CN213012644U - System for removing copper and bismuth ions in 1, 4-butynediol - Google Patents
System for removing copper and bismuth ions in 1, 4-butynediol Download PDFInfo
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- CN213012644U CN213012644U CN202021660777.8U CN202021660777U CN213012644U CN 213012644 U CN213012644 U CN 213012644U CN 202021660777 U CN202021660777 U CN 202021660777U CN 213012644 U CN213012644 U CN 213012644U
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- reactor
- butynediol
- butanediol
- copper
- adsorption
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- 229910001451 bismuth ion Inorganic materials 0.000 title claims abstract description 50
- 229910001431 copper ion Inorganic materials 0.000 title claims abstract description 39
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 239000010949 copper Substances 0.000 title claims abstract description 19
- DLDJFQGPPSQZKI-UHFFFAOYSA-N but-2-yne-1,4-diol Chemical compound OCC#CCO DLDJFQGPPSQZKI-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 238000001179 sorption measurement Methods 0.000 claims abstract description 48
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000003054 catalyst Substances 0.000 claims abstract description 26
- QAAXRTPGRLVPFH-UHFFFAOYSA-N [Bi].[Cu] Chemical compound [Bi].[Cu] QAAXRTPGRLVPFH-UHFFFAOYSA-N 0.000 claims abstract description 16
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 claims abstract description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 50
- 239000007788 liquid Substances 0.000 claims description 38
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 33
- 229910052759 nickel Inorganic materials 0.000 claims description 25
- 239000003463 adsorbent Substances 0.000 claims description 24
- 150000002500 ions Chemical class 0.000 claims description 24
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 11
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 11
- 239000007789 gas Substances 0.000 claims description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 abstract description 18
- 230000015572 biosynthetic process Effects 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 8
- 238000003786 synthesis reaction Methods 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 abstract 4
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 25
- 229910052782 aluminium Inorganic materials 0.000 description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 13
- 238000005984 hydrogenation reaction Methods 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 229910052797 bismuth Inorganic materials 0.000 description 5
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 5
- 238000003795 desorption Methods 0.000 description 3
- 241001501970 Prionailurus bengalensis Species 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 1
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 description 1
- -1 aluminum ions Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
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Abstract
A system for removing copper and bismuth ions in 1, 4-butynediol belongs to the technical field of 1, 4-butanediol production processes. The system comprises a butynediol reactor, an adsorption reactor and a butanediol reactor, wherein an aluminum-nickel adsorption layer is arranged in the adsorption reactor. According to the method, the copper bismuth ion removal system is arranged, so that the device can be used for effectively removing the copper bismuth ions in the 1, 4-butynediol while the normal production of qualified 1, 4-Butanediol (BDO) products is ensured, and the removal rate of the copper bismuth ions can reach more than 99%. The system reduces the influence of copper bismuth ions on the BDO synthesis catalyst, improves the selectivity and the service life of the BDO synthesis catalyst, reduces the butanol yield of the BDO device, and improves the economic benefit of the BDO device.
Description
Technical Field
The utility model relates to a desorption system of copper bismuth ion in 1, 4-butynediol, it belongs to BYD and refines or BDO production technology technical field.
Background
The main process technologies adopted at present comprise an Envyda process, a three-dimensional process, an F-T process and an ISP process, the acetylene and the formaldehyde generate crude BYD under the action of a copper bismuth catalyst, the crude BYD is rectified to generate refined BYD, the refined BYD is hydrogenated on a nickel-based catalyst to generate BDO, the crude BDO is rectified to generate a high-purity product BDO, the main byproduct of BYD hydrogenation is butanol, the butanol content in the crude BDO is increased along with the increase of the service time of the nickel-based hydrogenation catalyst, the butanol content is gradually increased from 0.5% in the initial stage to about 5% in the final stage of the hydrogenation catalyst, and the butanol content is also an important index for judging the use endpoint of the nickel-based hydrogenation catalyst. Through analysis, one of the main reasons for increasing butanol in the BDO hydrogenation synthesis process is that refined BYD contains 0.2-5ppm of copper bismuth ions due to the copper bismuth catalyst adopted in the BYD synthesis, and the copper bismuth ions are gradually adsorbed on the nickel-based hydrogenation synthesis catalyst along with the increase of the operation time of the BDO hydrogenation synthesis catalyst, so that the activity of the catalyst is changed, and the butanol content in the BDO is gradually increased.
Disclosure of Invention
For solving the problem that exists among the prior art, the utility model provides a desorption system of copper bismuth ion in 1, 4-butynediol, this system has introduced the device that copper bismuth ion adsorbs the desorption, does not introduce new ion harmful to BDO hydrogenation catalyst simultaneously, has guaranteed nickel base hydrogenation catalyst's long-term stability, has reduced the content of butanol in the BDO.
The utility model provides a technical scheme that technical problem adopted is: a system for removing copper and bismuth ions in 1, 4-butynediol comprises a butynediol reactor and a butanediol reactor, wherein an acetylene bottle in the system is connected to the butynediol reactor through a gas inlet of the butynediol reactor after passing through an acetylene pipe, and a formaldehyde bottle is connected to the butynediol reactor through a gas inlet of the butynediol reactor after passing through a formaldehyde pipe; the butynediol reactor is connected with a first liquid pipe through a butynediol outlet, and the first liquid pipe is connected to the adsorption reactor through an adsorber inlet after sequentially passing through a first liquid valve, a liquid pump and a first ion monitor; the adsorption reactor is connected to a second liquid pipe through an outlet of the adsorber, and the second liquid pipe sequentially passes through a second ion monitor and a second liquid valve and then is connected to the butanediol reactor through a liquid inlet; a hydrogen cylinder is connected to the butanediol reactor through a gas inlet of the butanediol reactor after passing through a hydrogen pipe; the butanediol reactor is connected with a butanediol pipe through a butanediol outlet; an aluminum nickel adsorbent layer is arranged in the adsorption reactor.
The butynediol reactor is internally provided with a copper bismuth catalyst layer, and the butanediol reactor is internally provided with a nickel-based catalyst layer.
The adsorption reactor is in a cylinder type, a tube type or a box type.
The inlet of the adsorber is arranged at the lower part of the adsorption reactor, and the outlet of the adsorber is arranged at the upper part of the adsorption reactor.
The aluminum-nickel adsorbent layer can be provided with an aluminum adsorbent, a nickel adsorbent or an aluminum-nickel mixed adsorbent. The adsorbent is porous aluminum and nickel or porous aluminum or nickel, the aluminum content is 5-100%, the nickel content is 5-100%, and the specific surface area of the adsorbent or catalyst is 5-1000m2Per g, the preferred specific surface area is 40-500m2The grain size is 0.1mm-100mm, preferably 1-50 mm.
The system is suitable for a BYD liquid copper and bismuth removing system containing copper and bismuth, and comprises a reaction device which adopts acetylene and formaldehyde to react to generate BYD and adopts BYD hydrogenation to generate BDO. The system adsorbs an adsorbent which is filled in the reactor and can adsorb copper and bismuth ions, so that the BYD liquid can remove the contained copper and bismuth ions through the reactor. The form of the reaction reactor can be various forms of reactors such as a cylinder type, a tube type, a box type and the like, and the number of the reactors can be one or more;
the BYD liquid inlet and outlet of the reactor can be arranged at any position of the reactor, and the BYD liquid can be fully contacted with the adsorbent or the catalyst.
The temperature in the reaction process can be 0-180 ℃, and the preferable reaction temperature is 30-100 ℃; the pressure in the reaction process can be any pressure, and the preferable reaction pressure is normal pressure-2.0 MPa; the liquid hourly space velocity in the reaction process is 0.1-20L/(L.cat). h, and the preferable liquid hourly space velocity is 0.5-5L/(L.cat). h.
The utility model has the advantages that: the system is suitable for a BYD liquid copper and bismuth removing system containing copper and bismuth, and comprises a reaction device which adopts acetylene and formaldehyde to react to generate BYD and adopts BYD hydrogenation to generate BDO. The system adsorbs an adsorbent which is filled in the reactor and can adsorb copper and bismuth ions, so that the BYD liquid can remove the contained copper and bismuth ions through the reactor. The copper bismuth ions in the BYD are adsorbed by a nickel-based or aluminum-based adsorbent, so that the concentration of the copper bismuth ions in the BYD can be greatly reduced, and the copper ions and the bismuth ions in the BYD can be reduced by over 99 percent; meanwhile, the components of the adopted nickel-based or aluminum-based adsorbent are the same as those of the BDO hydrogenation and catalyst formation, and trace nickel ions or aluminum ions introduced by the adsorbent cannot influence the performance of the BDO hydrogenation and catalyst formation, so that the amount of copper and bismuth adsorbed on the surface of the nickel-based catalyst in the using process can be greatly reduced, the using time of the catalyst is prolonged, the amount of over-hydrogenated product butanol is reduced, and the economic benefit of the whole BDO device is improved.
Drawings
FIG. 1 is a system for removing copper and bismuth ions from 1, 4-butynediol.
In the figure: 1. butynediol reactor, 1a, butynediol reactor gas inlet, 1b, butynediol outlet, 2, adsorption reactor, 2a, adsorber inlet, 2b, adsorber outlet, 2c, nickel-cobalt adsorption layer, 3, butanediol reactor, 3a, liquid inlet, 3b, butanediol reactor gas inlet, 3c, nickel-based catalyst layer, 3d, butanediol outlet, 4, first liquid tube, 5, second liquid tube, 6, liquid pump, 7, first ion monitor, 8, second ion detector, 9, first liquid valve, 10, second liquid valve, 11, acetylene cylinder, 11a, acetylene tube, 12, formaldehyde cylinder, 12a, formaldehyde hydrogen tube, 13, cylinder, 13a, hydrogen tube, 14, butanediol tube.
Detailed Description
FIG. 1 shows a system for removing copper and bismuth ions from 1, 4-butynediol, which comprises a butynediol reactor 1 and a butanediol reactor 3, wherein an acetylene cylinder 11 in the system is connected to the butynediol reactor 1 through a butynediol reactor gas inlet 1a after passing through an acetylene pipe 11a, and a formaldehyde cylinder 12 is connected to the butynediol reactor 1 through a butynediol reactor gas inlet 1a after passing through a formaldehyde pipe 12 a; the butynediol reactor 1 is connected with a first liquid pipe 4 through a butynediol outlet 1b, and the first liquid pipe 4 is connected with the adsorption reactor 2 through an adsorber inlet 2a after sequentially passing through a first liquid valve 9, a liquid pump 6 and a first ion monitor 7; the adsorption reactor 2 is connected to a second liquid pipe 5 through an adsorber outlet 2b, and the second liquid pipe 5 is connected to the butanediol reactor 3 through a liquid inlet 3a after sequentially passing through a second ion monitor 8 and a second liquid valve 10; the hydrogen cylinder 13 is connected to the butanediol reactor 3 through a gas inlet 3b of the butanediol reactor after passing through a hydrogen pipe 13 a; the butanediol reactor 3 is connected with a butanediol pipe 14 through a butanediol outlet 3 d; an aluminum nickel adsorbent layer 2c is arranged in the adsorption reactor 2.
The butynediol reactor 1 is internally provided with a copper bismuth catalyst layer 1d, and the butanediol reactor 3 is internally provided with a nickel-based catalyst layer 3 c. The adsorption reactor 2 is a cylinder type, a tube type or a box type. The adsorber inlet 2a is disposed at the lower portion of the adsorption reactor 2, and the adsorber outlet 2b is disposed at the upper portion of the adsorption reactor 2.
Example 1
In the adsorption reactor 2, an adsorbent 1.0m containing 60% of nickel and 40% of aluminum and having a specific surface area of 150m2/g is filled in an aluminum-nickel adsorption layer 2c3BYD solution containing 2.2ppm of copper ions and 0.56ppm of bismuth ions at 0.2MPa and 55 deg.C per hour at 1.5 m3The rate of the second ion detector 8 is introduced into the adsorption reactor 2 from the lower part of the reactor, the materials are discharged from the outlet 2b of the upper adsorber, the content of copper ions and bismuth ions is measured by the second ion detector 8, and the removal rate of the copper ions and the bismuth ions is calculated, see an example table.
Example 2
Sponge nickel containing 100% of nickel is filled in the aluminum nickel adsorption layer 2c in the adsorption reactor 2, and the specific surface area is 87m2Adsorbent 1.0 m/g3BYD solution containing 2.2ppm of copper ions and 0.56ppm of bismuth ions at 0.2MPa and 55 deg.C per hour at 1.5 m3From the rate of reactionThe lower part of the device is introduced into an adsorption reactor 2, the materials are discharged from an outlet 2b of an upper adsorber, the content of copper ions and bismuth ions is measured by a second ion monitor 8, and the removal rate of the copper ions and the bismuth ions is calculated, see an embodiment table.
Example 3
In the adsorption reactor 2, an adsorbent 1.0m containing 60% of nickel and 40% of aluminum and having a specific surface area of 150m2/g is filled in an aluminum-nickel adsorption layer 2c3BYD solution containing 2.2ppm of copper ions and 0.56ppm of bismuth ions at 0.2MPa and 85 deg.C per hour at 1.5 m3The rate of the second ion detector 8 is introduced into the adsorption reactor 2 from the lower part of the reactor, the materials are discharged from the outlet 2b of the upper adsorber, the content of copper ions and bismuth ions is measured by the second ion detector 8, and the removal rate of the copper ions and the bismuth ions is calculated, see an example table.
Example 4
In the adsorption reactor 2, an adsorbent 1.0m containing 60% of nickel and 40% of aluminum and having a specific surface area of 150m2/g is filled in an aluminum-nickel adsorption layer 2c3BYD solution containing 2.2ppm of copper ions and 0.56ppm of bismuth ions at 0.2MPa and a reaction temperature of 55 deg.C at 4.5 m per hour3The rate of the second ion detector 8 is introduced into the adsorption reactor 2 from the lower part of the reactor, the materials are discharged from the outlet 2b of the upper adsorber, the content of copper ions and bismuth ions is measured by the second ion detector 8, and the removal rate of the copper ions and the bismuth ions is calculated, see an example table.
Example 5
In the adsorption reactor 2, an adsorbent 1.0m containing 60% of nickel and 40% of aluminum and having a specific surface area of 150m2/g is filled in an aluminum-nickel adsorption layer 2c3BYD solution containing 2.2ppm of copper ions and 0.56ppm of bismuth ions at 0.2MPa and 55 deg.C per hour at 1.5 m3The rate of the second ion detector 8 is introduced into the adsorption reactor 2 from the lower part of the reactor, the materials are discharged from the outlet 2b of the upper adsorber, the content of copper ions and bismuth ions is measured by the second ion detector 8, and the removal rate of the copper ions and the bismuth ions is calculated, see an example table.
Example 6
In the adsorption reactor 2, an adsorbent 1.0m containing 60% of nickel and 40% of aluminum and having a specific surface area of 150m2/g is filled in an aluminum-nickel adsorption layer 2c3The adsorbent is divided into two parts, which are respectively filled in seriesBYD solution containing 2.2ppm copper ions and 0.56ppm bismuth ions at 1.5 m/h in two adsorption reactors at 0.2MPa and 55 deg.C3The rate of the second ion detector 8 is introduced into the adsorption reactor 2 from the lower part of the reactor, the materials are discharged from the outlet 2b of the upper adsorber, the content of copper ions and bismuth ions is measured by the second ion detector 8, and the removal rate of the copper ions and the bismuth ions is calculated, see an example table.
Example 7
In the adsorption reactor 2, an adsorbent 1.0m containing 60% of nickel and 40% of aluminum and having a specific surface area of 150m2/g is filled in an aluminum-nickel adsorption layer 2c3BYD solution containing 0.2ppm copper ion and 0.13ppm bismuth ion at 0.2MPa and 55 deg.C per hour at 1.5 m3The rate of the second ion detector 8 is introduced into the adsorption reactor 2 from the lower part of the reactor, the materials are discharged from the outlet 2b of the upper adsorber, the content of copper ions and bismuth ions is measured by the second ion detector 8, and the removal rate of the copper ions and the bismuth ions is calculated, see an example table.
Example 8
In the adsorption reactor 2, an adsorbent 1.0m containing 60% of nickel and 40% of aluminum and having a specific surface area of 150m2/g is filled in an aluminum-nickel adsorption layer 2c3BYD solution containing 2.2ppm of copper ions and 0.56ppm of bismuth ions at 0.8 m/hr at 0.2MPa and 85 deg.C3The rate of the second ion detector 8 is introduced into the adsorption reactor 2 from the lower part of the reactor, the materials are discharged from the outlet 2b of the upper adsorber, the content of copper ions and bismuth ions is measured by the second ion detector 8, and the removal rate of the copper ions and the bismuth ions is calculated, see an example table.
Examples table
Claims (4)
1. A system for removing copper and bismuth ions in 1, 4-butynediol comprises a butynediol reactor (1) and a butanediol reactor (3), and is characterized in that: in the system, an acetylene bottle (11) is connected to a butynediol reactor (1) through a butynediol reactor gas inlet (1 a) after passing through an acetylene pipe (11 a), and a formaldehyde bottle (12) is connected to the butynediol reactor (1) through a butynediol reactor gas inlet (1 a) after passing through a formaldehyde pipe (12 a); the butynediol reactor (1) is connected with a first liquid pipe (4) through a butynediol outlet (1 b), and the first liquid pipe (4) is connected to the adsorption reactor (2) through an adsorber inlet (2 a) after sequentially passing through a first liquid valve (9), a liquid pump (6) and a first ion monitor (7); the adsorption reactor (2) is connected to a second liquid pipe (5) through an adsorber outlet (2 b), and the second liquid pipe (5) is connected to the butanediol reactor (3) through a liquid inlet (3 a) after sequentially passing through a second ion monitor (8) and a second liquid valve (10); a hydrogen cylinder (13) is connected to the butanediol reactor (3) through a hydrogen pipe (13 a) and a butanediol reactor gas inlet (3 b); the butanediol reactor (3) is connected with a butanediol pipe (14) through a butanediol outlet (3 d); an aluminum nickel adsorbent layer (2 c) is arranged in the adsorption reactor (2).
2. The system for removing copper and bismuth ions in 1, 4-butynediol according to claim 1, wherein: a copper bismuth catalyst layer (1 d) is arranged in the butynediol reactor (1), and a nickel-based catalyst layer (3 c) is arranged in the butanediol reactor (3).
3. The system for removing copper and bismuth ions in 1, 4-butynediol according to claim 1, wherein: the adsorption reactor (2) is in a cylinder type, a tube type or a box type.
4. The system for removing copper and bismuth ions in 1, 4-butynediol according to claim 1, wherein: the adsorber inlet (2 a) is arranged at the lower part of the adsorption reactor (2), and the adsorber outlet (2 b) is arranged at the upper part of the adsorption reactor (2).
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| CN202021660777.8U CN213012644U (en) | 2020-08-11 | 2020-08-11 | System for removing copper and bismuth ions in 1, 4-butynediol |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202021660777.8U CN213012644U (en) | 2020-08-11 | 2020-08-11 | System for removing copper and bismuth ions in 1, 4-butynediol |
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Address after: 116052 327 Shun Le street, Lushun Economic Development Zone, Dalian, Liaoning Patentee after: Dalian Ruike Technology Co.,Ltd. Address before: 116052 327 Shun Le street, Lushun Economic Development Zone, Dalian, Liaoning Patentee before: DALIAN RUIKE SCIENCE & TECHNOLOGY Co.,Ltd. |
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Denomination of utility model: A system for removing copper and bismuth ions from 1,4-butynediol Effective date of registration: 20221108 Granted publication date: 20210420 Pledgee: Guangfa Bank Co.,Ltd. Dalian Branch Pledgor: Dalian Ruike Technology Co.,Ltd. Registration number: Y2022210000192 |
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Date of cancellation: 20231108 Granted publication date: 20210420 Pledgee: Guangfa Bank Co.,Ltd. Dalian Branch Pledgor: Dalian Ruike Technology Co.,Ltd. Registration number: Y2022210000192 |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of utility model: A Removal System for Copper and Bismuth Ions in 1,4-Butynediol Effective date of registration: 20231110 Granted publication date: 20210420 Pledgee: Guangfa Bank Co.,Ltd. Dalian Branch Pledgor: Dalian Ruike Technology Co.,Ltd. Registration number: Y2023210000277 |