CN1587077A - Process for extracting lignin by acid separation - Google Patents
Process for extracting lignin by acid separation Download PDFInfo
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- CN1587077A CN1587077A CN 200410062787 CN200410062787A CN1587077A CN 1587077 A CN1587077 A CN 1587077A CN 200410062787 CN200410062787 CN 200410062787 CN 200410062787 A CN200410062787 A CN 200410062787A CN 1587077 A CN1587077 A CN 1587077A
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- black liquor
- lignin
- xylogen
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Abstract
The present invention relates to the extraction process of acid out lignin, and is especially the process of treating waste digestion liquid produced during making paper pulp to extract lignin. The extraction process includes depositing separation to eliminate fiber mud and silt from black liquor, cooling black liquor containing lignin, adding flocculent and acid to deposit lignin, and filtering to obtain lignin containing product. The said process has high lignin extracting rate up to 95 %, and the obtained lignin has excellent water filtering performance and dryness over 25 %.
Description
Technical field:
The present invention relates to a kind of process for extracting lignin by acid separation, specifically a kind of cooking waste liquor that paper-making pulping is produced is handled, and therefrom extracts the method for xylogen.
Background technology:
In the alkaline process process, fibrous material and alkali lye generate the organism sodium salt and are dissolved in the cooking liquor after the chemical reaction of boiling, because of being black, so be called black liquor.Inorganics mainly is bonded sodium salt and free NaOH, Na in the black liquor
2SO
4, Na
2S, Na
2CO
3Reach the inorganic ash content that raw material is brought into, wherein major part is and black liquor organic compound bonded sodium.Organism mainly comprises the alkaline bleach liquor degradation product of xylogen and carbohydrate.
Xylogen is the aromatic polymer of a class complexity in the vegetable cell, and it is cellulosic tamanori, to increase the physical strength of plant materials.
Xylogen always with the Mierocrystalline cellulose association, with Mierocrystalline cellulose and hemicellulose be the main component that constitutes the plant skeleton.With regard to total amount, on the earth xylogen next in number only to Mierocrystalline cellulose, estimate that the annual whole world can produce 150,000,000,000 tons of xylogen by plant-growth.
Xylogen owing to be not fully utilized, has become environmental pollutant as the by product of wood saccharification industry and paper industry, has seriously polluted environment.A large amount of black liquids of paper mill discharge in the past contain considerable xylogen, have seriously polluted surface water and underground water, promptly cause a series of environment and social concern.
So the feasible method of xylogen is extracted in research from black liquid, make xylogen become useful thing, and it is utilized, be the important means that solves the black liquid contaminate environment.
Paper-making pulping has two kinds of methods; The first is with the acid accumulator sulfite solution boiling wood fragments of the calcium that contains free sulfurous acid, magnesium, sodium, ammonia, the script xylogen is sulfonated is water miscible sulfonated lignin, Mierocrystalline cellulose is then separated out, leach Mierocrystalline cellulose, remaining promptly is spent pulping liquor, handle the promptly precipitable xylogen of separating out with milk of lime; It two is straw or wheat straws with concentrated caustic liquid high temperature steaming wood fragments or chopping, and this moment, lignin dissolution became alkali lignin originally, and Mierocrystalline cellulose is separated out filtration, and remaining is usually said black liquor, uses the acid treatment black liquor, can separate out xylogen.But the xylogen solids content of using the processing of this kind method is generally less than 10%, and the state thickness, and drainability is poor, can't utilize again, can only be as waste treatment.
Because the restriction of various conditions up to now, does not still have a kind of method that all can satisfy extraction xylogen from the heavy industrialization paper-making pulping black liquor technically, economically.
The integrated conduct method of the open papermaking wastewater of Chinese patent CN01115000.9 " method of a kind of wheat straw alkaline pulping black liquor zero release " relates to following content:
1) with containing SO
2And CO
2Waste gas make black liquor PH reduce to 6-8 earlier, extract xylogen then;
2) with 1/4th black liquor dissolving polyacrylamide (before the A section);
3) polyacrylamide solution is sneaked into whole black liquor (A section);
4) add 93% sulfuric acid and make PH reduce to 1 (B section), xylogen is separated out;
5) tiltedly net separates.
Chinese patent CN99116492.X " process for removing lignin from black liquor in making paper by soda pulping " discloses following content:
1) directly the alkalitropism black liquor adds organic polymer ionogen (independent or mixing adds multiple materials such as positively charged ion, positively charged ion, non-ionic polyacrylamide);
2) add acid (preferably sulfuric acid, phosphoric acid), transfer pH value, separate out xylogen less than 5;
3) use the universal method separating lignin.
The undeclared efficient of removing fibered plaster that leaves standstill of the content of above-mentioned patent disclosure, leave standstill the rotten concrete influence that produces of the overtime acidifying that causes, the vitriolic consumption, final pH value and lignin extraction rate reach 90% concrete data, what is more important, on this technical barrier of lignin extraction, each stepping step, an even very little technical progress, all be considered to extremely difficult, though relate to the technology contents of some lignin extraction in the above-mentioned patent, but these contents are enough not concrete in detail, for those skilled in the art, reproduce this and invent described technical scheme and technique effect, material impact is arranged.
Summary of the invention:
The object of the present invention is to provide a kind of process for extracting lignin by acid separation, specifically provide a kind of cooking waste liquor that paper-making pulping is produced and handle, therefrom extract the method for xylogen.
Contain a large amount of xylogen in a large amount of black liquids that alkaline process produces, xylogen is that the form with the solubility sodium phenolate exists in basic solution, thereby when adding acid, xylogen is transformed into insoluble free phenol gradually and separates out from black liquor.
The primary process of technology of the present invention is to pass through precipitate and separate, remove fibered plaster and silt in the black liquor, the black liquor that will contain xylogen then cools, and the cooling back adds flocculation agent in black liquor, add acid then and make the xylogen precipitation, obtain containing the product section of xylogen after the filtration.
Process for extracting lignin by acid separation of the present invention is suitable for existing alkaline process paper technology, and its main process may further comprise the steps:
The black liquor pre-treatment that paper-making pulping is obtained purifies, and the black liquor after the purification cools off by cooling system, makes the temperature of black liquor reduce to 0-35 ℃; Cooled black liquor enters storage pool and collects, and gets wherein a part of black liquor as solvent, after wherein adding flocculation agent, mixing, itself and other a part of black liquor is merged, and enters the first order reaction tempering tank, behind the uniform mixing, enters the secondary main reactor; Add H to the secondary main reactor simultaneously
2SO
4Or H
2SO
4Mixed solution; With the reaction mixture filtration treatment, obtain lignin product.
When obtaining xylogen, the filtrate after the filtration treatment enters filtrate collection pond precipitation, isolates supernatant liquor, and its understorey quality is partly returned and entered the first order reaction tempering tank, continues reaction.
H to the adding of secondary main reactor
2SO
4Mixed solution is H
2SO
4Doubly measure the mixed solution of supernatant liquor in the collecting tank with 0-5.
Described black liquor pre-treatment is for to leave standstill black liquor in settling tank, the time is 8-12 hour; Main purpose is to remove impurity such as silt in the black liquor, fibered plaster; Being beneficial to so on the one hand and obtaining the higher xylogen of purity, is that the removal of fibered plaster can make xylogen have better drainability in the treating processes of back on the other hand, and promptly xylogen is easy to separate with water; And the existence of fibered plaster is except that directly causing xylogen drainability difference, and anaerobic acidification is rotten in a short time also can to make black liquor, and follow-up treating processes can't be carried out.Therefore, must carry out pre-treatment timely to the black liquor that slurrying obtains; Pretreated time control ratio is strict, overlong time, and the xylogen part is anaerobic acidification easily, and the total system of back can't normally be carried out; Time is too short, and fibered plaster and sediment deposition amount are few, and xylogen partly contains fibered plaster and silt is more, and viscosity is bigger, causes xylogen and water to be difficult for separating.
Cooling system can be the two-stage series connection cooling tower; It is in series by two cooling towers, and black liquor cools off through two-stage countercurrent; Technology of the present invention requires strict especially to black liquor temperature, black liquor enters before the main reactor, and must cool the temperature to just has good treatment effect below 35 ℃, and the temperature of black liquor is low more, and treatment effect is good more.
Described flocculation agent is preferably anion-polyacrylamide (PAM).
The anion-polyacrylamide molecular weight is 300-2000 ten thousand, and degree of hydrolysis is 15-50%, and preferred molecular weight is 1500-1800 ten thousand, and the selective hydrolysis degree is 30-50%.
The anion-polyacrylamide add-on is a 100-200 gram/cubic meter, is preferably 100-120 gram/cubic meter.
Get wherein a part of black liquor as dissolution with solvents PAM, can reduce cost on the one hand, simplify technology, can not increase new solvent on the other hand, slow down the pressure of subsequent processes.PAM when dissolving should black liquor enter the mouth vertical direction above evenly add with black liquor, otherwise, just can't well dissolve in case concentrate to add, can cause the waste of raw material medicament, the while may cause line clogging.
Described H
2SO
4For concentration greater than 93% H
2SO
4H
2SO
4It is 1.5-2 that add-on is answered the pH value of the reaction mixture of meeting tier 2 main reactor.
Described first order reaction tempering tank should be able to make PAM solution and cooling black liquor thorough mixing, otherwise can't reach the optimum handling effect.The present invention preferably adopts the flap reactive tank to mix, and cold black liquid contacts with the square crossing of PAM solution simultaneously, just mixes in the initial stage, has increased mixing efficiency.
Described secondary main reactor is fallen mixed system for the level Four staged; H
2SO
4Add fashionable, reactive tank add the inlet and bottom land can use grouan slabstone covering protection.
Described filtering system is an oblique net filtration system, and this system adopts acid-resistant glass steel plate to make filter plate, makes filtering net with the acidproof polyester webs of 30-40 order, collects the xylogen part of holding back, and promptly gets the target product xylogen; The mass dryness fraction of gained xylogen (solids content) can reach more than 25%, and xylogen is pie, does not contain xylogen in the filtrate substantially.Tiltedly the net filtration system is the basic place that technology black liquor treatment capacity of the present invention is big, investment is little, when the material that reacts completely enters this system, can in a short period of time xylogen and filtrate be separated.
There are two effects in described filtrate collection pond, and the one, centralized collection filtrate, its supernatant liquor can enter subsequent technique and handle, and reduces production costs; The 2nd, contained lignin recovery in the filtrate is utilized again, return again and enter the first order reaction groove, participate in reaction, can increase the productive rate of xylogen, reduce cost.Return enter the first order reaction groove before, should make a large amount of cooling black liquor and the abundant mixing of PAM solution after, add the lignin liquor of filtrate collection pond lower floor again, and abundant mixing.
Adding H to the secondary main reactor
2SO
4The time, the sulfuric acid of adding mixes formation H with the collecting tank supernatant liquor of 0-5 times of weight
2SO
4Mixed solution enters the secondary main reactor; Both solved H
2SO
4With the empyreumatic problem of xylogen in the concentrated black liquid, it is excessive because of concentration, viscosity to have solved reactant again, does not have flowability, is difficult to the blended problem, thereby makes technology of the present invention can well handle concentrated black liquid.Above-mentioned utilization again to supernatant liquor, every alkaline process gained black liquor, technology of the present invention is all applicable, particularly adopts the slurrying of preimpregnation digesting technoloy and the high concentration black liquor that obtains is particularly suitable.
Adopt processing method of the present invention to handle the black liquor that paper-making pulping obtains, extract xylogen, have following characteristics;
The disposable extraction yield height of √ xylogen can reach more than 90%, reaches as high as 95%;
The handled xylogen of √ has good drainability, and under the additional situation of using any equipment, natural filtration half an hour, the xylogen mass dryness fraction can reach more than 25%; Be beneficial to and be recycled;
The √ reaction process is directly perceived, and is easy and simple to handle;
√ compares with lignin separation process for extracting of the prior art, and technology one-time investment of the present invention is little, and processing power is big;
√ all is suitable for the black liquor that alkaline process obtains.
Description of drawings:
Fig. 1 is a process for extracting lignin by acid separation schema of the present invention
Fig. 2 adopts preimpregnation digesting technoloy black liquor of pulp making for the present invention is directed to, and carries out the extraction process schema of lignin by acid separation
Embodiment:
Embodiment 1
500 side's black liquor were left standstill in the pond 10 hours, make wherein fibered plaster and sediment deposition, the upper strata black liquor enters the cooling of two-stage series connection cooling tower, makes the temperature of black liquor reduce to 35 ℃; Cooled black liquor enters storage pool and collects, getting 50 side's black liquor as solvent, is 1,500 ten thousand polyacrylamide (Gongyi City blue star water-purifying material factory, APAM to wherein adding molecular weight, white particle) 50kg, add fashionablely, above black liquor inlet vertical direction, evenly add, after in special-purpose dissolving tank, mixing with black liquor, squeeze into the flap reactive tank by volume pump, merge with other a part of black liquor, behind the uniform mixing, enter and have the secondary main reactor that the level Four staged is fallen mixed system; Adding simultaneously, is 93% H to secondary main reactor adding concentration by ceramic pump
2SO
4Adding of reactive tank enters the mouth and bottom land use grouan slabstone covering protection.The reactive tank effluent liquid filters by oblique net filtration system, and damming obtains the 450t lignin product, and mass dryness fraction is 25%; Tiltedly the net filtration system adopts the acid-resistant glass steel plate to make filter plate, makes filtering net with the acidproof polyester webs of 40 orders.Filtrate enters the filtrate collection pond, and its lower floor contains xylogen and partly returns and enter the first order reaction tempering tank, continues to participate in subsequent reactions.
Embodiment 2
1000 side's black liquor were left standstill in the pond 8 hours, make wherein fibered plaster and sediment deposition, the upper strata black liquor enters the cooling of two-stage series connection cooling tower, makes the temperature of black liquor reduce to 30 ℃; Cooled black liquor enters storage pool and collects, get 200 side's black liquor as solvent, to wherein adding molecular weight is polyacrylamide (Gongyi City blue star water-purifying material factory of 1,000 ten thousand, APAM, white particle) 120kg, add fashionable, above black liquor inlet vertical direction, evenly add with black liquor, after in special-purpose dissolving tank, mixing, squeeze into the flap reactive tank by volume pump, merge with other a part of black liquor, behind the uniform mixing, enter and have the secondary main reactor that the level Four staged is fallen mixed system; Adding simultaneously, is 95% H to secondary main reactor adding concentration by ceramic pump
2SO
4Adding of reactive tank enters the mouth and bottom land use grouan slabstone covering protection.The reactive tank effluent liquid filters by oblique net filtration system, and damming obtains the 948t lignin product, and mass dryness fraction is 30%; Tiltedly the net filtration system adopts the acid-resistant glass steel plate to make filter plate, makes filtering net with the acidproof polyester webs of 30 orders.
Filtrate enters the filtrate collection pond, and its lower floor contains xylogen part and can return and enter the first order reaction tempering tank, continues to participate in subsequent reactions.
Supernatant liquid in the collecting tank mixes according to 5: 1 weight ratio with 95% the vitriol oil, enters the secondary main reactor, participates in reaction.
Embodiment 3
1000 side's black liquor were left standstill in the pond 12 hours, make wherein fibered plaster and sediment deposition, the upper strata black liquor enters the cooling of two-stage series connection cooling tower, makes the temperature of black liquor reduce to 20 ℃; Cooled black liquor enters storage pool and collects, get 300 side's black liquor as solvent, to wherein adding the 200kg molecular weight is 2,000 ten thousand polyacrylamide (Yixing City angel synthetic chemistry company limited), add fashionablely, above black liquor inlet vertical direction, evenly add, after in special-purpose dissolving tank, mixing with black liquor, squeeze into the flap reactive tank by volume pump, merge with other a part of black liquor, behind the uniform mixing, enter and have the secondary main reactor that the level Four staged is fallen mixed system; Adding simultaneously, is 100% H to secondary main reactor adding concentration by ceramic pump
2SO
4Adding of reactive tank enters the mouth and bottom land use grouan slabstone covering protection.The reactive tank effluent liquid filters by oblique net filtration system, and damming obtains the 932t lignin product, and mass dryness fraction is 35%; Tiltedly the net filtration system adopts the acid-resistant glass steel plate to make filter plate, makes filtering net with the acidproof polyester webs of 35 orders.
Filtrate enters the filtrate collection pond, and its lower floor contains xylogen part and can return and enter the first order reaction tempering tank, continues to participate in subsequent reactions.
Supernatant liquid in the collecting tank mixes according to 3: 1 weight ratio with 100% the vitriol oil, enters the secondary main reactor, participates in reaction.
Comparative example 1
This comparative example is used the integrated conduct method of the open papermaking wastewater of Chinese patent CN01115000.9 " method of a kind of wheat straw alkaline pulping black liquor zero release ", compares with embodiment 1, with the effect of checking the inventive method.
Description according to embodiment among the CN01115000.9, with COD greater than 80,000 black liquor 300t through steeping the vent gas treatment that colored alkali produces in producing, pH value was reduced to 8 o'clock, getting 20,000 tons of black liquor, to add molecular weight be polyacrylamide (Gongyi City blue star water-purifying material factory of 1,500 ten thousand, APAM, white particle) 25kg stirred after 4 hours, mixed with the remainder black liquor, add then 93% sulfuric acid to PH be 1, thorough mixing obtains 103.6 tons in the xylogen of mass dryness fraction 25% by oblique net separator, and extraction yield is 73.9%.
Comparative example 2
According to Chinese patent CN99116492.X " process for removing lignin from black liquor in making paper by soda pulping " disclosed method, according to embodiment 1, experimentize, the xylogen that the 1000mL black liquor obtains only has the 33g dry product, and extraction yield is lower.
Claims (10)
1, a kind of process for extracting lignin by acid separation, its main process comprises: the black liquor pre-treatment that paper-making pulping is obtained purifies, and the black liquor after the purification cools off by cooling system, makes the temperature of black liquor reduce to 0-35 ℃; Cooled black liquor enters storage pool and collects, and gets wherein a part of black liquor as solvent, after wherein adding flocculation agent, mixing, itself and other a part of black liquor is merged, and enters the first order reaction tempering tank, behind the uniform mixing, enters the secondary main reactor; Add H to the secondary main reactor simultaneously
2SO
4Or its mixed solution; With the reaction mixture filtration treatment, obtain lignin product.
2, technology according to claim 1 is characterized in that the filtrate after the filtration treatment enters filtrate collection pond precipitation, isolates supernatant liquor, and its understorey quality is partly returned and entered the first order reaction tempering tank, continues reaction.
3, technology according to claim 1 and 2 is characterized in that the H that adds to the secondary main reactor
2SO
4Mixed solution is H
2SO
4Doubly measure the mixed solution of supernatant liquor in the collecting tank with 0-5.
4, according to claim 1,2 or 3 described technologies, it is characterized in that described black liquor pre-treatment for black liquor is left standstill in settling tank, the time is 8-12 hour.
5,, it is characterized in that described cooling system is the two-stage series connection cooling tower according to claim 1,2 or 3 described technologies.
6, according to claim 1,2 or 3 described technologies, it is characterized in that described flocculation agent is an anion-polyacrylamide, the anion-polyacrylamide molecular weight is 300-2000 ten thousand, degree of hydrolysis is 15-50%; Preferred molecular weight is 1500-1800 ten thousand, and the selective hydrolysis degree is 30-50%.
7,, it is characterized in that described flocculant addition is a 100-200 gram/cubic meter according to claim 1,2 or 3 described technologies; Be preferably 100-120 gram/cubic meter.
8, according to claim 1,2 or 3 described technologies, it is characterized in that described H
2SO
4For concentration greater than 93% H
2SO
4H
2SO
4It is 1.5-2 that add-on is answered the pH value of the reaction mixture of meeting tier 2 main reactor.
9,, it is characterized in that described first order reaction tempering tank adopts flap reactive tank and/or secondary main reactor to fall mixed system for the level Four staged according to claim 1,2 or 3 described technologies.
10, according to claim 1,2 or 3 described technologies, it is characterized in that described filtering system is an oblique net filtration system, this system adopts acid-resistant glass steel plate to make filter plate, makes filtering net with the acidproof polyester webs of 30-40 order.
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|---|---|---|---|
| CNB2004100627870A CN100358811C (en) | 2003-08-26 | 2004-07-09 | Process for extracting lignin by acid separation |
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|---|---|---|---|
| CN03156409.7 | 2003-08-26 | ||
| CN03156409 | 2003-08-26 | ||
| CNB2004100627870A CN100358811C (en) | 2003-08-26 | 2004-07-09 | Process for extracting lignin by acid separation |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101503431B (en) * | 2008-02-04 | 2011-05-25 | 西南科技大学 | Technology for extracting high purity lignin from pulping black liquor by organic carboxyl acid method |
| CN102635011A (en) * | 2012-04-12 | 2012-08-15 | 谢明文 | Recycling comprehensive utilization technology for pulping black liquor or red liquor |
| CN102701201A (en) * | 2012-06-21 | 2012-10-03 | 山东大学 | Method for preparing activated carbon powder with lignin from alkaline papermaking black liquor |
| CN105018160A (en) * | 2015-06-24 | 2015-11-04 | 济南圣泉集团股份有限公司 | Coal water slurry dispersant and its preparation method and use |
| CN106675058A (en) * | 2016-12-11 | 2017-05-17 | 雷笑天 | Preparation method of biomass graphite electrode bonding agent |
| CN108484931A (en) * | 2018-05-09 | 2018-09-04 | 上海昶法新材料有限公司 | A method of the extracting and developing lignin from reducing rules treatment fluid |
| CN108864441A (en) * | 2017-10-13 | 2018-11-23 | 济宁明升新材料有限公司 | A method of extracting lignin from reducing rules treatment fluid |
| CN108864440A (en) * | 2017-10-13 | 2018-11-23 | 济宁明升新材料有限公司 | A method of extracting lignin from alkaline pulping black liquor |
| CN108951251A (en) * | 2017-05-19 | 2018-12-07 | 济宁明升新材料有限公司 | A method of extracting separating lignin from dissolving pulp pre-cooked liquid |
| WO2019174109A1 (en) * | 2018-03-16 | 2019-09-19 | 伍鹏 | Method for manufacturing nano-carbon microparticle |
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| CN1125696A (en) * | 1995-09-14 | 1996-07-03 | 王钦静 | Treatment and circulating reuse method for paper-making waste water |
| CN1059644C (en) * | 1996-01-31 | 2000-12-20 | 迁安县华丰造纸厂 | Treating method for black liquor of pape-making |
| CN1057512C (en) * | 1996-07-12 | 2000-10-18 | 山东省高唐县造纸厂 | Harnessing method for papermaking waste water |
| CN1229156A (en) * | 1998-03-13 | 1999-09-22 | 刘平 | Double-retrieving of lignin and alkali from papermaking black liquor |
| CN2619967Y (en) * | 2002-11-11 | 2004-06-09 | 刘树军 | Papermaking device capable of removing black liquor contamination |
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| CN101503431B (en) * | 2008-02-04 | 2011-05-25 | 西南科技大学 | Technology for extracting high purity lignin from pulping black liquor by organic carboxyl acid method |
| CN102635011A (en) * | 2012-04-12 | 2012-08-15 | 谢明文 | Recycling comprehensive utilization technology for pulping black liquor or red liquor |
| CN102635011B (en) * | 2012-04-12 | 2013-10-23 | 谢明文 | Recycling comprehensive utilization technology for pulping black liquor or red liquor |
| CN102701201A (en) * | 2012-06-21 | 2012-10-03 | 山东大学 | Method for preparing activated carbon powder with lignin from alkaline papermaking black liquor |
| CN102701201B (en) * | 2012-06-21 | 2015-11-18 | 山东大学 | A kind of lignin from alkaline paper-making black liquor prepares the method for Powdered Activated Carbon |
| CN105018160B (en) * | 2015-06-24 | 2017-08-11 | 济南圣泉集团股份有限公司 | Coal water slurry dispersing agent and its preparation method and application |
| CN105018160A (en) * | 2015-06-24 | 2015-11-04 | 济南圣泉集团股份有限公司 | Coal water slurry dispersant and its preparation method and use |
| CN106675058A (en) * | 2016-12-11 | 2017-05-17 | 雷笑天 | Preparation method of biomass graphite electrode bonding agent |
| CN108951251A (en) * | 2017-05-19 | 2018-12-07 | 济宁明升新材料有限公司 | A method of extracting separating lignin from dissolving pulp pre-cooked liquid |
| CN108951251B (en) * | 2017-05-19 | 2021-04-06 | 济宁明升新材料有限公司 | Method for extracting and separating lignin from dissolving pulp precooking liquid |
| CN108864441A (en) * | 2017-10-13 | 2018-11-23 | 济宁明升新材料有限公司 | A method of extracting lignin from reducing rules treatment fluid |
| CN108864440A (en) * | 2017-10-13 | 2018-11-23 | 济宁明升新材料有限公司 | A method of extracting lignin from alkaline pulping black liquor |
| WO2019174109A1 (en) * | 2018-03-16 | 2019-09-19 | 伍鹏 | Method for manufacturing nano-carbon microparticle |
| US11261094B2 (en) | 2018-03-16 | 2022-03-01 | Peng Wu | Method for manufacturing nano-carbon microparticle |
| CN108484931A (en) * | 2018-05-09 | 2018-09-04 | 上海昶法新材料有限公司 | A method of the extracting and developing lignin from reducing rules treatment fluid |
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