CN114466824A - High-concentration iron-series flocculant and production method thereof - Google Patents
High-concentration iron-series flocculant and production method thereof Download PDFInfo
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- CN114466824A CN114466824A CN202080068376.XA CN202080068376A CN114466824A CN 114466824 A CN114466824 A CN 114466824A CN 202080068376 A CN202080068376 A CN 202080068376A CN 114466824 A CN114466824 A CN 114466824A
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- C02F1/00—Treatment of water, waste water, or sewage
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Abstract
According to the present invention, an ultra-high concentration polymeric ferric sulfate solution that cannot be produced by a conventional production method due to a long reaction time can be produced in a short time. When the concentration of sulfate ion is [ SO ]4 2‑]And the total iron concentration is [ T-Fe ]](in terms of molar concentration), the raw materials are adjusted so as to satisfy the following relationship, and the polymeric ferric sulfate solution is produced by a high-temperature high-pressure reaction of the raw materials. Molar ratio of sulfate ions to total iron (SO)4 2‑T-Fe) of at least 1.2 and when the sulfate ion concentration is [ SO ]4 2‑]When is in [ SO ]4 2‑]At most 35% by weight.
Description
Technical Field
The invention relates to a high-concentration iron-based flocculant for wastewater treatment and a production method thereof.
Background
The applicant of the present patent application has sold wastewater treatment chemicals centered on the originally developed iron-based inorganic polymeric flocculant "Polytetsu" (registered trademark), and has a plurality of related patents.
Among these patents, patent document 1 describes that sodium nitrite and an oxidizing agent as a catalyst are added to ferrous sulfate (FeSO) as an iron-based raw material4) And an oxidation reaction is caused to proceed for about 10 hours at normal temperature and pressure, thereby obtaining polymeric ferric sulfate ([ Fe ]2(OH)n(SO4)3-n/2]mHere, 0<n is less than or equal to 2, and m is a natural number).
However, since this method requires a long reaction time, it is required to shorten the reaction time by some method.
Then, the production method of the iron-based inorganic flocculant described in patent document 2 is to use magnetite (Fe)3O4) As a method of an iron-based raw material, and a molar ratio of sulfate ions to iron ions is adjusted, and thereafter a reaction is carried out at a temperature of 120 to 180 ℃ in a closed vessel. The method is a production method aiming at shortening the reaction time by conducting the reaction at high temperature and high pressure, but the method still requires a reaction time of 0.8 to 1.5 hours.
Patent document 3 discloses a method for producing an iron-based flocculant in which iron sesquioxide (Fe) as an iron-based raw material is used2O3) Dissolved in excess sulfuric acid to form iron (Fe) sulfate2(SO4)3) And then partially neutralized with hydrated iron trioxide.
However, since this method consists of two steps of a step of dissolving ferric oxide in sulfuric acid and a step of partially neutralizing the formed ferric sulfate, there is a drawback that the production method becomes complicated and a polymeric ferric sulfate solution cannot be efficiently formed. In the examples, it is described that the reaction is required to be carried out by heating for about 3 hours while maintaining at 100 ℃.
Documents of the prior art
Patent document
Patent document 1: japanese patent laid-open No. S51-17516
Patent document 2: japanese patent No.3379204
Patent document 3: japanese patent No.2741137
Disclosure of Invention
Problems to be solved by the invention
As described above, in the conventional art, although attempts have been made to produce a polymeric ferric sulfate solution by selecting various iron compounds as iron-based raw materials and reacting them in various reaction forms, there have been problems including generation of more free sulfuric acid and reaction residues and an extended production time for producing a polymeric ferric sulfate solution resistant to practical use.
Although detailed later, it is considered that, among iron-based flocculants, flocculants having a higher total iron concentration have higher characteristics as flocculants. The applicant of the present patent application produced and sold an iron-based inorganic polymeric flocculant, "Polytetsu" (R) having a total iron concentration of about 11.0 to 12.5%, (referred to as "common product"). Since the iron-based inorganic polymeric flocculant has high flocculation ability and dewatering property if the total iron concentration is high, an iron-based inorganic polymeric flocculant having a total iron concentration of 12.5 or more has been produced recently and sold as a "high concentration product".
However, even if a flocculant having a high total iron concentration is produced, the total iron concentration is limited to 12.7% (less than 13%) at the highest, and is also affected by the above-described problem of extension of the production time, and a polymeric ferric sulfate solution of 13.0% or more cannot be produced.
Here, unless expressed as a molar concentration, the concentration in the present invention means% by weight, and [ T-Fe%]Represents the weight concentration of total iron; and [ SO4 2-]Represents the weight concentration of sulfate ions.
Here, the total iron concentration refers to a concentration including not only iron dissolved in the raw material liquid but also iron that is not dissolved in the raw material liquid and is present in the raw material liquid as a solid (powder or the like). Since even the iron-based powder present in the raw material liquid contributes to the production reaction of the polymeric ferric sulfate solution, it is reasonable to include an iron-based component that is not dissolved in the raw material liquid in the concentration of iron.
However, in the polymeric ferric sulfate solution produced by the present invention, the concentration is also expressed as the total iron concentration, but it is natural that all iron is dissolved.
The present invention has been made to solve these problems, and an object thereof is to provide a production method capable of producing a polymeric ferric sulfate solution having a high total iron concentration in a short time as compared with conventional products.
Means for solving the problems
To solve these problems, the present invention is constituted by the following technical means.
(1) A method for producing an iron-based flocculant comprising a polymeric ferric sulfate solution, the method comprising reacting a raw material liquid containing ferrous sulfate and sulfuric acid in a closed vessel under high temperature and high pressure conditions, the raw material liquid satisfying the following conditions:
molar ratio of sulfate ions to total iron (SO)4 2-The ratio of/T-Fe) is more than 1.2; and
when the weight concentration of sulfate ions is less than [ SO ]4 2-]When is represented by [ SO ]4 2-]35% by weight or less.
(2) The method for producing an iron-based flocculant according to (1), further comprising adding nitric acid or a nitrite salt as a catalyst to the closed vessel.
(3) The process for producing an iron-based flocculant according to (1) or (2), wherein the high-temperature high-pressure reaction conditions are a temperature of 100 ℃ or higher and a pressure of 0.3MPa or higher.
(4) An iron-based flocculant, wherein the iron-based flocculant is a high-concentration polymeric ferric sulfate solution with a total iron concentration of 13 to 16 wt%.
ADVANTAGEOUS EFFECTS OF INVENTION
The ultra-high concentration iron-based flocculant of the present invention is characterized in that the concentration thereof is higher than that of a high concentration iron-based flocculant commercially available by the applicant of the present invention, and has high flocculation ability and dewatering performance. In addition, since the ultra-high concentration iron-based flocculant has a lower water content than a general product, the product transportation cost can be reduced.
Further, according to the method for producing an iron-based flocculant of the present invention, the production time of 10 hours or more required in the conventional method can be greatly shortened, and the iron-based flocculant can be produced efficiently.
Drawings
FIG. 1 shows a region where polymeric ferric sulfate can be produced by a high temperature and high pressure reaction.
FIG. 2 is a graph showing the concentration shift after filtering a sample having a precipitate formed.
FIG. 3 is a graph showing the concentration shift after concentrating a sample in which no precipitate is formed.
Detailed Description
Here, before describing the technical features of the production method of the iron-based flocculant according to the present invention, an inorganic flocculant will be described first.
Generally, in sewage sludge treatment, suspended particles and colloidal particles in sludge are flocculated with a flocculant, and dehydration treatment and solid-liquid separation are performed. Suspended particles and colloidal particles in sewage sludge are generally negatively charged on their surfaces and are in a stable state due to the repulsive force of surface charges and hydration. Flocculants are chemicals that adsorb on the surface of these particles to neutralize surface charge and weaken the repulsive forces between the particles to thereby flocculate the particles.
Iron-based flocculants are typical inorganic flocculants, and positively charged iron ions neutralize negative charges on the surface of suspended matter such as suspended particles and colloidal particles to perform flocculation. Therefore, the iron-based flocculant always exhibits flocculation as long as iron ions are present, and since the flocculation ability to suspended matter is improved, a higher iron ion concentration can reduce the amount of flocculant to be added.
In order to stabilize the presence of iron ions in the flocculant, a certain amount of negative ions must be present. In the case of iron-based flocculants, sulfate ions generally play such a role. When the amount of negative ions has an appropriate molar ratio relationship with the amount of iron ions, the iron-based flocculant becomes stable, but in the case of an excessive amount of negative ions, or in the case of an insufficient amount thereof, the iron-based flocculant becomes unstable, and causes deposition as crystals or the like.
Then, in the case of sewage sludge treatment by using such an iron-based flocculant, iron ions adsorb on the surfaces of suspended particles and colloidal particles and are recovered as solid components, but sulfate ions eventually remain in the treated water.
Therefore, since the treated water becomes strongly acidic, in order to discharge the treated water to a river, the treated water needs to be neutralized with a large amount of a neutralizing agent; this is considered to be one of the factors that increase the cost of sewage sludge treatment. That is, as a characteristic required for an iron-based flocculant, the total iron concentration ([ T-Fe ] contained in the flocculant is required]) High, and sulfate ion concentration ([ SO ]4 2-]) Low.
In the product of a polymeric ferric sulfate solution using ferrous sulfate as a raw material, the following chemical reaction is considered to proceed.
m[2FeSO4+(1-n/2)H2SO4+1/2O2+(n-1)H2O]→[Fe2(OH)n(SO4)3-n/2]m
Wherein n is more than 0 and less than or equal to 2, and m is a natural number.
The present invention provides a method for forming a high [ T-Fe ] solution in a short time for an iron-based flocculant composed of the above polymeric ferric sulfate solution, and an iron-based flocculant produced thereby.
In the present invention, when ferrous sulfate (FeSO)4) When used as a solid raw material and the oxidation reaction is carried out under high-temperature and high-pressure conditions, the relationship between the total iron concentration and the sulfate ion concentration of the raw material liquid to be fed is set within a specific range. The invention is realized by leading the molar ratio (SO) of sulfate ions to total iron4 2-/T-Fe) is a specific value or more, and the sulfate ion concentration [ SO ]4 2-]Below a certain value, an extremely remarkable effect is obtained that the reaction can be completed in a short time that cannot be estimated by the conventional technique, and thisIn addition, the total iron concentration ([ T-Fe ] which could not be produced by the conventional technique can be produced]) Ultra high polymeric ferric sulfate solution.
More specifically, the present invention is characterized in that a raw material liquid containing ferrous sulfate and sulfuric acid is reacted under high-temperature and high-pressure conditions, and the raw material liquid satisfies the following conditions.
Molar ratio of sulfate ions to total iron (SO)4 2-The value of/T-Fe) is 1.2 or more.
When the weight concentration of sulfate ions is less than [ SO ]4 2-]When is represented by [ SO ]4 2-]35% by weight or less.
The present inventors have newly found that when the total iron concentration of ferrous sulfate and the concentration of sulfate ion have such a relationship, an ultra-high concentration polymeric ferric sulfate solution can be obtained in a short time without generating a precipitate.
(high temperature high pressure reaction)
The method described in patent document 1 is a conventional production method performed by the present inventors. In this method, it is conceivable that the reaction is carried out under three phases of a solid phase, a liquid phase and a gas phase in association with each other at ordinary temperature and pressure. This is because NO is perceived as being present during the reactionxThe resulting tan gas, and NOxThe odor of (2).
However, in the process of the present invention, NO is perceived even when the autoclave is opened after the reaction is completedxThe odor of (2). Therefore, in the high-temperature high-pressure reaction of the present invention, it is presumed that a reaction involving a solid phase and a liquid phase is carried out, in which FeSO as a solid raw material4·7H2O is dissolved in the sulfuric acid liquid and oxidation reaction is performed.
Thus, it is conceivable that FeSO as a solid raw material is more easily carried out due to the reaction under high-temperature conditions4·7H2Dissolving O; and due to the reaction under high pressure conditions, partial oxygen partial pressure increases and the amount of dissolved oxygen in the liquid phase increases, whereby the dissolved oxygen directly contributes to nitrite ion NO2-And Fe2+And greatly promotes the oxidation reaction of iron ions.
(reaction temperature and reaction pressure)
The temperature in the container needs to be adjusted in the range of 100 to 150 ℃.
If the reaction temperature is lower than 100 ℃, the oxidation reaction of ferrous sulfate does not proceed sufficiently. If higher than 150 ℃, a residual yellow precipitate is identified and X-ray analysis indicates that the precipitate is Fe (OH) SO4。
Although specific experimental data are omitted, the present inventors confirmed that the higher the reaction pressure, the more efficient the reaction proceeds. This fact can be said to be natural in consideration of the reaction mechanism of the above-mentioned high-temperature high-pressure reaction.
Therefore, the reaction pressure in the present invention may be set in consideration of actual conditions such as product cost, and may be 0.3MPa or more.
(catalyst)
In order to promote the reaction to form the above polymeric ferric sulfate solution, a catalyst is preferably used. Preferred catalysts to promote the reaction include nitric acid and nitrite; nitrites include sodium, potassium, etc. salts of nitrous acid. From the viewpoint of the function of promoting the reaction and the cost, nitric acid is preferable.
[ experiment 1]
As high-temperature high-pressure reaction conditions, the inventors of the present invention set a reaction temperature of 110 ℃, a reaction pressure of 0.30MPa, and a reaction time of 10 minutes, and prepared raw material liquids containing ferrous sulfate and sulfuric acid at various concentrations. Nitric acid was added thereto as a catalyst and a high-temperature high-pressure reaction was performed. Then, after the reaction time had elapsed, it was checked whether or not a precipitate was generated.
[ experiment 2]
Further, as high-temperature high-pressure reaction conditions, the reaction temperature was set to 120 ℃, the reaction pressure was 10.00MPa, and the reaction time was 10 minutes, and raw material liquids containing ferrous sulfate and sulfuric acid at various concentrations were prepared. Nitric acid was added thereto as a catalyst and a high-temperature high-pressure reaction was performed. Then, after the reaction time had elapsed, it was checked whether or not a precipitate was generated.
The results of the experiment on whether or not the precipitate was formed are summarized in tables 1 and 2.
In the case of experiment 1 in which the experiment was carried out under the conditions of the reaction temperature of 110 ℃ and the reaction pressure of 0.30MPa, and in the case of experiment 2 in which the experiment was carried out under the conditions of the reaction temperature of 120 ℃ and the reaction pressure of 10.00MPa, it was found that exactly the same results were given on the formation of the precipitate. That is, the results in tables 1 and 2 are the same as those in experiments 1 and 2.
Total iron concentration [ T-Fe ] shown in Table 1]And total sulfuric acid concentration [ SO ]4 2-]The case of (a) forms a polymeric ferric sulfate solution without forming a precipitate, and is an example of the present invention; and the case shown in table 2 confirmed the formation of precipitates and is a comparative example of the present invention.
[ Table 1]
Added concentration without generating precipitate
[ Table 2]
The added concentration of the formed precipitate
(specific region)
These results are shown in summary in fig. 1. The area occupied by the o marks is the area where the polymeric ferric sulfate solution formed without the formation of precipitates. This area is an area designated by the present invention, and is hereinafter referred to as "specific area". T-Fe indicated by white O marks contained in specific regions]And [ SO4 2-]Is the raw material composition of the examples of the present invention. By reacting the compositions each under high temperature and high pressure conditions, a reddish brown solution of polymeric ferric sulfate can be obtained.
On the other hand, the case of carrying out the reaction at high temperature and high pressure by using the starting material composition represented by a mark a outside the specific region corresponds to a comparative example of the present invention. In any case where these compositions were used, the formation of a precipitate was confirmed; and in the molar ratio of sulfate ions to total ironRatio (SO)4 2-T-Fe) below 1.2, the precipitate was determined to be chalcanthite.
The present inventors specified a specific region from the following two conditions.
First, the upper limit of the region may be set SO that the sulfate ion concentration [ SO ] by weight4 2-]35% by weight or less.
Then, the lower limit of the area may be specified by an oblique straight line upward to the right. The oblique lines are each a straight line representing the molar ratio (SO) of sulfate ions to total iron4 2-T-Fe) is 1.2 or more, and the ordinate and abscissa in the figure represent the weight concentration of sulfate ions and the weight concentration of total iron, respectively.
The above [ T-Fe ] specified in the present invention]And [ SO4 2-]The specific region of the composition of the raw material (b) means a region in which the formation of the polymeric ferric sulfate solution can be stably performed under high temperature and high pressure conditions.
The technical significance of a specific region can be confirmed by the following additional experiments 1 and 2.
(additional experiment 1)
[T-Fe]And [ SO4 2-]The samples (hereinafter, labeled (14.0:28.0)) at concentrations of 14% and 28%, respectively, and the sample (15.0:30.0) in FIG. 1 produced precipitates. Filtering the sample; and the concentration of the solution after removing the precipitate was measured, and the compositions of the solutions were (12.8:27.2) and (14.5:29.8), respectively.
These are numerical values within the area designated by the present invention. That is, even when the sample is one in which precipitates are generated, it is confirmed that the corresponding solution portion is a composition contained in a specific region of the total iron concentration and the total sulfate ion concentration specified in the present invention. Fig. 2 shows the contents.
(additional experiment 2)
According to FIG. 1, both samples (15.0:32.0) and (15.0:34.0) were samples in which no precipitate was formed. The samples were maintained for one month in three environments (i) 50 ℃ in a desiccator, (ii) about 20 ℃ in the laboratory, and (iii) 10 ℃ in an incubator; thereafter, the sample was observed for change. As a result, precipitates were observed only in (i) a sample at 50 ℃ in a desiccator (15.0: 34.0).
The reason is considered to be due to the following.
For samples (15.0:32.0) and (15.0:34.0) kept in a desiccator at 50 ℃ for one month, [ T-Fe ] was measured again]And [ SO4 2-]And each measured value was (16.0:34.0) and (16.0: 36.0). Fig. 3 shows the contents.
Although the sample held in the desiccator was concentrated by evaporation of water, even if the sample was already concentrated, it was [ T-Fe ]]And [ SO4 2-]The concentration relationship of (a) in the sample in the region specified in the present invention, no precipitate was detected. However, as a result of the concentration, the sample whose concentration relationship deviates from the above-mentioned region due to the concentration generates precipitates.
Therefore, only the sample (15.0:34.0) under the condition (i) produced a precipitate.
(reaction time)
The production method using the conventional technique described in patent document 1 is a method of oxidizing ferrous sulfate at normal temperature and pressure; and even if a catalyst, an oxidizing agent, etc. are designed, this method can only obtain a solution having a total iron concentration ([ T-Fe ]) of up to about 12.5%, and is a method in which the reaction time is as long as 16 hours or more.
By adopting the high-temperature and high-pressure method, the invention successfully and greatly shortens the reaction time.
In the example shown in fig. 1, the reaction was completed within 30 minutes in all samples from a high concentration solution with a total iron concentration of 12.5% to an ultra-high concentration solution with a total iron concentration of up to 16%. The reaction time is of course dependent on the total iron concentration; and the reaction was completed in 7.5 minutes in a solution with a total iron concentration of 12.5%, and in 30 minutes even in a solution with a total iron concentration of 16%. Here, the completion of the reaction is judged by measuring the concentration of ferrous iron in the sample solution.
The fact that the reaction can be carried out in such a short time is an extremely remarkable effect which cannot be expected in the conventional art.
(ultra high concentration solution)
To confirm the effect attributed to the fact that the polymeric ferric sulfate solution was ultra-high in concentration, flocculation tests were performed on the following samples a and B. Sample a is a sample having the same total iron concentration as a sample produced by taking more than 16 hours in the conventional technique. On the other hand, sample B is a sample produced by the present invention in which the total iron concentration is ultrahigh.
[ Table 3]
| Sample (I) | [T-Fe] | [SO4 2-] | [SO4 2-]/[T-Fe] |
| Sample A | 12.7 | 32.5 | 1.49 |
| Sample B | 14.7 | 31.5 | 1.25 |
Separately adding sample a and sample B to a liquid to be treated of coloring water of a propylene pigment as a simulant liquid, the total iron addition amount of sample a and sample B becomes the same by reducing the addition amount of sample B, that is, by making the flocculation ability by iron ions the same; and the flocculation abilities of the two were compared.
The conditions of the flocculation test are shown in table 4.
[ Table 4]
| Sample (I) | Addition amount (μ L) | Total iron content (g) | pH (after addition) | NaOH addition amount (μ L) |
| Sample A | 380 | 6.91×10-2 | 2.82 | 340 |
| Sample B | 258 | 6.91×10-2 | 3.73 | 180 |
| Increase or decrease | The reduction is 32 percent | Are identical to each other | The reduction is 47 percent |
Since sample B is in an ultra-high concentration, the amount of sample B added can be reduced by as much as 32% compared to sample a, in the case where the flocculation ability of sample B is made the same as that of sample a. Then, since in the case of sample B, [ SO ]4 2-]As shown in table 1, is low, and therefore, the pH of the liquid to be treated after the flocculation treatment can be suppressed from decreasing; therefore, the amount of caustic soda added for neutralization can be reduced by 47% as compared with the case of using sample a.
Then, the condition after the floc formation was observed; the sample B, which is an ultra-high concentration, has a higher floc formation ability and also has a higher floc settling speed. Although the iron amount of sample B was made the same as that of sample a, sample B had a higher flocculation ability.
The reason for this is believed to be because sample B polymerizes more and favors the cross-linking and adsorption of floes. This is also confirmed by the fact that the ultra-high concentration sample of sample B has a higher liquid viscosity than sample a.
Industrial applicability
The present invention relates to a flocculant used for wastewater treatment such as sewage, and since a flocculant exhibiting high flocculation performance can be produced in a short time, the flocculant can be widely used in the field of wastewater treatment.
Claims (4)
1. A production method of iron-based flocculant comprises the steps of polymerizing ferric sulfate solution,
the method comprises reacting a raw material solution containing ferrous sulfate and sulfuric acid in a closed container under high temperature and high pressure conditions,
the raw material liquid meets the following conditions:
molar ratio of sulfate ions to total iron (SO)4 2-The ratio of/T-Fe) is more than 1.2; and
when the weight concentration of sulfate ions is less than [ SO ]4 2-]When is represented by [ SO ]4 2-]35% by weight or less.
2. The method for producing a iron-based flocculant according to claim 1, further comprising adding nitric acid or a nitrite salt as a catalyst to the closed vessel.
3. The method for producing an iron-based flocculant according to claim 1 or 2, wherein the reaction conditions of high temperature and high pressure are a temperature of 100 ℃ or more and a pressure of 0.3MPa or more.
4. A ferric flocculant, wherein the ferric flocculant is a high concentration polymeric ferric sulfate solution having a total ferric concentration of 13 to 16 wt%.
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| Application Number | Priority Date | Filing Date | Title |
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| JP2019-179191 | 2019-09-30 | ||
| JP2019179191A JP2021053580A (en) | 2019-09-30 | 2019-09-30 | High-concentration iron-based flocculant, and method for producing same |
| PCT/JP2020/036337 WO2021065732A1 (en) | 2019-09-30 | 2020-09-25 | High-concentration iron-based flocculant, and method for producing same |
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| KR (1) | KR20220069092A (en) |
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| JP3379204B2 (en) | 1994-04-06 | 2003-02-24 | 王子製紙株式会社 | Method for producing iron-based inorganic coagulant |
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- 2020-09-25 KR KR1020227014081A patent/KR20220069092A/en unknown
- 2020-09-25 WO PCT/JP2020/036337 patent/WO2021065732A1/en active Application Filing
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| CN1109027A (en) * | 1994-11-30 | 1995-09-27 | 华南理工大学 | Production of iron polysulfate |
| AU3043499A (en) * | 1998-03-23 | 1999-10-18 | Imperial College Of Science, Technology And Medicine | Preparation and uses of mixed metal coagulants |
| JP2000185921A (en) * | 1998-12-22 | 2000-07-04 | Taki Chem Co Ltd | Production of ferric sulfate solution |
| JP2000191328A (en) * | 1998-12-25 | 2000-07-11 | Taki Chem Co Ltd | Production of ferric sulfate solution |
| CN101786708A (en) * | 2010-03-01 | 2010-07-28 | 株式会社东洋贸易 | Iron-based flocculating agent and preparation method thereof |
| CN104071853A (en) * | 2014-07-17 | 2014-10-01 | 广西平果锋华科技有限公司 | Method utilizing waste sulfuric acid and ferrous sulfate to produce polymeric ferric sulfate through oxygen pressurizing |
| CN104355336A (en) * | 2014-10-17 | 2015-02-18 | 陕西华陆化工环保有限公司 | Method of utilizing ferrous sulfate waste residue to prepare polymeric ferric sulfate |
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| JP2018008837A (en) * | 2016-07-12 | 2018-01-18 | 日鉄鉱業株式会社 | Manufacturing method of ferric polysulfate, and solidification inhibitor for sludge incinerator |
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| Publication number | Publication date |
|---|---|
| KR20220069092A (en) | 2022-05-26 |
| TW202122146A (en) | 2021-06-16 |
| WO2021065732A1 (en) | 2021-04-08 |
| JP2021053580A (en) | 2021-04-08 |
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