CN115869900A - Composite dechlorinating agent and preparation method thereof - Google Patents
Composite dechlorinating agent and preparation method thereof Download PDFInfo
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- CN115869900A CN115869900A CN202211682031.0A CN202211682031A CN115869900A CN 115869900 A CN115869900 A CN 115869900A CN 202211682031 A CN202211682031 A CN 202211682031A CN 115869900 A CN115869900 A CN 115869900A
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- Prior art keywords
- clay
- dechlorination
- agent
- molecular sieve
- nano
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- 230000000382 dechlorinating effect Effects 0.000 title claims abstract description 69
- 239000002131 composite material Substances 0.000 title claims abstract description 7
- 238000002360 preparation method Methods 0.000 title description 7
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 83
- 239000002245 particle Substances 0.000 claims abstract description 61
- 238000006298 dechlorination reaction Methods 0.000 claims abstract description 45
- 239000004927 clay Substances 0.000 claims abstract description 44
- 239000002808 molecular sieve Substances 0.000 claims abstract description 40
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 40
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000460 chlorine Substances 0.000 claims abstract description 34
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 34
- 238000002156 mixing Methods 0.000 claims abstract description 22
- 150000001875 compounds Chemical class 0.000 claims abstract description 19
- 229910001948 sodium oxide Inorganic materials 0.000 claims abstract description 19
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000005469 granulation Methods 0.000 claims abstract description 17
- 230000003179 granulation Effects 0.000 claims abstract description 17
- 239000011159 matrix material Substances 0.000 claims abstract description 11
- 238000005245 sintering Methods 0.000 claims abstract description 11
- 239000012802 nanoclay Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract description 6
- 238000001179 sorption measurement Methods 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 238000002407 reforming Methods 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 235000019270 ammonium chloride Nutrition 0.000 description 4
- 150000001805 chlorine compounds Chemical class 0.000 description 4
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 4
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 229910001504 inorganic chloride Inorganic materials 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000004045 organic chlorine compounds Chemical class 0.000 description 1
- 150000002897 organic nitrogen compounds Chemical class 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a composite dechlorinating agent; the clay-based composite material is prepared by sequentially granulating, blending, granulating and blending a matrix made of clay, nano-sodium oxide, nano-clay and a molecular sieve dechlorinating agent, wherein firstly, the clay is used as the matrix and is granulated by a granulator to obtain clay particles; secondly, mixing the nano sodium oxide and the nano clay uniformly, carrying out ball granulation on the surfaces of clay particles, and then carrying out high-temperature sintering to obtain inorganic dechlorination particles; and finally, uniformly mixing inorganic chlorine dechlorination particles, a molecular sieve dechlorinating agent with the diameter of 4-5mm and a molecular sieve dechlorinating agent with the diameter of 2-3mm to obtain the compound dechlorinating agent. The compound dechlorinating agent has the beneficial effects of strong chloride adsorption capacity, good dechlorinating effect and low cost.
Description
Technical Field
The invention relates to the field of dechlorinating agents, in particular to a compound dechlorinating agent and a preparation method thereof.
Background
The harm of chloride to a reformate production device is mainly reflected in the corrosion of HCl to equipment and pipelines, ammonium chloride blocks tower tray sieve holes, and hydrogen chloride in a gaseous state does not seriously corrode the equipment and the pipelines, but hydrochloric acid is formed once water is met, so that a strong corrosion effect is generated; further, since the organic chlorine compound in naphtha generates hydrogen chloride in the case of pre-hydrogenation, the organic nitrogen compound generates ammonia in the pre-hydrogenation reaction condition, and ammonium chloride can be generated from hydrogen chloride and ammonia, and ammonium chloride can be precipitated at a low temperature portion to block the sieve holes of the tray in the column, thereby lowering the separation accuracy, dechlorination should be performed in time in the above-mentioned process.
In order to solve the above technical problems, in the prior art, a fixed bed dechlorinating agent is mostly adopted to remove chlorides, the dechlorinating agent comprises materials such as activated alumina and zinc oxide, the activated alumina has the defect of promoting the formation of organic chlorides, gum and green oil, the zinc oxide type dechlorinating agent has the problems of particle breakage and pressure drop accumulation, further causing the defects of poor dechlorinating effect, incapability of removing organic chlorides and short service life of the dechlorinating agent, and particularly, the dechlorinating effect is poor at 40-80 ℃ in a reforming section, further causing the increase of dechlorinating cost and frequent agent replacement. Therefore, in the production of naphtha and reformate, it is urgently needed to develop a dechlorinating agent and a preparation method thereof, which have strong chloride adsorption capacity, good dechlorinating effect and low cost, so as to effectively remove inorganic chlorides and organic chlorides in gas phase and liquid phase, and further avoid the influence of equipment corrosion, ammonium chloride deposition and the like on production equipment.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a compound dechlorinating agent with strong chloride adsorption capacity, good dechlorinating effect and low cost and a preparation method thereof, so as to effectively remove inorganic chloride and organic chloride in gas phase and liquid phase.
In order to solve the problems, the invention provides the following technical scheme:
a composite dechlorinating agent is prepared from clay matrix, nano-class sodium oxide, nano-class clay and molecular sieve dechlorinating agent through granulating, mixing, granulating and mixing, and features high dechlorinating effect, low cost and high safety.
The invention adopts nano-scale sodium oxide as the main agent of the inorganic dechlorination particles, has the characteristics of quick low-temperature dechlorination reaction and high chlorine capacity, adopts the strong polarity combination of the molecular sieve dechlorination agent and the organic chlorine, has the characteristic of high efficiency of removing the organic chlorine, and adopts the blending of the inorganic chlorine dechlorination particles and the molecular sieve dechlorination agent to achieve the characteristic of low cost of removing ton oil. In addition, the phi 4-5mm type molecular sieve dechlorinating agent and the phi 2-3mm type molecular sieve dechlorinating agent refer to molecular sieve dechlorinating agents with the pore diameters of 4-5mm and 2-3mm respectively, and the molecular sieve dechlorinating agent is prepared by blending sodium oxide particles and a molecular sieve.
Preferably, the technical scheme of the invention also comprises that the weight part ratio of the phi 4-5mm type molecular sieve dechlorinating agent to the phi 2-3mm type molecular sieve dechlorinating agent is 1-5.
Another objective of the present application is to provide a method for preparing a compound dechlorinating agent, comprising the following steps:
(1) Taking clay as a matrix, and granulating by a granulator to obtain clay particles;
(2) Mixing nano sodium oxide and nano clay uniformly, carrying out ball granulation on the surfaces of clay particles, and then carrying out high-temperature sintering to obtain inorganic dechlorination particles;
(3) The inorganic chlorine dechlorination particles, the molecular sieve dechlorination agent with the diameter of 4-5mm and the molecular sieve dechlorination agent with the diameter of 2-3mm are evenly mixed to obtain the compound dechlorination agent.
The composite dechlorinating agent prepared by the method can ensure that the actual working chlorine capacity is more than or equal to 8 percent, the inorganic chlorine removal rate is more than or equal to 98 percent, the organic chlorine removal rate is more than or equal to 40 percent and the ton oil treatment cost is less than or equal to 1.00 yuan under the working condition of a reforming device in a wide-range working environment at the temperature of 40-200 ℃.
Preferably, the technical scheme of the invention also comprises that the particle size of the clay particles in the step (1) is 0.8-1.2mm.
The technical scheme of the invention also comprises that in the step (2), the nano-scale sodium oxide and the nano-scale clay are uniformly mixed, and the ball granulation is continued on the surface of clay particles, wherein the particle size of the ball granulation is 3-5mm.
Further, the technical scheme of the invention also comprises that the weight part ratio of the nano-scale sodium oxide to the nano-scale clay in the step (2) is 4-10.
Preferably, the temperature of the high-temperature sintering in the step (2) is 500-1000 ℃.
The technical scheme of the invention also comprises that the weight portion ratio of the inorganic chlorine dechlorination particles, the phi 4-5mm type molecular sieve dechlorination agent and the phi 2-3mm type molecular sieve dechlorination agent is 5-8: 1-5 parts of: 1-5 parts.
The preferable scheme of the preparation method of the compound dechlorinating agent comprises the following steps:
(1) Taking clay as a matrix, and granulating by a granulator to obtain clay particles with the particle size of 0.8-1.2 mm;
(2) Uniformly mixing 4-10 parts of nano sodium oxide and 1-3 parts of nano clay, continuously carrying out ball granulation on the surfaces of clay particles, wherein the particle size is 3-5mm, and then carrying out high-temperature sintering to obtain inorganic chlorine dechlorination particles;
(3) Uniformly mixing 5-8 parts of inorganic chlorine dechlorination particles, 1-5 parts of a phi 4-5mm type molecular sieve dechlorinating agent and 1-5 parts of a phi 2-3mm type molecular sieve dechlorinating agent to obtain the compound dechlorinating agent.
It should be noted that, the above-mentioned scheme does not limit the weight portion of the clay particles, and the ball granulation particle size is 3-5mm.
The invention has the beneficial effects that: compared with the prior art, the invention aims to provide the compound dechlorinating agent with strong chloride adsorption capacity, good dechlorinating effect and low cost and the preparation method thereof, in order to realize the technical effects, the invention uses clay particles, nano-scale sodium oxide and nano-scale clay to carry out ball granulation, the ball granulation is uniformly mixed with molecular sieve dechlorinating agents with different pore diameters after high-temperature sintering, the nano-scale sodium oxide is used as a main agent of inorganic dechlorinating particles, has the characteristics of quick dechlorinating reaction at low temperature and high chlorine capacity, the nano-scale clay has the characteristic of strong adsorption capacity, the molecular sieve dechlorinating agent and organic chlorine have strong polarity combination, the dechlorinating agent has the characteristic of high organic chlorine removal efficiency, the inorganic chlorine dechlorinating particles and the molecular sieve dechlorinating agent are mixed to achieve the characteristic of low ton oil removal cost, and the compound dechlorinating agent prepared by the method has the characteristics of more than or equal to 8 percent of actual working chlorine removal rate, more than or equal to 98 percent of organic chlorine removal rate, and less than or equal to 40 percent of ton oil treatment cost less than 1.00 yuan under the working condition of a reforming device at 40-200 ℃.
Detailed Description
In order to make those skilled in the art better understand the technical solutions of the present invention, the technical solutions of the present invention will be clearly and completely described below with reference to the embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) Taking clay as a matrix, and granulating by a granulator to obtain clay particles with the particle size of 0.8 mm;
(2) Mixing 10 parts of nano sodium oxide and 2 parts of nano clay uniformly, carrying out ball granulation on the surfaces of clay particles continuously until the particle size is 4mm, and then carrying out high-temperature sintering to obtain inorganic dechlorination particles;
(3) Uniformly mixing 8 parts of inorganic chlorine dechlorination particles, 2 parts of a phi 4-5mm type molecular sieve dechlorination agent and 2 parts of a phi 2-3mm type molecular sieve dechlorination agent to obtain the compound dechlorination agent.
The compound dechlorinating agent prepared by the method has the actual working chlorine capacity of 8.9 percent, the inorganic chlorine removal rate of 99.2 percent, the organic chlorine removal rate of 45 percent and the ton oil treatment cost of 0.87 yuan under the working condition of a 40-200 ℃ reforming device.
Example 2
(1) Taking clay as a matrix, and granulating by a granulator to obtain clay particles with the particle size of 1 mm;
(2) Uniformly mixing 8 parts of nano-scale sodium oxide and 3 parts of nano-scale clay, continuously carrying out ball granulation on the surfaces of clay particles, wherein the particle size is 3mm, and then carrying out high-temperature sintering to obtain inorganic dechlorination particles;
(3) And uniformly mixing 6 parts of inorganic chlorine dechlorination particles, 3 parts of a phi 4-5mm type molecular sieve dechlorinating agent and 3 parts of a phi 2-3mm type molecular sieve dechlorinating agent to obtain the compound dechlorinating agent.
The compound dechlorinating agent prepared by the method has the actual working chlorine capacity of 9.1 percent, the inorganic chlorine removal rate of 99.3 percent, the organic chlorine removal rate of 53 percent and the ton oil treatment cost of 0.91 yuan under the working condition of a 40-200 ℃ reforming device.
Example 3
(1) Taking clay as a matrix, and granulating by a granulator to obtain clay particles with the particle size of 1.2 mm;
(2) Uniformly mixing 6 parts of nano-scale sodium oxide and 4 parts of nano-scale clay, continuously carrying out ball granulation on the surfaces of clay particles, wherein the particle size is 5mm, and then carrying out high-temperature sintering to obtain inorganic dechlorination particles;
(3) 6 parts of inorganic chlorine dechlorination particles, 4 parts of a dechlorination agent with a phi 4-5mm molecular sieve and 4 parts of a dechlorination agent with a phi 2-3mm molecular sieve are uniformly mixed to obtain the compound dechlorination agent.
The compound dechlorinating agent prepared by the method has the actual working chlorine capacity of 8.6 percent, the inorganic chlorine removal rate of 99.3 percent, the organic chlorine removal rate of 59 percent and the ton oil treatment cost of 0.95 yuan under the working condition of a 40-200 ℃ reforming device.
Although the present invention has been described in detail by way of the preferred embodiments, the present invention is not limited thereto. Various equivalent modifications or substitutions can be made on the embodiments of the present invention by those skilled in the art without departing from the spirit and the spirit of the present invention, and the modifications or substitutions are within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (9)
1. A compound dechlorinating agent is characterized in that: the dechlorination agent is prepared by sequentially carrying out granulation, blending, granulation and blending processes on a matrix made of clay, nano-scale sodium oxide, nano-scale clay and a molecular sieve dechlorination agent, wherein the molecular sieve dechlorination agent is a combination of a phi 4-5mm type molecular sieve dechlorination agent and a phi 2-3mm type molecular sieve dechlorination agent.
2. The complex dechlorination agent according to claim 1, characterized in that: the weight portion ratio of the phi 4-5mm type molecular sieve dechlorinating agent to the phi 2-3mm type molecular sieve dechlorinating agent is 1-5.
3. The method for preparing a complex dechlorinating agent according to claim 1, wherein the dechlorinating agent comprises: the method comprises the following steps:
(1) Taking clay as a matrix, and granulating by a granulator to obtain clay particles;
(2) Mixing nano sodium oxide and nano clay uniformly, carrying out ball granulation on the surfaces of clay particles continuously, and then carrying out high-temperature sintering to obtain inorganic dechlorination particles;
(3) The compound dechlorinating agent is obtained by uniformly mixing inorganic chlorine dechlorinating particles, a phi 4-5mm type molecular sieve dechlorinating agent and a phi 2-3mm type molecular sieve dechlorinating agent.
4. A method for preparing a complex dechlorinating agent according to claim 3, characterized by: the particle size of the clay particles in the step (1) is 0.8-1.2mm.
5. A method for preparing a complex dechlorinating agent according to claim 3, characterized by: and (3) uniformly mixing the nano-scale sodium oxide and the nano-scale clay in the step (2), and continuing ball granulation on the surfaces of clay particles, wherein the particle size of the ball granulation is 3-5mm.
6. The method for preparing a complex dechlorinating agent according to claim 5, wherein the dechlorinating agent comprises: the weight part ratio of the nano-scale sodium oxide to the nano-scale clay in the step (2) is 4-10.
7. A method for preparing a complex dechlorinating agent according to claim 3, characterized by: the temperature of the high-temperature sintering in the step (2) is 500-1000 ℃.
8. A process for producing a composite dechlorinating agent according to claim 3, comprising: the weight portion ratio of the inorganic chlorine dechlorination particles, the phi 4-5mm type molecular sieve dechlorination agent and the phi 2-3mm type molecular sieve dechlorination agent is 5-8: 1-5 parts of: 1-5 parts.
9. A method for preparing a complex dechlorinating agent according to claim 3, characterized by: the method comprises the following steps:
(1) Taking clay as a matrix, and granulating by a granulator to obtain clay particles with the particle size of 0.8-1.2 mm;
(2) Uniformly mixing 4-10 parts of nano sodium oxide and 1-3 parts of nano clay, continuously carrying out ball granulation on the surfaces of clay particles, wherein the particle size is 3-5mm, and then carrying out high-temperature sintering to obtain inorganic chlorine dechlorination particles;
(3) 5-8 parts of inorganic chlorine dechlorination particles, 1-5 parts of a phi 4-5mm molecular sieve dechlorination agent and 1-5 parts of a phi 2-3mm molecular sieve dechlorination agent are uniformly mixed to obtain the compound dechlorination agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211682031.0A CN115869900A (en) | 2022-12-27 | 2022-12-27 | Composite dechlorinating agent and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211682031.0A CN115869900A (en) | 2022-12-27 | 2022-12-27 | Composite dechlorinating agent and preparation method thereof |
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| CN115869900A true CN115869900A (en) | 2023-03-31 |
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| CN202211682031.0A Pending CN115869900A (en) | 2022-12-27 | 2022-12-27 | Composite dechlorinating agent and preparation method thereof |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1223898A (en) * | 1998-11-24 | 1999-07-28 | 湖北省化学研究所 | Dechlorinating agent and its preparing method |
| CN1539921A (en) * | 2003-10-28 | 2004-10-27 | 王晓东 | Composite multifunctional dechlorination agent |
| CN112892580A (en) * | 2021-01-19 | 2021-06-04 | 浙江卫星能源有限公司 | Normal-temperature gas-phase dechlorinating agent and preparation method thereof |
| CN113736507A (en) * | 2020-05-27 | 2021-12-03 | 中国石油天然气股份有限公司 | Liquid-phase dechlorinating agent, preparation method and application thereof |
| CN114210307A (en) * | 2022-01-05 | 2022-03-22 | 上海恒业微晶材料科技股份有限公司 | Preparation method and application of novel carbon-silicon material |
| CN115193427A (en) * | 2022-07-27 | 2022-10-18 | 山东秋水化学科技有限公司 | Molecular sieve for dechlorination and preparation method thereof |
-
2022
- 2022-12-27 CN CN202211682031.0A patent/CN115869900A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1223898A (en) * | 1998-11-24 | 1999-07-28 | 湖北省化学研究所 | Dechlorinating agent and its preparing method |
| CN1539921A (en) * | 2003-10-28 | 2004-10-27 | 王晓东 | Composite multifunctional dechlorination agent |
| CN113736507A (en) * | 2020-05-27 | 2021-12-03 | 中国石油天然气股份有限公司 | Liquid-phase dechlorinating agent, preparation method and application thereof |
| CN112892580A (en) * | 2021-01-19 | 2021-06-04 | 浙江卫星能源有限公司 | Normal-temperature gas-phase dechlorinating agent and preparation method thereof |
| CN114210307A (en) * | 2022-01-05 | 2022-03-22 | 上海恒业微晶材料科技股份有限公司 | Preparation method and application of novel carbon-silicon material |
| CN115193427A (en) * | 2022-07-27 | 2022-10-18 | 山东秋水化学科技有限公司 | Molecular sieve for dechlorination and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 解国应等: "吸附法脱除油品中有机氯研究进展", 《石油化工》, vol. 49, no. 4, 15 April 2020 (2020-04-15), pages 411 - 414 * |
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