CN110256302A - A kind of method of complexometric extraction production H acid - Google Patents
A kind of method of complexometric extraction production H acid Download PDFInfo
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- CN110256302A CN110256302A CN201910570207.5A CN201910570207A CN110256302A CN 110256302 A CN110256302 A CN 110256302A CN 201910570207 A CN201910570207 A CN 201910570207A CN 110256302 A CN110256302 A CN 110256302A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
- C07C303/22—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof from sulfonic acids, by reactions not involving the formation of sulfo or halosulfonyl groups; from sulfonic halides by reactions not involving the formation of halosulfonyl groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/42—Separation; Purification; Stabilisation; Use of additives
- C07C303/44—Separation; Purification
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Abstract
The invention discloses a kind of method of complexometric extraction production H acid, includes the following steps: the nitrobased NPK reaction solution cooling 1) by refined naphthalene after sulfonation, nitrification, denitration, nitrobased NPK solid is precipitated；2) after adding water to be beaten nitrobased NPK solid, mother liquor is melted with H soda acid and is neutralized, by the sulfur dioxide removal of generation, collect；3) filtrate is extracted using complexing extractant, sulfuric acid content is 30%-50% in residual filtrate extracted, and extract liquor is after washing, lye back extraction, and sulfuric acid content is 15-25% in water lotion；4) by step 2) and 3) obtained in nitrobased NPK salting liquid, be acidified after catalytic hydrogenation or after iron powder reducing, filter to obtain amino T acid solution；5) alkali is added into amino T acid solution and methanol carries out alkali fusion, the sulfur dioxide collected in step 2) is acidified alkali fusion liquid, obtained solid is filtered, water is added to be beaten, it is acidified, filtered with the water lotion in step 3) again, filter cake obtains product through washing, filtering, drying.
Description
Technical field
The invention belongs to the preparation technical fields of H acid, and in particular to a kind of method of complexometric extraction production H acid.
Background technique
Disclosing the information of the background technology part, it is only intended to increase understanding of the overall background of the invention, without certainty
It is considered as recognizing or implying in any form that information composition has become existing skill well known to persons skilled in the art
Art.
H acid (1- amino-8-naphthol -3,6- disulfonate sodium) is the important intermediate for producing reactive dye.Currently, H is sour
Production using refined naphthalene as raw material, the processes such as sulfonated, nitrification, denitration, neutralization, reduction and sodium chloride are saltoutd first prepare amino
T acid, amino T acid again through the processes such as alkali fusion, acidification production H acid, however, production H acid during generation mother liquor belong to high concentration,
Highly acidity, high salinity, high chroma, highly toxic " five is high " organic wastewater, COD (Chemical Oxygen
Demand-COD it) is up to 8-10 ten thousand, salinity is up to 10-20%, and coloration is up to 4000-6000 times, using traditional biochemistry and object
Change method is difficult to effectively to these " five is high " treatment of Organic Wastewater；And use the methods of unconventional extraction, pyrolysis, absorption place
Reason only pre-processes cost and is as high as thousands of members, but also can not accomplish thorough, effective processing.Currently, the country there is no enterprise's energy
" five the is high " organic wastewater generated in processing H acid production is enough effectively treated, and makes up to discharge standard.Although there are also useless
Water can be by MVR concentration production ammonium sulfate, the salt-mixture of sodium chloride, but this salt-mixture is because containing large amount of organic, and is difficult to
Purification, can only be used as fixed-end forces.
It is replaced in traditional ammonium hydroxide with potassium hydroxide and denitration liquid produces nitrobased NPK, and replace hydroxide with potassium hydroxide
Soda is molten, generates potassium sulfate mother liquid through MVR condensing crystallizing, high-temperature calcination and produces potassium sulfate, can solve the ring of puzzlement enterprise
Guarantor's problem, while the yield of product is also improved, but the shortcomings that inventor's this method of discovery is that potassium hydroxide dosage is too big, often
11 tons of potassium hydroxide or more of ton H acid product consumption 48% are unfavorable for controlling the production cost of product.And with alkali fusion mother liquor come in
And denitration liquid, reduce the dosage of alkali, it is particularly possible to further neutralize denitration liquid instead of ammonium hydroxide with magnesia unslacked, lime etc., reduce
Waste water yield, greatly reduces cost.But production process has magnesium sulfate or calcium sulfate generates, and abraum salt amount is relatively large, and
It needs to these abraum salt treatment and uses.
Summary of the invention
For above-mentioned the technical problems existing in the prior art, the object of the present invention is to provide a kind of complexometric extractions to produce H
The method of acid.
In order to solve the above technical problems, the technical solution of the present invention is as follows:
A kind of method of complexometric extraction production H acid, includes the following steps:
1) the nitrobased NPK reaction solution cooling by refined naphthalene after sulfonation, nitrification, denitration, is precipitated nitrobased NPK solid, is precipitated
Nitrobased NPK solid and filtrate mass ratio be 1:0.8-1.2；
2) after adding water to be beaten nitrobased NPK solid, mother liquor is melted with H soda acid and is neutralized, the sulfur dioxide removal of generation obtains
Nitrobased NPK salting liquid；
3) filtrate after filtering nitrobased NPK is extracted using complexing extractant, sulfuric acid content in residual filtrate extracted
For 30%-50% (mass percent), extract liquor obtains nitrobased NPK salting liquid, sulfuric acid in water lotion after washing, lye back extraction
Content is 15-25% (mass percent)；
4) by step 2) and 3) obtained in nitrobased NPK salting liquid be separately added into catalyst, catalytic hydrogenation or iron powder reducing,
Solution after reduction is acidified, filters to obtain amino T acid, and acidification is residual filtrate extracted described in step 3) with acid；
5) it will be added alkali in amino T acid and methanol carries out alkali fusion, after alkali fusion terminal, sulfur dioxide that will collect in step 2)
Alkali fusion liquid is acidified, after obtained solid is filtered, water is added to be beaten, then is acidified, filtered with the water lotion in step 3),
Filter cake obtains product through washing, filtering, drying.
Strip liquor after the nitrobased NPK solid and extraction nitrobased NPK that filter out, with by adding hydrogen or iron powder reducing to produce
Amino T acid, the acidification of amino T acid can replace sulfuric acid with the residual filtrate after complexometric extraction nitrobased NPK with acid.Extract nitrobased NPK
Extract liquor afterwards, is first washed with water, and the sulfate moieties for extracting extract liquor are washed into water.Control leaching requirement, the sulfuric acid in wash water
Content is up to 20% or so.This part dilute sulfuric acid is colorless and transparent, organic matter very little, can be used for the acidification acid of H acid, without influencing
The product quality of H acid.
This method, which can not only be reduced, neutralizes denitration liquid alkaline alkali, amino T acid acidification sulfuric acid dosage, H acid acidification sulfuric acid use
Amount, and a kind of alkali is only used in entire production process, only a kind of salt, the concentrated crystallization recycling sulfate of mother liquor are dense in mother liquor
Contract out for produce in, production process without exhaust gas, waste water and waste residue generate.Production technology is environmentally protective, overall cost compared with
25% or more traditional handicraft decline.
In some embodiments, in step 1), nitrobased NPK reaction solution is cooled to -5 DEG C -10 DEG C.
In some embodiments, in step 2), the content that the H soda acid melts mesh liquid sulfite sodium is 35%-45%.
In some embodiments, in step 2), after adding water to be beaten nitrobased NPK solid, mother liquor is melted with H soda acid and is neutralized, until
The pH value of nitrobased NPK slurries is 4-6.
In some embodiments, in step 3), the complexing extractant is N235With the mixing of solvent naphtha and alkyl ether benzene
Object, N235Mass percent in complexing extractant is 20%-50%, can for 20%, 25%, 30%, 35%, 40%,
45% or 50%.
Further, the solvent naphtha is 200# solvent naphtha or kerosene.
Further, the benzene alkyl ether compound includes methyl phenyl ethers anisole, phenetole, this butyl ether, benzene octyl ether etc..
In some embodiments, in step 3), sulfuric acid content is 35%-45% (matter in the residual filtrate extracted
Measure percentage).
In filtrate after extracting nitrobased NPK, the content of nitrobased NPK can drop to 0.5% hereinafter, sulfuric acid content is 40% left
The right side can be used for the acidification of amino T acid.
In some embodiments, in step 4), the catalyst is Raney nickel, and the temperature of catalytic hydrogenation is 80-120
℃。
In some embodiments, in step 5), the alkali is sodium hydroxide or potassium hydroxide.
Further, the mass fraction of the alkali is 40-50%.
Further, in step 5), the temperature of alkali fusion is 160-195 DEG C, and the time of alkali fusion is 1-3 hours.
The invention has the benefit that
In the present invention by by denitration object decrease temperature crystalline, filter out nitrobased NPK, the neutralization of nitrobased NPK alkali fusion mother liquor is gone forward side by side
One step also original production amino T acid.Mother liquor after filtering nitrobased NPK, uses N235Filtrate is extracted with solvent naphtha, then uses lye
Back extraction, strip liquor is through also original production amino T acid.Extract nitrobased NPK after filtrate, the content of nitrobased NPK can drop to 0.5% with
Under, sulfuric acid content 40% or so can be used for the acidification acid of amino T acid.The extract liquor of nitrobased NPK is extracted, first uses water before back extraction
The sulfuric acid scrubbing for extracting into extract liquor is come out, leaching requirement is adjusted, the sulfuric acid concentration of wash-off is colorless and transparent available up to 20% or so
Sour without influencing quality in the acidification of H acid, by this circulation, not only save neutralization denitration liquid uses alkali and amino T
Acid, H acid acidification sulfuric acid only have a kind of salt, the concentrated knot of mother liquor moreover, only using a kind of alkali in entire production process in mother liquor
Crystalline substance recycling sulfate, the water jacket being concentrated out are used in production, and production process is generated without exhaust gas, waste water, waste residue.Production technology green
Environmental protection efficiently solves H acid environmental protection of enterprise problem, and comprehensive production cost is compared with 25% or more traditional handicraft decline.
Specific embodiment
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.Unless another
It indicates, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singular
Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or their combination.
Embodiment 1
A method of H acid is produced by complexometric extraction, is included the following steps；
1) 600 parts of the nitrobased NPK reaction solution after traditional handicraft sulfonation, nitrification, denitration of refined naphthalene (parts by weight) is taken, is stirred
5 DEG C are cooled to, filtering obtains 280 parts of nitrobased NPK solid, 320 parts of filtrate.
2) 280 parts plus water mashing of nitrobased NPK solid, melts mother liquor (sodium sulfite content 39.82%) with 360 parts of H soda acids
It neutralizes, generates sulfur dioxide (sulfur dioxide generated during removing neutralization reaction at 80-100 DEG C), be used for H soda acid melt
Neutralization, up to nitrobased NPK sodium solution after scrubbing CO_2.
3) by filtrate in step 1) with complexing extractant (N235: 200# solvent naphtha: methyl phenyl ethers anisole=3:4:3, weight ratio) extraction
It takes, water sulfuric acid is 41.3% after remaining extraction after nitrobased NPK extraction, and extract liquor first uses 80 parts of water washings, obtains sulfuric acid content
100 parts of 20% or so wash water, then extract liquor is stripped with 15% sodium hydroxide solution, 287 parts of (strip liquors of strip liquor
As nitrobased NPK sodium solution).
4) 15 parts of Raney nickels are added in the nitrobased NPK sodium solution for obtaining step (2), in 120 DEG C plus hydrogen to terminal, filter
Catalyst is removed, with the dilute sulfuric acid acidification generated after extraction in (3), is obtained by filtration 298 parts of acid of amino T, the content of amino T acid
38.5%.
5) 5 parts of Raney nickels are added in the strip liquor of step (3), add hydrogen to terminal at 120 DEG C.Catalyst is filtered off, then is passed through
It is acidified, is obtained by filtration 89 parts of acid of amino T, content 32.8%.
6) 195 part of 48% sodium hydroxide is added in 290 parts of amino T acid and 60 parts of methanol carries out alkali fusion, in 185-188 DEG C of temperature
Lower alkali fusion 1.5 hours are spent, blowing is diluted with water, and with the SO 2 acidifying of generation in (2), the solid was filtered, and solid is beaten with water
Slurry generates dilute sulfuric acid acidification, filtering with the wash water of step 3), and filter cake uses 1 times of washing again, refilters, dries and obtain product 108
Part, content 85.78%, purity 99.15%.
Embodiment 2
A kind of method of complexing abstraction production H acid, includes the following steps:
1) 800 parts of the nitrobased NPK reaction solution after traditional handicraft sulfonation, nitrification, denitration of refined naphthalene (parts by weight) is taken, is stirred
0 DEG C is cooled to, is obtained by filtration 409 parts of nitrobased NPK solid, 391 parts of filtrate.
2) it is beaten with water for 409 parts of nitrobased NPK, melts mother liquor (potassium sulfite content 42.36%) with 660 parts of H soda acids and neutralize, produce
Raw sulfur dioxide, has used the neutralization of H soda acid melt, up to nitrobased NPK potassium solution after scrubbing CO_2.
3) by the filtrate after filtering nitrobased NPK solid in step 1) with complexing extractant (N235: 200# solvent naphtha: phenetole
=2:4:4, weight ratio) extraction, the dilute sulfuric acid that remaining aqueous solution is 39.8% after nitrobased NPK extraction, 100 parts of water of extract liquor
It washes, obtains 128 parts of dilute sulfuric acid that content is 19.3%, then be stripped with 20% potassium hydroxide to extract liquor, strip liquor 362
Part, it is nitrobased NPK potassium solution.
4) step 2) is obtained to nitrobased NPK potassium solution to merge in, 20 parts of Raney nickels is added, at 80 DEG C, add hydrogen to eventually
Point filters off catalyst, is neutralized with generation dilute sulfuric acid (content 39.8%) after extraction in (3), is obtained by filtration 370 parts of acid of amino T, ammonia
The content 41.3% of base T acid.
5) 6 parts of Raney nickels are added in strip liquor in example 3, add hydrogen to terminal at 120 DEG C.Catalyst is filtered off, then through acid
Change, be obtained by filtration 108 parts of acid of amino T, content 34.6%.
6) 360 part of 48% potassium hydroxide is added in 350 parts of amino T acid and 90 parts of methanol carries out alkali fusion, at 165 DEG C -168 DEG C
Alkali fusion two hours, blowing was diluted with water, and is acidified, is filtered after acidification, solid water with the sulfur dioxide collected in step 1)
Mashing is acidified with the dilute sulfuric acid (content 19.3%) that washing extract liquor generates in step 3), is refiltered, filter cake uses 1 times of washing again
It washs, filtering drying, obtains 180 parts of H acid monopotassium salt, content 81.6%, purity 99.46%.
Embodiment 3
A method of H acid is produced by complexometric extraction, is included the following steps；
1) 600 parts of the nitrobased NPK reaction solution after traditional handicraft sulfonation, nitrification, denitration of refined naphthalene (parts by weight) is taken, is stirred
- 5 DEG C are cooled to, filtering obtains 300 parts of nitrobased NPK solid, 300 parts of filtrate.
2) 300 parts of water mashing are added in nitrobased NPK solid, melt mother liquor (sodium sulfite content 39.82%) with 360 parts of H soda acids
It neutralizes, generates sulfur dioxide, for the neutralization of H soda acid melt, up to nitrobased NPK sodium solution after scrubbing CO_2.
3) by filtrate in step 1) with complexing extractant (N235: 200# solvent naphtha: butoxy benzene=2:5:3, weight ratio) extraction
It takes, the dilute sulfuric acid that the aqueous solution after nitrobased NPK extraction is 38%, extract liquor first uses 90 parts of water washings, obtains sulfuric acid content 18%
100 parts of wash water, then extract liquor is stripped with 15% sodium hydroxide solution, (strip liquor is nitro T to 290 parts of strip liquor
Acid sodium solution).
4) the nitrobased NPK sodium solution for obtaining step (2) merges, and 50 parts of Raney nickels are added, in 100 DEG C plus hydrogen to eventually
Point filters off catalyst, with the dilute sulfuric acid acidification generated after extraction in (3), is obtained by filtration 290 parts of acid of amino T, amino T acid contains
Amount 40.5%.
5) 4 parts of Raney nickels are added in the strip liquor in step 3, in 100-120 DEG C plus hydrogen to terminal, filter off catalyst,
It is acidified again, 86 parts of amino T acid, content 35.3% is obtained by filtration.
6) 197 part of 48% sodium hydroxide is added in 290 parts of amino T acid and 61 parts of methanol carries out alkali fusion, in 185-188 DEG C of temperature
Lower alkali fusion 1.5 hours are spent, blowing is diluted with water, and with the SO 2 acidifying of collection in (2), the solid was filtered, and solid is beaten with water
Slurry, with the acidification of the wash water dilute sulfuric acid of step 3), filtering, filter cake uses 1 times of washing again, refilters, dries and obtain 109 parts of product, contains
Amount 85.57%, purity 99.25%.
The foregoing is merely preferred embodiment of the present application, are not intended to limit this application, for the skill of this field
For art personnel, various changes and changes are possible in this application.Within the spirit and principles of this application, made any to repair
Change, equivalent replacement, improvement etc., should be included within the scope of protection of this application.
Claims (10)
1. a kind of method of complexometric extraction production H acid, characterized by the following steps:
1) the nitrobased NPK reaction solution cooling by refined naphthalene after sulfonation, nitrification, denitration, is precipitated nitrobased NPK solid, makes precipitation
Nitrobased NPK solid and the mass ratio of filtrate are 1:0.8-1.2；
2) after adding water to be beaten nitrobased NPK solid, mother liquor is melted with H soda acid and is neutralized, by the sulfur dioxide removal of generation, obtains nitro
T acid salt solution；
3) filtrate is extracted using complexing extractant, sulfuric acid content is 30%-50%, quality percentage in residual filtrate extracted
Number, extract liquor obtain nitrobased NPK salting liquid after washing, lye back extraction, and sulfuric acid content is 15-25%, quality percentage in water lotion
Number；
4) the nitrobased NPK salting liquid that step 2) obtains is separately added into catalyst, catalytic hydrogenation or iron powder reducing, it is molten after reduction
Liquid is acidified, filters to obtain amino T acid solution, and acidification is residual filtrate extracted described in step 3) with acid；
5) alkali is added into amino T acid and methanol carries out alkali fusion, acid is carried out to alkali fusion liquid with the sulfur dioxide generated in step 2)
Change, by obtained solid after filtering, water is added to be beaten, then be acidified, filtered with the water lotion in step 3), filter cake is through washing, mistake
Filter, drying, obtain product.
2. the method for complexometric extraction production H acid according to claim 1, it is characterised in that: in step 1), by nitrobased NPK
Reaction solution is cooled to -5 DEG C~10 DEG C.
3. the method for complexometric extraction production H acid according to claim 1, it is characterised in that: in step 2), the H soda acid
The content of molten mother liquor sulfite sodium is 35%-45%.
4. the method for complexometric extraction production H acid according to claim 1, it is characterised in that: in step 2), by nitrobased NPK
After solid adds water to be beaten, melting mother liquor to be neutralized to the pH value of nitrobased NPK slurries with H soda acid is 4-6.
5. the method for complexometric extraction production H acid according to claim 1, it is characterised in that: in step 3), the complexing extraction
Taking agent is N235The mixture of solvent naphtha and alkyl ether benzene, N235Mass percent in complexing extractant is 20%-50%.
6. the method for complexometric extraction production H acid according to claim 5, it is characterised in that: the solvent naphtha is that 200# is molten
Agent oil or kerosene.Alkyl ether benzene is methyl phenyl ethers anisole, phenetole, butoxy benzene, benzene octyl ether etc..
7. the method for complexometric extraction production H acid according to claim 1, it is characterised in that: in step 3), after the extraction
Residual filtrate in sulfuric acid content be 35%-45%, mass percent.
8. the method for complexometric extraction production H acid according to claim 1, it is characterised in that: in step 4), the catalyst
For Raney nickel, the temperature of catalytic hydrogenation is 80-120 DEG C.
9. the method for complexometric extraction production H acid according to claim 1, it is characterised in that: in step 5), the alkali is hydrogen
Sodium oxide molybdena or potassium hydroxide；
Further, the mass fraction of the alkali is 40-50%.
10. the method for complexometric extraction production H acid according to claim 1, it is characterised in that: in step 5), the temperature of alkali fusion
Degree is 160-195 DEG C, and the time of alkali fusion is 1-3 hours.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910570207.5A CN110256302B (en) | 2019-06-27 | 2019-06-27 | Method for producing H acid by complex extraction |
| PCT/CN2019/105277 WO2020052577A1 (en) | 2018-09-13 | 2019-09-11 | Process for producing h acid by recycling alkali fusion mother liquor |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910570207.5A CN110256302B (en) | 2019-06-27 | 2019-06-27 | Method for producing H acid by complex extraction |
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| CN110256302B CN110256302B (en) | 2020-07-17 |
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| WO (1) | WO2020052577A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118439978A (en) * | 2024-06-28 | 2024-08-06 | 山东创蓝垚石环保技术有限公司 | Process for producing H acid by recycling T acid mother liquor |
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| US4324742A (en) * | 1978-06-15 | 1982-04-13 | Sugai Chemical Industry Co., Ltd. | Process for separation of naphthalenedisulfonic acids |
| JPS5951253A (en) * | 1982-09-14 | 1984-03-24 | Sugai Kagaku Kogyo Kk | Novel preparation of 1,8-dinitronaphthalene-3,6-disulfonic acid, and preparation of high-purity 1-amino-8- hydroxynaphthalene-3,6-disulfonic acid using its method |
| CN104592063A (en) * | 2014-12-24 | 2015-05-06 | 青岛奥盖克化工股份有限公司 | Environment-friendly production process of H acid |
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| DE3020441A1 (en) * | 1980-05-29 | 1981-12-03 | Bayer Ag, 5090 Leverkusen | METHOD FOR PRODUCING NITRONAPHTHALINE SULPHONIC ACIDS |
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2019
- 2019-06-27 CN CN201910570207.5A patent/CN110256302B/en active Active
- 2019-09-11 WO PCT/CN2019/105277 patent/WO2020052577A1/en active Application Filing
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| JPS5951253A (en) * | 1982-09-14 | 1984-03-24 | Sugai Kagaku Kogyo Kk | Novel preparation of 1,8-dinitronaphthalene-3,6-disulfonic acid, and preparation of high-purity 1-amino-8- hydroxynaphthalene-3,6-disulfonic acid using its method |
| CN104592063A (en) * | 2014-12-24 | 2015-05-06 | 青岛奥盖克化工股份有限公司 | Environment-friendly production process of H acid |
| CN109096155A (en) * | 2018-07-09 | 2018-12-28 | 山东垚石化工科技有限公司 | A kind of technique that H acid is produced by alkali fusion mother liquid recycling |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118439978A (en) * | 2024-06-28 | 2024-08-06 | 山东创蓝垚石环保技术有限公司 | Process for producing H acid by recycling T acid mother liquor |
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| WO2020052577A1 (en) | 2020-03-19 |
| CN110256302B (en) | 2020-07-17 |
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