CN102643191B - Heavy phase lactic acid processing technology - Google Patents

Heavy phase lactic acid processing technology Download PDF

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Publication number
CN102643191B
CN102643191B CN201210085311.3A CN201210085311A CN102643191B CN 102643191 B CN102643191 B CN 102643191B CN 201210085311 A CN201210085311 A CN 201210085311A CN 102643191 B CN102643191 B CN 102643191B
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lactic acid
phase
heavy phase
formula
solvent
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CN102643191A (en
Inventor
魏琦峰
刘喆
任秀莲
崔耀军
张博斌
张成伟
陈泳兴
王新
刘清华
陆德营
李志民
葛大森
刘金聚
孟科华
张树银
朱守林
孙自华
胡敏
代陶
魏坤
徐向阳
邢涛
韩英杰
毛洪涛
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Henan Jindan Lactic Acid Technology Co ltd
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Henan Jindan Lactic Acid Technology Co ltd
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Abstract

The invention discloses a heavy phase lactic acid processing technology. The heavy phase lactic acid processing technology comprises the following steps: (a) diluting: diluting heavy phase lactic acid till the mass fraction of the lactic acid is 10-60%; (b) decoloring through a carbon column: loading granular carbon in the carbon column and decoloring through the carbon column to get the heavy phase lactic acid to be extracted; and (c) extracting: wherein an organic extraction phase comprises an extracting agent, a solvent and a phase regulating agent, the extracting agent is of an amide type compound or a mixture of the amide type compounds, the solvent is of liquid paraffin, the phase regulating agent is of an alcohol type compound or the mixture of the alcohol type compounds, and the weight ratio of the three, namely the extracting agent, the solvent and the phase regulating agent is (5.5-6.5):(2.5-3.5):(0.5-1); the weight ratio of the organic extraction phase to the heavy phase lactic acid to be extracted is (1.1-1.5):1, and the extraction operation temperature is 20-70 DEG C; and the lactic acid is selectively transferred into the organic extraction phase to form a loaded organic phase, impurities in the heavy phase lactic acid are effectively separated from the lactic acid, the technological route is simple and the production cost is low.

Description

Heavy phase lactic acid treatment process
Technical field
The present invention relates to the organic extraction phase of using in extraction, particularly heavy phase lactic acid treatment process.
Background technology
Lactic acid is as foodstuff additive and industrial chemicals, and its Application Areas is more and more extensive, especially the market has openings of fine purification of lactic acid large (being raw material as production lactates, ester class and poly(lactic acid) etc. all need fine purification of lactic acid).But in lactic acid purification process, can produce raw material total mass 15% heavy phase lactic acid (heavy phase lactic acid: be common lactic acid in treating process, a part of lactic acid is distilled out, is called fine purification of lactic acid; And sugar in residual lactic acid and former lactic acid, pigment, albumen etc. are called as heavy phase lactic acid, are again black lactic acid; Because it can only be used for Feedstuff Enterprises on a small scale, therefore be referred to as again feed grade lactic acid; In heavy phase lactic acid, lactic acid content is generally 75-85%).
The purposes of heavy phase lactic acid is narrow, and consumption is little, is difficult to sell on market.Even if utilize traditional method to reprocess and produce lactic acid heavy phase lactic acid, the lactic acid that still has 5-8% in heavy phase lactic acid can not extract and be used; Moreover, heavy phase lactic acid is reprocessed to the cost of producing lactic acid higher than the selling price of lactic acid, lose more than gain on the contrary.This also causes fine purification of lactic acid expensive indirectly, is also restricting the accurately machined industrial scale of lactic acid simultaneously.
Summary of the invention
For the deficiencies in the prior art, the object of the present invention is to provide a kind of heavy phase lactic acid treatment process, can, by the most of lactic acid extraction in heavy phase lactic acid in organic phase, make to utilize heavy phase lactic acid can produce fine purification of lactic acid, and operational path be simple, production cost is low.
Technical scheme of the present invention is achieved in that heavy phase lactic acid treatment process, comprises the steps:
(a) dilution: the massfraction that heavy phase lactic acid is diluted to lactic acid is 10-60%;
(b) charcoal post decolouring: loaded particles charcoal in charcoal post, obtains heavy phase lactic acid to be extracted after the decolouring of charcoal post;
(c) extraction: organic extraction is made up of extraction agent, solvent and phase modifier, extraction agent is the mixture of amides or amides, solvent is whiteruss, phase modifier is the mixture of alcohol compound or alcohol compound, extraction agent, solvent and phase modifier three's mass ratio (5.5-6.5): (2.5-3.5): (0.5-1); Organic extraction phase is (1.1-1.5) with the mass ratio of heavy phase lactic acid to be extracted: 1, and extracting operation temperature is 20-70 DEG C; Lactic acid is transferred to selectively in organic extraction mutually and formed load organic phases, make the impurity in heavy phase lactic acid obtain effective separation with lactic acid; Water is after reverse osmosis membrane processing, and dialyzate is used for diluting initial feed heavy phase lactic acid; Concentrated solution decomposes in IC bio-reactor produces biogas, for the thermal source of feed drying.
Above-mentioned heavy phase lactic acid treatment process, the massfraction that in step (a), heavy phase lactic acid is diluted to lactic acid is 20%-30%; The middle extraction agent of step (c), solvent and phase modifier three's mass ratio 6: 3: 0.8; Organic extraction phase is 1.15: 1 with the mass ratio of heavy phase lactic acid to be extracted, and temperature is 30-45 DEG C.
Above-mentioned heavy phase lactic acid treatment process, in step (c), the time of balancing each other is 25-50min.
Above-mentioned heavy phase lactic acid treatment process, amides has as shown in the formula the structure shown in (I):
Wherein R1 is hydrogen, chain alkylene or alicyclic hydrocarbon radical, and R2 is hydrogen, chain alkylene or alicyclic hydrocarbon radical, and R3 is hydrogen, chain alkylene or alicyclic hydrocarbon radical.
Above-mentioned heavy phase lactic acid treatment process, R1, R2 and R3 are alkyl.
Above-mentioned heavy phase lactic acid treatment process, alcohol compound has as shown in the formula the structure shown in (II):
Wherein R4 is hydrogen, chain alkylene or alicyclic hydrocarbon radical, and R5 is hydrogen, chain alkylene or alicyclic hydrocarbon radical, and R6 is chain alkylene or alicyclic hydrocarbon radical.
The invention has the beneficial effects as follows: the present invention looks for another way, adopting heavy phase lactic acid is raw material production lactic acid and lactic acid salt, adds organic extraction phase, lactic acid is transferred to organic phase selectively and form load organic phases, makes impurity and lactic acid obtain effective separation.For the subsequent disposal obtain lactic acid salt of load organic phases and utilize lactic acid salt obtain lactic acid, can take method of the prior art to carry out.Prior art is existing is converted into Lactated method by the lactic acid in organic phase, the load organic phases that is equally applicable to obtain in this patent, and this patent is not described in detail in this.Adopting heavy phase lactic acid is raw material, has solved the restraining factors of purified grade lactic acid, and resource is rationally utilized.
Embodiment
embodiment 1
In the present embodiment, heavy phase lactic acid treatment process comprises the steps:
(a) dilution: the massfraction that heavy phase lactic acid is diluted to lactic acid is 20%;
(b) charcoal post decolouring: loaded particles charcoal in charcoal post, obtains heavy phase lactic acid to be extracted after the decolouring of charcoal post;
(c) extraction: organic extraction is made up of extraction agent, solvent and phase modifier, and extraction agent is amides, and solvent is whiteruss, and phase modifier is alcohol compound.Amides has as shown in the formula the structure shown in (I):
Wherein R1 is CH 3(CH 2) 3-, R2 is hydrogen, R3 is CH 3(CH 2) 3-.
Alcohol compound has as shown in the formula the structure shown in (II):
Wherein R4 is hydrogen, and R5 is hydrogen, and R6 is CH 3cH 2-.
Extraction agent, solvent and phase modifier three's mass ratio 5.5: 2.5: 0.5; Organic extraction phase is 1.1: 1 with the mass ratio of heavy phase lactic acid to be extracted, and extracting operation temperature is 30 DEG C, organic extraction phase is fully mixed with heavy phase lactic acid to be extracted, and stratification, the time of balancing each other is 30min; In water, lactic acid massfraction is 0.5%.Lactic acid is transferred to selectively in organic extraction mutually and formed load organic phases, make the impurity in heavy phase lactic acid obtain effective separation with lactic acid; Water is after reverse osmosis membrane processing, and dialyzate is used for diluting initial feed heavy phase lactic acid; Concentrated solution decomposes in work C bio-reactor produces biogas, for the thermal source of feed drying.
The load organic phases obtaining can be utilized the known obtain lactic acid from organic phase of prior art or Lactated method, carries out follow-up extraction step.
embodiment 2
The difference of the present embodiment and embodiment 1 is: the massfraction that in step (a), heavy phase lactic acid is diluted to lactic acid is 30%; In step (c): extraction agent, solvent and phase modifier three's mass ratio 6.5: 3.5: 1.Extraction agent is amides, and solvent is whiteruss, and phase modifier is alcohol compound.
Amides has as shown in the formula the structure shown in (I):
Wherein R1 is (CH 2) 5cH-, R2 is hydrogen, R3 is CH 3(CH 2) 7-.
Alcohol compound has as shown in the formula the structure shown in (II):
Wherein R4 is hydrogen, and R5 is hydrogen, and R6 is CH 3(CH 2) 5-.
Be 1.5: 1 fully to mix with heavy phase ammonium lacate to be extracted according to mass ratio by organic extraction phase,, extracting operation temperature is 33 DEG C, stratification, the time of balancing each other is 36min; In water, lactic acid massfraction is 0.4%.
embodiment 3
The difference of the present embodiment and embodiment 1 is: the massfraction that in step (a), heavy phase lactic acid is diluted to lactic acid is 25%; In step (c): extraction agent, solvent and phase modifier three's mass ratio 6: 3: 0.8.Extraction agent is amides, and solvent is whiteruss, and phase modifier is alcohol compound.
Amides has as shown in the formula the structure shown in (I):
Wherein R1 is CH 3(CH 2) 9-, R2 is hydrogen, R3 is CH 3(CH 2) 6-.
Alcohol compound has as shown in the formula the structure shown in (II):
Wherein R4 is hydrogen, and R5 is hydrogen, and R6 is CH 3cH 2-.
Be 1.3: 1 fully to mix with heavy phase ammonium lacate to be extracted according to mass ratio by organic extraction phase, extracting operation temperature is 33 DEG C, stratification, and the time of balancing each other is 50min; In water, lactic acid massfraction is 0.3%.
embodiment 4
The difference of the present embodiment and embodiment 1 is: the massfraction that in step (a), heavy phase lactic acid is diluted to lactic acid is 28%; In step (c): extraction agent, solvent and phase modifier three's mass ratio 5.7: 3.2: 0.7.Extraction agent is amides, and solvent is whiteruss, and phase modifier is alcohol compound.
Amides has as shown in the formula the structure shown in (I):
Wherein R1 is (CH 3) 2cHCH 2cH (CH 2cH 3) CH 2-, R2 is CH 3(CH 2) 2-, R3 is (CH 3) 2cHCH (CH 3) CH 2-.
Alcohol compound has as shown in the formula the structure shown in (II):
Wherein R4 is hydrogen, and R5 is hydrogen, and R6 is CH 3cH 2cH (CH 3) CH 2-.
Be 1.2: 1 fully to mix with heavy phase ammonium lacate to be extracted according to mass ratio by organic extraction phase, extracting operation temperature is 45 DEG C, stratification, and the time of balancing each other is 45min; In water, lactic acid massfraction is 0.5%.
embodiment 5
The difference of the present embodiment and embodiment 1 is: the massfraction that in step (a), heavy phase lactic acid is diluted to lactic acid is 21%; In step (c): extraction agent, solvent and phase modifier three's mass ratio 6.2: 2.8: 0.6.Extraction agent is amides, and solvent is whiteruss, and phase modifier is alcohol compound.
Amides has as shown in the formula the structure shown in (I):
Wherein R1 is CH 3cH (CH 3) CH 2-, R2 is CH 3-, R3 is CH 3(CH 2) 2cH (CH 3) (CH 2) 2-.
Alcohol compound has as shown in the formula the structure shown in (II):
Wherein R4 is hydrogen, and R5 is hydrogen, and R6 is CH 3(CH 2) 2-.
Be 1.4: 1 fully to mix with heavy phase ammonium lacate to be extracted according to mass ratio by organic extraction phase, extracting operation temperature is 40 DEG C, stratification, and the time of balancing each other is 30min; In water, lactic acid massfraction is 0.3%.
embodiment 6
The difference of the present embodiment and embodiment 1 is: the massfraction that in step (a), heavy phase lactic acid is diluted to lactic acid is 28%; In step (c); Extraction agent, solvent and phase modifier three's mass ratio 6: 3: 0.8.Extraction agent is amides, and solvent is whiteruss, and phase modifier is alcohol compound.
Amides has as shown in the formula the structure shown in (I):
Wherein R1 is CH 3(CH 2) 9-, R2 is CH 3cH 2-, R3 is CH 3(CH 2) 2cH (CH 3) (CH 2) 2-.
Alcohol compound has as shown in the formula the structure shown in (II):
Wherein R4 is CH 3-, R5 is hydrogen, R6 is CH 3(CH 2) 2-.
Be 1.3: 1 fully to mix with heavy phase ammonium lacate to be extracted according to mass ratio by organic extraction phase, extracting operation temperature is 36 DEG C, stratification, and the time of balancing each other is 40min; In water, lactic acid massfraction is 0.5%.
embodiment 7
The difference of the present embodiment and embodiment 1 is: the massfraction that in step (a), heavy phase lactic acid is diluted to lactic acid is 26%; In step (c); Extraction agent, solvent and phase modifier three's mass ratio 6.5: 3.5: 1.Extraction agent is amides, and solvent is whiteruss, and phase modifier is alcohol compound.
Amides has as shown in the formula the structure shown in (I):
Wherein R1 is CH 3cH (CH 3) CH 2-, R2 is CH 3cH 2-, R3 is CH 3(CH 2) 4-.
Alcohol compound has as shown in the formula the structure shown in (II):
Wherein R4 is hydrogen, and R5 is hydrogen, and R6 is CH 3(CH 2) 5-.
Be 1.25: 1 fully to mix with heavy phase ammonium lacate to be extracted according to mass ratio by organic extraction phase, extracting operation temperature is 31 DEG C, stratification, and the time of balancing each other is 35min; In water, lactic acid massfraction is 0.7%.
embodiment 8
The difference of the present embodiment and embodiment 1 is: the massfraction that in step (a), heavy phase lactic acid is diluted to lactic acid is 24%; In step (c): extraction agent, solvent and phase modifier three's mass ratio 6.5: 2.5: 1.Extraction agent is amides, and solvent is whiteruss, and phase modifier is alcohol compound.
Amides has as shown in the formula the structure shown in (I):
Wherein R1 is (CH 3) 2cH CH 2cH (CH 2cH 3) CH 2-, R2 is hydrogen, R3 is (CH 3) 2cHCH (CH 3) CH 2-.
Alcohol compound has as shown in the formula the structure shown in (II):
Wherein R4 is CH 3-, R5 is hydrogen, R6 is CH 3cH 2-.
Be 1.15: 1 fully to mix with heavy phase ammonium lacate to be extracted according to mass ratio by organic extraction phase, extracting operation temperature is 33 DEG C, stratification, and the time of balancing each other is 30min; In water, lactic acid massfraction is 0.2%.
embodiment 9
The difference of the present embodiment and embodiment 1 is: the massfraction that in step (a), heavy phase lactic acid is diluted to lactic acid is 22%; In step (c): extraction agent, solvent and phase modifier three's mass ratio 5.5: 3: 0.5.Extraction agent is amides, and solvent is whiteruss, and phase modifier is alcohol compound.
Amides has as shown in the formula the structure shown in (I):
Wherein R1 is (CH 2) 5cH-, R2 is CH 3-, R3 is (CH 2) 5cH-.
Alcohol compound has as shown in the formula the structure shown in (II):
Wherein R4 is hydrogen, and R5 is hydrogen, and R6 is CH 3cH 2cH (CH 3) CH 2-.
Be 1.23: 1 fully to mix with heavy phase ammonium lacate to be extracted according to mass ratio by organic extraction phase, extracting operation temperature is 38 DEG C, stratification, and the time of balancing each other is 40min; In water, lactic acid massfraction is 0.7%.
embodiment 10
The difference of the present embodiment and embodiment 1 is: the massfraction that in step (a), heavy phase lactic acid is diluted to lactic acid is 27%; In step (c): extraction agent, solvent and phase modifier three's mass ratio 6: 3: 0.8.Extraction agent is amides, and solvent is whiteruss, and phase modifier is alcohol compound.
Amides has as shown in the formula the structure shown in (I):
Wherein R1 is CH 3(CH 2) 3-, R2 is hydrogen, R3 is (CH 2) 5cHCH 2-.
Alcohol compound has as shown in the formula the structure shown in (II):
Wherein R4 is hydrogen, and R5 is hydrogen, and R6 is CH 3cH 2cH (CH 3) CH 2-.
Be 1.36: 1 fully to mix with heavy phase ammonium lacate to be extracted according to mass ratio by organic extraction phase, extracting operation temperature is 37 DEG C, stratification, and the time of balancing each other is 25min; In water, lactic acid massfraction is 0.5%.
embodiment 11
The difference of the present embodiment and embodiment 1 is: the massfraction that in step (a), heavy phase lactic acid is diluted to lactic acid is 26.5%; In step (c): extraction agent, solvent and phase modifier three's mass ratio 6: 3: 0.8.Extraction agent is amides, and solvent is whiteruss, and phase modifier is alcohol compound.
Amides has as shown in the formula the structure shown in (I):
Wherein R1 is CH 3(CH 2) 9-, R2 is CH 3(CH 2) 2-, R3 is CH 3(CH 2) 2cH (CH 3) (CH 2) 2-.
Alcohol compound has as shown in the formula the structure shown in (II):
Wherein R4 is hydrogen, and R5 is hydrogen, and R6 is CH 3(CH 2) 2-.
Be 1.44: 1 fully to mix with heavy phase ammonium lacate to be extracted according to mass ratio by organic extraction phase, extracting operation temperature is 32 DEG C, stratification, and the time of balancing each other is 30min; In water, lactic acid massfraction is 0.3%.
embodiment 12
The difference of the present embodiment and embodiment 1 is: the massfraction that in step (a), heavy phase lactic acid is diluted to lactic acid is 24%; In step (c): extraction agent, solvent and phase modifier three's mass ratio 6: 3: 0.8.Extraction agent is the mixture [volume ratio of the two is 1: 1] of the amides in embodiment 11 and embodiment 10, and solvent is whiteruss, and phase modifier is the mixture [volume ratio of the two is 1: 1] of the alcohol compound in embodiment 11 and embodiment 10.
Be 1.5: 1 fully to mix with heavy phase ammonium lacate to be extracted according to mass ratio by organic extraction phase, extracting operation temperature is 36 DEG C, stratification, and the time of balancing each other is 25min; In water, lactic acid massfraction is 0.2%.
In the above-described embodiments, the massfraction that heavy phase lactic acid can be diluted to lactic acid is any number between 10%-60%, extracting operation temperature can be any number between 20-70 DEG C, under similarity condition, all can realize the most lactic acid in heavy phase lactic acid are transferred to formation load organic phases in organic extraction mutually selectively, make the impurity in heavy phase lactic acid obtain effective separation with lactic acid, lactic acid massfraction in water is reduced to below 1%.The massfraction that preferably heavy phase lactic acid is diluted to lactic acid is 20%-30%, and temperature is 30-45 DEG C, can realize so better effect of extracting.
In above-described embodiment 2, embodiment 9 and embodiment 10, (CH 2) 5cH-represents that a hydrogen of hexanaphthene is substituted.
Above-described embodiment is only for the invention example is clearly described, and the not restriction to the invention embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here without being also listed as thoroughly all embodiments.And the apparent variation of being extended out thus or variation are still among the protection domain in the invention claim.

Claims (1)

1. heavy phase lactic acid treatment process, is characterized in that, comprises the steps:
(a) dilution: the massfraction that heavy phase lactic acid is diluted to lactic acid is 24%;
(b) charcoal post decolouring: loaded particles charcoal in charcoal post, obtains heavy phase lactic acid to be extracted after the decolouring of charcoal post;
(c) extraction: organic extraction is made up of extraction agent, solvent and phase modifier, extraction agent is the mixture that the amides of structure shown in two kinds of formula I mixes according to volume ratio 1:1, solvent is whiteruss, and phase modifier is the mixture that the alcohol compound of structure shown in two kinds of formula II mixes according to volume ratio 1:1;
The first compound shown in described two kinds of formulas (I) in structural compounds refers to that the R1 in formula (I) is CH 3(CH 2) 3-, R2 is hydrogen, R3 is (CH 2) 5cHCH 2-compound, the second compound refers in formula (I) that R1 is CH 3(CH 2) 9-, R2 is CH 3(CH 2) 2-, R3 is CH 3(CH 2) 2cH (CH 3) (CH 2) 2-compound;
The first compound shown in described two kinds of formula II in the compound of structure refers to that the R4 in formula II is hydrogen, and R5 is hydrogen, and R6 is CH 3cH 2cH (CH 3) CH 2-, the second compound refers to that in formula II, R4 is hydrogen, and R5 is hydrogen, and R6 is CH 3(CH 2) 2-;
Described extraction agent, solvent and phase modifier three's mass ratio 6:3:0.8; Organic extraction phase is 1.5:1 with the mass ratio of heavy phase lactic acid to be extracted, and extracting operation temperature is 36 DEG C; Organic extraction phase is fully mixed with heavy phase lactic acid to be extracted, stratification, the time of balancing each other is 25min; In water, lactic acid massfraction is 0.2%; Lactic acid is transferred to selectively in organic extraction mutually and formed load organic phases, make the impurity in heavy phase lactic acid obtain effective separation with lactic acid; Water is after reverse osmosis membrane processing, and dialyzate is used for diluting initial feed heavy phase lactic acid; Concentrated solution decomposes in IC bio-reactor produces biogas, for the thermal source of feed drying.
CN201210085311.3A 2012-03-28 2012-03-28 Heavy phase lactic acid processing technology Active CN102643191B (en)

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CN1407962A (en) * 1999-10-12 2003-04-02 普拉克生化公司 Continuous process for preparing lactic acid
CN1293033C (en) * 1999-10-12 2007-01-03 普拉克生化公司 Continuous process for preparing lactic acid
CN1509197A (en) * 2001-03-15 2004-06-30 A��E��˹�������칫˾ Process for obtaining organic and from organic acid ammonium salt, an organic acid amide, or alkylamine organic acid complex
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Inventor after: Zhang Bobin

Inventor after: Zhang Chengwei

Inventor after: Chen Yongxing

Inventor after: Wang Xin

Inventor after: Liu Qinghua

Inventor before: Liu Zhe

Inventor before: Meng Kehua

Inventor before: Zhang Shuyin

Inventor before: Zhu Shoulin

Inventor before: Sun Zihua

Inventor before: Hu Min

Inventor before: Cui Yaojun

Inventor before: Zhang Chengwei

Inventor before: Wang Xin

Inventor before: Liu Qinghua

Inventor before: Lu Deying

Inventor before: Li Zhimin

Inventor before: Ge Dasen

Inventor before: Liu Jinju

COR Change of bibliographic data

Free format text: CORRECT: INVENTOR; FROM: LIU ZHE CUI YAOJUN ZHANG CHENGWEI WANG XIN LIU QINGHUA LU DEYING LI ZHIMINGE DASEN LIU JINJU MENG KEHUA ZHANG SHUYIN ZHU SHOULIN SUN ZIHUA HU MIN TO: WEI QIFENG LIU ZHE REN XIULIAN CUI YAOJUN ZHANG BOBIN ZHANG CHENGWEI CHEN YONGXING WANG XIN LIU QINGHUA LU DEYING LI ZHIMIN GE DASEN LIU JINJU MENG KEHUA ZHANG SHUYIN ZHU SHOULIN SUN ZIHUA HU MIN DAITAO WEI KUN XU XIANGYANG XING TAO HAN YINGJIE MAO HONGTAO

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