449525B CN 201310385407 A CN201310385407 A CN 201310385407A CN 103449525 B CN103449525 B CN 103449525B
- Authority
- CN
- China
- Prior art keywords
- molybdenum
- molybdenum hexafluoride
- reactor
- hexafluoride
- fluorine gas
- 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
- 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 41
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000011737 fluorine Substances 0.000 claims abstract description 35
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 35
- 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
- 239000011733 molybdenum Substances 0.000 claims abstract description 17
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 17
- 238000000746 purification Methods 0.000 claims abstract description 15
- 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
- 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
- 238000000034 method Methods 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
- 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
- 238000011049 filling 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
Landscapes
- 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, chemical vapor deposition molybdenum silicide or molybdenum film can be used as in microelectronics industry, to make low resistance, dystectic interconnection line.At present, the preparation method of molybdenum hexafluoride has the following two kinds:
(i) molybdenum and bromine trifluoride reaction
Lead to bromine trifluoride and be heated to 350 DEG C on molybdenum and can obtain molybdenum hexafluoride, reaction equation is as follows:
Mo+2BrF
3→MoF
6+Br
2
(II) in the presence of the air, molybdenum pentachloride and fluorine gas react
In the presence of the air, to MoCl
5in logical fluorine gas also can generate molybdenum hexafluoride, reaction equation is as follows:
2MoCl
5+ 6F
2→2MoF
6+ 5Cl
2
Method (i) in, 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 problems such as reaction conditions is wayward, reaction process is complicated.
Summary of the invention
The present invention solves the shortcoming existed in prior art to propose, and its objective is that providing a kind of reacts preparation method that is simple, that be easy to control, obtain the high molybdenum hexafluoride of product purity.
Technical scheme of the present invention is: a kind of processing method preparing molybdenum hexafluoride, comprises following step
Rapid:
(i) fluorine gas purification
Fluorine gas in fluorine gas surge tank is passed in cooling tower, be cooled to-70 ~-90 DEG C, first remove a large amount of hydrogen fluoride gas in fluorine gas, the fluorine gas containing a small amount of hydrogen fluoride gas is passed into again and is equipped with in the absorption tower of Sodium Fluoride, under 100 DEG C of conditions, remove remaining a small amount of hydrogen fluoride in fluorine gas;
(II) building-up reactions
Metal molybdenum is placed in reactor, be preheating to 200 DEG C,-0.1 ~-0.09MPa is evacuated to reactor, slowly pass into the fluorine gas after purification, fluorine gas and metal molybdenum contact and building-up reactions occur in reactor, and the temperature of reaction of reactor maintains 200 ~ 350 DEG C, and the reaction times is 2 ~ 4 hours, pressure maintains-0.05 ~ 0MPa, and building-up reactions generates the thick product of molybdenum hexafluoride;
(III) removes the light impurity in the thick product of molybdenum hexafluoride
Containing the light impurity such as oxygen, nitrogen from the reactor 4 thick product of gaseous state molybdenum hexafluoride out, gaseous state molybdenum hexafluoride is made to condense in collector 5 by freezing mode, the temperature of collector 5 maintains-50 ~ 0 DEG C, extract the light impurity such as uncooled oxygen, nitrogen in system, make it after exhaust gas processing device carbonating tower, adsorption tower process, emptying by vacuum pump set;
(IV) purification molybdenum hexafluoride
Then the distillation temperature to 40 DEG C of collector is improved, the temperature to 35 DEG C of reflux column, molybdenum hexafluoride starts gasification, open the valve on product steel cylinder, receive molybdenum hexafluoride product, in purification process, the temperature of molybdenum hexafluoride product steel cylinder controls at-50 ~ 0 DEG C, stops collecting, obtain sterling molybdenum hexafluoride when system pressure obviously declines.
The main body of described collector is the cylinder with condensation and heating unit, and upper end is the reflux column with condensation chuck.
Described reactor, collector and the material filling steel cylinder and connecting tube thereof are 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.
Accompanying drawing explanation
Fig. 1 is the schema of the preparation method of molybdenum hexafluoride of the present invention.
Wherein:
1 fluorine gas snubber 2 cooling tower
3 absorption tower 4 reactors
5 collector 6 product steel cylinders
7 carbonating tower 8 adsorption towers
9 vacuum pump set.
Embodiment
Be described in detail with the preparation method of embodiment to molybdenum hexafluoride of the present invention 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 purification
By the fluorine gas (F in fluorine gas surge tank 1
2) pass in cooling tower 2, be cooled to-70 ~-90 DEG C, first remove a large amount of hydrogen fluoride (HF) gas in fluorine gas, will pass in the absorption tower 3 that Sodium Fluoride (NaF) is housed again containing a small amount of hydrofluoric fluorine gas, remaining a small amount of hydrogen fluoride in fluorine gas is removed under 100 DEG C of conditions
(II) building-up reactions
Metal molybdenum is placed in reactor 4, be preheating to 200 DEG C,-0.1 ~-0.09MPa is evacuated to reactor 4, slowly pass into the fluorine gas after purification, fluorine gas and metal molybdenum contact and building-up reactions occur in reactor 4, and the temperature of reaction of reactor 4 maintains 200 ~ 350 DEG C, reaction times is 2 ~ 4 hours, pressure maintains-0.05 ~ 0MPa, and 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
Containing the light impurity such as oxygen, nitrogen from the reactor 4 thick product of gaseous state molybdenum hexafluoride out, gaseous state molybdenum hexafluoride is made to condense in collector 5 by freezing mode, the temperature of collector 5 maintains-50 ~ 0 DEG C, extract the light impurity such as uncooled oxygen, nitrogen in system, make it after exhaust gas processing device carbonating tower 7, adsorption tower 8 process, emptying by vacuum pump set 9
(IV) purification molybdenum hexafluoride
Then the distillation temperature to 40 DEG C of collector 5 is improved, the temperature to 35 DEG C of reflux column, molybdenum hexafluoride starts gasification, open the valve on product steel cylinder 6, receive molybdenum hexafluoride product, in purification process, the temperature of molybdenum hexafluoride product steel cylinder 6 controls at-50 ~ 0 DEG C, stops collecting, obtain sterling molybdenum hexafluoride when system pressure obviously declines.
Wherein, the main body of collector 5 is the cylinder with condensation and heating unit, and upper end is the reflux column with 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
50g metal molybdenum is placed in reactor 4, to reactor sealing leak hunting qualified after, be preheating to 200 DEG C, stop heating ,-0.1Mpa is evacuated to reactor 4.In reactor 4, slowly pass into the fluorine gas after purification, metal molybdenum and fluorine gas building-up reactions generate molybdenum hexafluoride, reactor 4 temperature control 200 DEG C, pressure maintains-0.05MPa, after 2 hours, reaction terminates.
From the reactor 4 thick product introduction collector 5 of molybdenum hexafluoride out, collector 5 temperature is-50 DEG C, 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 DEG C, the temperature to 35 DEG C of reflux column, the temperature of product steel cylinder 6 maintains 0 DEG C, product-collecting is in steel cylinder, and obtain 90g molybdenum hexafluoride product, its purity can reach more than 99%.
Embodiment 2
100g metal molybdenum is placed in reactor 4, to reactor 4 sealing leak hunting qualified after, be preheating to 200 DEG C, stop heating ,-0.05Mpa is evacuated to reactor 4.In reactor 4, slowly pass into the fluorine gas after purification, metal molybdenum and fluorine gas building-up reactions generate molybdenum hexafluoride, reactor 4 temperature control 280 DEG C, pressure maintains-0.08MPa, after 3 hours, reaction terminates.
From the reactor 4 thick product introduction collector 5 of molybdenum hexafluoride out, collector 5 temperature is-25 DEG C, 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 DEG C, the temperature to 35 DEG C of reflux column, the temperature of product steel cylinder 6 maintains-25 DEG C, and product-collecting is in steel cylinder, obtain 190g molybdenum hexafluoride product, its purity can reach more than 99%.
Embodiment 3
200g metal molybdenum is placed in reactor 4, to reactor 4 sealing leak hunting qualified after, be preheating to 200 DEG C, stop heating ,-0.09Mpa is evacuated to reactor 4.In reactor 4, slowly pass into the fluorine gas after purification, metal molybdenum and fluorine gas building-up reactions generate molybdenum hexafluoride, reactor 4 temperature control 350 DEG C, pressure maintains 0MPa, after 4 hours, reaction terminates.
From the reactor 4 thick product introduction collector 5 of molybdenum hexafluoride out, the temperature of collector 5 is 0 DEG C, 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 DEG C, the temperature to 35 DEG C of reflux column, the temperature of product steel cylinder 6 maintains-50 DEG C, product-collecting is in steel cylinder, and obtain 410g molybdenum hexafluoride product, its purity can reach 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. a preparation method for 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 DEG C, first remove a large amount of hydrogen fluoride gas in fluorine gas, fluorine gas containing a small amount of hydrogen fluoride gas is passed in the absorption tower (3) that Sodium Fluoride is housed again, under 100 DEG C of conditions, remove remaining a small amount of hydrogen fluoride;
(II) building-up reactions
Metal molybdenum is placed in reactor (4), be preheating to 200 DEG C,-0.1 ~-0.09MPa is evacuated to reactor (4), slowly pass into the fluorine gas after purification, fluorine gas and metal molybdenum contact and building-up reactions occur in reactor (4), and the temperature of reaction of reactor (4) maintains 200 ~ 350 DEG C, and the reaction times is 2 ~ 4 hours, pressure maintains-0.05 ~ 0MPa, and building-up reactions generates the thick product of molybdenum hexafluoride;
(III) removes the light impurity in the thick product of molybdenum hexafluoride
Containing the light impurity such as oxygen, nitrogen from reactor (4) the thick product of gaseous state molybdenum hexafluoride out, gaseous state molybdenum hexafluoride is made to condense in collector (5) by freezing mode, the temperature of collector (5) maintains-50 ~ 0 DEG C, extract the light impurity such as uncooled oxygen, nitrogen in system, make it after exhaust gas processing device carbonating tower (7), adsorption tower (8) process, emptying by vacuum pump set (9);
(IV) purification molybdenum hexafluoride
Then the distillation temperature to 40 DEG C of collector (5) is improved, the temperature to 35 DEG C of reflux column, molybdenum hexafluoride starts gasification, open the valve on product steel cylinder (6), receive molybdenum hexafluoride product, in purification process, the temperature of molybdenum hexafluoride product steel cylinder (6) controls at-50 ~ 0 DEG C, stops collecting, obtain sterling molybdenum hexafluoride when system pressure obviously declines.
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 condensation chuck.
3. the preparation method of molybdenum hexafluoride according to claim 1, is characterized in that: the material of described reactor (4), collector (5) and product steel cylinder (6) and connecting tube thereof is stainless steel or Monel metal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310385407.6A CN103449525B (en) | 2013-08-30 | 2013-08-30 | Preparation method of molybdenum hexafluoride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310385407.6A CN103449525B (en) | 2013-08-30 | 2013-08-30 | Preparation method of molybdenum hexafluoride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103449525A CN103449525A (en) | 2013-12-18 |
| CN103449525B true CN103449525B (en) | 2015-05-13 |
Family
ID=49732428
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310385407.6A Active CN103449525B (en) | 2013-08-30 | 2013-08-30 | Preparation method of molybdenum hexafluoride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103449525B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| 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 |
| CN111785407B (en) * | 2020-07-13 | 2022-08-16 | 中国科学院上海应用物理研究所 | 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103449525A (en) | 2013-12-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103449525B (en) | Preparation method of molybdenum hexafluoride | |
| CN104477850B (en) | The preparation method of a kind of chlorine trifluoride and device | |
| CN104555927B (en) | A kind of purification process of chlorine trifluoride | |
| KR101605255B1 (en) | Method and apparatus for recovering iodine heptafluoride-derived iodine fluoride compound | |
| CN104477849B (en) | A kind of preparation method of chlorine trifluoride | |
| CN211871386U (en) | Device for pre-purifying nitrogen trifluoride crude product prepared by electrolysis | |
| CN104973629A (en) | Purification method of tungsten hexafluoride gas | |
| CN106517118A (en) | Preparation device and method of electronic grade red phosphorus | |
| CN213707743U (en) | A purification system based on molten salt recycling | |
| CN104192823A (en) | Vapor purification method of carbon nanotubes | |
| CN103497086A (en) | Preparation method of perfluoropropane | |
| KR102155727B1 (en) | Cyclohexasilane and method of preparing the same | |
| CN102849792B (en) | Method for preparing titanium tetrafluoride | |
| CN104140085B (en) | The apparatus and method of water and carbon dioxide in a kind of deep removal nitrous oxide | |
| CN114524421A (en) | Method for recovering nitrogen trifluoride from cold trap blow-down gas and preparing hydrofluoric acid | |
| CN108128758B (en) | SOF2 and SOF4 gas preparation method and system | |
| CN112090235B (en) | A purification system and purification process for hydrochloric acid by-product of chlorination reaction | |
| CN101723454A (en) | Method for preparing antimony pentafluoride | |
| CN103449371B (en) | Process method for purifying iodine pentafluoride | |
| CN101531400B (en) | Method for preparing antimony pentafluoride | |
| CN102115093B (en) | A kind of preparation method of high-purity enriched 11B boron trifluoride gas | |
| WO2021129322A1 (en) | Organic liquid purification and recovery device and method | |
| JP3641049B2 (en) | Production method of high purity hydrochloric acid | |
| CN105217575A (en) | A kind of reactive distillation removes the method for moisture in hydrogen fluoride | |
| CN102249188B (en) | Preparation method of germane gas |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Owner name: TIANJIN CHANGLU HUAXIN CHEMICAL INDUSTRY CO., LTD. Free format text: FORMER OWNER: RESEARCH INSTITUTE OF PHYSICAL AND CHEMICAL ENGINEERING OF NUCLEAR INDUSTRY HUAH Effective date: 20150518 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 300384 XIQING, TIANJIN TO: 300280 BINHAI NEW DISTRICT, TIANJIN |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20150518 Address after: Comprehensive service area Nangang Industrial Zone Development Zone 300280 Tianjin Binhai New Area Office Building second floor D building site 216 Patentee after: Huahe New-Technology Development Company, Research Institute of Physical and Chemical Engineering of Nuclear Industry Address before: 300384 Tianjin hi tech District of Xiqing City Huayuan Industrial Zone Development six road No. 6 Haitai green industry base building J room 104 Patentee before: Huahe New Technology Development Company, Research Institute of Physical and Chemical Engineering of Nuclear Industry |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20211124 Address after: 300180, No. 168 Jintang Road, Hedong District, Tianjin Patentee after: RESEARCH INSTITUTE OF PHYSICAL AND CHEMICAL ENGINEERING OF NUCLEAR INDUSTRY Address before: 300280 site [216], floor [2], building D, comprehensive service area, Nangang Industrial Zone, Binhai New Area Development Zone, Tianjin Patentee before: TIANJIN CHANGLU HUAXIN CHEMICAL CO.,LTD. |
|
| TR01 | Transfer of patent right |