CN1050241A - Lignin separator and purifying technique for black liquor - Google Patents
Lignin separator and purifying technique for black liquor Download PDFInfo
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- CN1050241A CN1050241A CN 90107652 CN90107652A CN1050241A CN 1050241 A CN1050241 A CN 1050241A CN 90107652 CN90107652 CN 90107652 CN 90107652 A CN90107652 A CN 90107652A CN 1050241 A CN1050241 A CN 1050241A
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- lignin
- black liquor
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- acid
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Abstract
Carry out industrial utilization in order from the papermaking digesting black liquor, to extract purer lignin, and make black liquor obtain administering, a whole set of equipment and the technology of lignin separator and separating lignin thereof purification black liquor have been invented, it is characterized in that this equipment and technology are the molten gas of black liquor, acid out and air supporting disjoint set are in same system and adopted (1) black digestion liquid preliminary treatment, (2) flocculation of lignin with separate, (3) four technological process and corresponding manufacturing conditions that step is formed such as post processing of the dehydration of lignin and (4) parting liquid, realize the production serialization, reached the purpose of turning harm into good.
Description
The present invention relates to the technical scheme of paper industry black digestion liquid lignin extraction and black liquor treatment, i.e. the Processes and apparatus of lignin separation, purifying black liquor.
At present, the medium and small papermaking enterprise of China is thousands of, and the overwhelming majority adopts soda pulping process, and does not possess the alkali recvery facility, and its black digestion liquid directly enters rivers, polluted source, and this has become one of major source of pollutant of China's industry.
Paper industry black digestion liquid Main Ingredients and Appearance is a lignin, in addition, also contains some glucide and inorganic matter etc.Lignin is a kind of macromolecule aromatic compound, is a kind of abundant, reproducible natural resources.Lignin product can be used in dozens of industrial departments such as road, bridge, dyestuff, ore dressing, oil drilling, feed, soil improvement widely.How to turn harm into good? country stands it for this reason and is " the Seventh Five-Year Plan " emphasis key scientific and technological projects.
The objective of the invention is research, design a new technology path administering black liquid, separating lignin, provide a kind of and can purify black liquor and can isolate equipment than Vinsol.Thereby make the lignin product of producing high-quality and high economic worth become possibility.
Be applicable to the technology of lignin separation, purification paper industry black digestion liquid, mainly finish by following four steps:
(1) preliminary treatment of paper industry black digestion liquid,
(2) flocculation of lignin with separate,
(3) dehydration of lignin,
(4) post processing of parting liquid.
Its corresponding manufacturing condition is as follows:
One, the preliminary treatment of paper industry black digestion liquid
Though because the lignin separator scope of application is wide, it requires the into concentration stabilize of machine black liquor, so the first step need carry out black liquid consistency and regulate, and promptly black liquid consistency is adjusted to 0.2 ' Be(Baume)～certain value between the 9 ' Be.Second step was that the black liquor of concentration stabilize is sent into black liquor preliminary treatment jar, sent into compressed air by air compressor simultaneously, and keeping its operating pressure is 2～4kg/cm
2, air compressor has automatic starting device, at insufficient pressure 2～4kg/cm
2Shi Zidong starting handle air is pressed into cylinder and delivers in the preliminary treatment jar.Size of this jar and black liquor inlet are different with the difference of production capacity, and black liquor advances jar flow can be at 0.5m
3/ hr～80m
3Select in/hr the scope.Black liquor time of staying in the preliminary treatment jar is different and different with black liquid consistency, can adjust in the scope at 3～30 minutes.By this process, dissolved into a large amount of microbubbles in the black liquor.
Two, the flocculation of lignin with separate
The inventor has studied the primary condition that lignin separates from the characteristic of research black liquor and lignin, design the lignin separator of lignin acid out and dissolved air flotation unification, this machine is made of flocculation zone and Disengagement zone, the black liquor of drawing from the preliminary treatment jar with prepare certain density acid, lead the into lignin flocculation zone of seperator in proportion by blender, fully mixing in time in back several seconds to tens second lignin promptly separates out, and be subjected to the bubble adhesion that black liquor brings into and float, flocculation zone is designed to round table-like, the acid that enters and black liquor are mixed in the limited small size in the bottom of rounding platform, react more all even complete, in addition, the lignin colloid of separating out stroke cross section along with rising when come-up increases gradually, the rate of climb slows down gradually, accomplish reposefully and fluid separation applications, arrive on the heavy caliber disc and escape into the Disengagement zone.
The pH value that enters the black liquor of flocculation zone is 8～14, mixes with the acid of introducing, and its pH value is adjusted to pH=2～4 o'clock, and lignin is separated out, and acid can be sulfuric acid, hydrochloric acid, nitric acid, technical grade or industrial waste acid; The concentration employing 10%(percentage by weight of acid) all can more than; The consumption of acid is difference with the difference of the pH value (depending on residual alkali number) of black liquor, reaches pH=2～4 with adjusting black liquor pH value and is as the criterion, and general consumption is that 0.5～4% of processed black liquor does not wait.Black liquor is 5～30 minutes in the flocculation zone time of staying; In the time of staying of Disengagement zone is 20～100 minutes.The linear velocity that lignin rises is 0.2～12cm/min, and the S shape scraper plate that is being rotated to the seperator top that floats is scraped in the lignin chute.Parting liquid takeoff line speed is 0.5～12.0cm/min.
Three, lignin dehydration
Carrying relatively large bubble from the isolated lignin material of piece-rate system, its severe is 0.5～0.9g/cm
3The lignin material enters the lignin storagetank, in groove, continue come-up, the lignin Water Extraction Machinery is drained, changed over to bottom water, material is heated to 70～90 ℃, makes its polycondensation become bigger particle, and from the lignin material, separate out a large amount of moisture content, free moisture content is drained, obtain moisture about 50% lignin material, can be transported to lignin source mill and process, necessary fashion can arrive air dried condition to the lignin dry materials with conventional drying mode.
Four, the post processing of parting liquid
Parting liquid pH=2～4 that the self-separation machine is discharged, and discharging standards pH=6～9 adopt sand filter to filter, and it is neutral that discharge liquor pH value reaches, and sand that its sand filter adopts is thin river sand or quartz sand.
The drawing of accompanying drawing is described as follows:
Fig. 1 is lignin separation, purifying black liquor technological process block-diagram.
Fig. 2 is lignin separation, purifying black liquor equipment flowsheet.
Fig. 3 is the structural representation of lignin separator.
The inventor is according to the characteristic of black liquor and lignin, adopt the method for the molten gas of black liquor, acid out, dissolved air flotation, designed the equipment of the lignin separation system that must satisfy above-mentioned basic production process conditions, this system equipment comprises that preliminary treatment jar, seperator and auxiliary device thereof form, its schematic diagram as shown in Figure 2:
1 is the concentrated black liquid storagetank,
2 are black liquor storagetank after the adjusting concentration,
3 are the preliminary treatment jar,
4 is lignin separator,
5 is separating lignin storing material groove,
6 is the lignin Water Extraction Machinery.
Wherein capital equipment is preliminary treatment jar and black liquid separation machine.
(1) preliminary treatment jar
The preliminary treatment jar is to be that cylinder connects the pressure vessel that forms in the middle of being hemisphere by two ends, is provided with Pressure gauge, safety valve and flowmeter, and its blade diameter length ratio is 5.5: 1～3: 1, and its volume depends on treating capacity.
(2) lignin seperator
Fig. 3 is the structural representation of lignin seperator, and 1 is blender among the figure; 2 is the black liquor import; 3 is the acid solution import; 4 is S shape scraper plate; 5 are the lignin outlet; 6 is chute; 7 is discharge channel; 8 is interior rounding platform wall.As shown in Figure 3: the lignin separation engine housing is connect by cylinder and last round platform, the following rounding All-China Federation of Taiwan Compatriots and forms, bottom in its shell is provided with an interior rounding platform 8, the volume of interior rounding platform is called the lignin flocculation zone, and the peripheral space of interior rounding platform and upper space thereof are the lignin separation district.
Flocculation zone central authorities are provided with the blender 1 that is connected with black liquor import 2 and acid solution import 3, the top whole circumference of Disengagement zone is lignin outlet 5, above lignin outlet 5, is provided with S shape scraper plate 4, above the seperator shell, be provided with lignin chute 6 with a slope along last round platform periphery.The bottom, Disengagement zone of interior rounding platform periphery is provided with discharge channel 7.The manufactured materials of lignin separator must be acidproof.
(3) auxiliary device
Storagetank after concentrated black liquid storagetank and the adjusting concentration is alkaline-resisting container.Parting liquid and lignin storing material groove are acid-resistant containers.The lignin Water Extraction Machinery is an indirect steam heater, is made of acid resisting material.
Below in conjunction with lignin separation purifying black liquor process flow diagram and embodiment, the invention will be further described:
Chinese alpine rush kraft cooking black liquor is delivered to the black liquid consistency regulating tank from the black liquor storagetank, and black liquid consistency is adjusted to the 1.2'Be(Baume) black liquor PH=12, and with 0.58m
3The speed of/hr pumps into A
3Steel is that the volume of material manufacturing is that φ 300mm * 1500mm, wall thickness are the preliminary treatment jar of 5mm.Send into compressed air, make this pressure tank maintain 2.4kg/cm
2, the time of staying is 12 minutes, and black liquor has dissolved in enough microbubbles, and black liquor is introduced flocculation zone into seperator from the middle part of lignin separator by blender then, and the flexible pipe that acid solution import 2 connects communicates with blender, and concentration is 30% H
2SO
4Enter flocculation zone simultaneously with black liquor, the acid consumption is the 0.7%(percentage by weight of processed black liquor) acid evenly spreads with black liquor and to mix, existing a large amount of lignin are separated out within 10 seconds, and be subjected to that original microbubble institute rest floats in the black liquor, stop at flocculation zone is 10 minutes, after the lignin of come-up enters the Disengagement zone, in the Disengagement zone time of staying is 30 minutes, lignin is with the speed come-up of 8cm/min, the S shape scraper plate 4 that arrival seperator top is being rotated is scraped in the lignin chute 6, and the lignin storagetank of sending into separation then leaves standstill deposits about 3 hours, and lignin continues come-up, parting liquid is discharged from the parting liquid outlet of storagetank bottom, the lignin that separates is sent into firing equipment, reach 90 ℃ in the indirect steam heating, lignin continues polycondensation, deviate from a large amount of parting liquids again, isolated lignin material is moisture about 50%, can pack, and send lignin source mill to process.
Clear liquid PH=3～4 behind the parting liquid that the self-separation machine is discharged adopt sand filter to filter, and it is neutral that the clear liquid pH value reaches.
The present invention has following good effect:
(1) adopt method of the present invention and for using the equipment of the method specialized designs, it is very remarkable to process papermaking industry black digestion liquid effect, CODcrClearance can reach 60～85% to the unit single treatment, reaches State Bureau of Environmental Protection, Ministry of Light Industry, the Ministry of Finance, State Scientific and Technological Commission and issues the index request that paper plant's black liquor treatment BOD, COD descend before nineteen ninety-five in " regulation of polluting about control paper industry water " jointly. Table one is the purifying black liquor effect in paper mill (take bagasse as raw material, use kraft cooking black liquor).
Table one:
The analysis data of raw black liquid and parting liquid provide by environmental protection supervision center, Foshan City in the table one.
(2) higher through the isolated lignin purity of seperator of the present invention, table two is the chemical composition of lignin material.
Table two:
| Analysis project | Content (%) |
| Lignin | 79.40 |
| The pentose class | 12.14 |
| Ash | 6.64 |
The plain material of shown in the table two this kind of purer initial wood mass is for the lignin product of making senior high value provides favourable condition.
(3) the present device floor space is little, technological operation is simple, realized entering continuously black liquor, continuous separating lignin and discharged continuously the target that clear liquid is turned harm into good, and the equipment investment expense is few, has the actuality of operation.
Claims (3)
1, is applicable to the technology of lignin separation, purification paper industry black digestion liquid, it is characterized in that the molten gas of black liquor, acid out and dissolved air flotation are combined in same system, and employing comprises the process of following four steps: the preliminary treatment of (1) paper industry black digestion liquid, (2) flocculation of lignin with separate, (3) dehydration of lignin, (4) post processing of parting liquid etc., its corresponding manufacturing condition is as follows:
(1) preliminary treatment of paper industry black digestion liquid: with full black liquor air soluble method
(1) the black liquid consistency adjustable range is 0.2 ' Be (Baume)～9, Be (Baume);
(2) operating pressure of preliminary treatment jar is 2～4kg/cm
2
(3) to enter the flow of preliminary treatment jar be 0.5m to black liquor
3/ hr～80m
3/ hr;
(4) time of staying of black liquor in the preliminary treatment jar is 3～30 minutes.
(2) flocculation of lignin with separate: with acid out flocculation and dissolved air flotation method;
(1) pH value that enters the black liquor of flocculation zone behind the molten gas of preliminary treatment jar is 8～14, mixes with the acid of introducing, and its pH value is adjusted to PH=2～4;
(2) black liquor is 5～30 minutes in the flocculation zone time of staying, in the time of staying of Disengagement zone is 20～100 minutes, with the linear velocity of 0.2～12cm/min come-up, the S shape scraper plate that is being rotated to the seperator top that floats is scraped in the lignin chute in lignin separator.
(3) lignin dehydration: use the thermal dehydration method
The lignin material that separates is heated to 70～90 ℃ fully separates out free waters a large amount of in the lignin.
(4) post processing of parting liquid: adjust pH value with the sand filtration method
Sand filter filters, and sand that sand filter adopts is the sand formula quartz sand of making detailed inquiries.
2, lignin separation according to claim 1, purifying technique for black liquor, it is characterized in that regulating the used acid of black liquor pH value that enters flocculation zone is that concentration is the 10%(percentage by weight) above sulfuric acid or hydrochloric acid or nitric acid or industrial waste acid; Its consumption is 0.5～4%(percentage by weight of processed black liquor).
3, for adopting lignin separation, the custom-designed lignin separator system equipment of purifying technique for black liquor, it is characterized in that:
(1) the preliminary treatment jar is to be hemispherical by two ends, the middle pressure vessel that is formed by connecting for columniform device, and its blade diameter length ratio is 5.5: 1～3: 1;
(2) lignin separator is made of flocculation zone and Disengagement zone, flocculation zone central authorities are provided with black liquor import (2) and acid solution import (3) and connect the blender (1) that communicates, the top of Disengagement zone is lignin outlet (5), top in lignin outlet (5), be provided with S shape scraper plate (4), above the seperator shell, be provided with lignin chute with a slope (6) along last round platform periphery, the bottom, Disengagement zone of interior rounding platform (8) periphery is provided with discharge channel (7).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90107652 CN1050241A (en) | 1990-09-08 | 1990-09-08 | Lignin separator and purifying technique for black liquor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90107652 CN1050241A (en) | 1990-09-08 | 1990-09-08 | Lignin separator and purifying technique for black liquor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1050241A true CN1050241A (en) | 1991-03-27 |
Family
ID=4880651
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 90107652 Pending CN1050241A (en) | 1990-09-08 | 1990-09-08 | Lignin separator and purifying technique for black liquor |
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| Country | Link |
|---|---|
| CN (1) | CN1050241A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102220135A (en) * | 2011-05-31 | 2011-10-19 | 苏州大学 | Leaching liquid for repairing organic phenol-contaminated soil and reparation method of organic phenol-contaminated soil |
| CN102277391A (en) * | 2011-08-25 | 2011-12-14 | 温志明 | Comprehensive utilization method of straw raw materials |
| CN102425075A (en) * | 2011-12-06 | 2012-04-25 | 南京大学 | Device and method for extracting and separating lignin in papermaking black liquor |
| CN102730876A (en) * | 2011-04-14 | 2012-10-17 | 富阳市清园城市综合污水处理有限公司 | Advanced treatment process for papermaking wastewater |
| CN105152458A (en) * | 2015-07-18 | 2015-12-16 | 常州大学 | Method for separating and recovering lignin in paper-making wastewater |
| CN105268461A (en) * | 2015-11-04 | 2016-01-27 | 高大元 | Method for recovering lignin from straw pulp black liquid to prepare lignin carbon carrier catalyst |
| CN106794425A (en) * | 2014-10-03 | 2017-05-31 | 斯道拉恩索公司 | Undergo the method that electric field purifies lignin by making the slurry containing lignin |
| CN108951252A (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 soda pulping cooking liquor |
-
1990
- 1990-09-08 CN CN 90107652 patent/CN1050241A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102730876A (en) * | 2011-04-14 | 2012-10-17 | 富阳市清园城市综合污水处理有限公司 | Advanced treatment process for papermaking wastewater |
| CN102730876B (en) * | 2011-04-14 | 2014-01-15 | 富阳市清园城市综合污水处理有限公司 | Advanced treatment process for papermaking wastewater |
| CN102220135A (en) * | 2011-05-31 | 2011-10-19 | 苏州大学 | Leaching liquid for repairing organic phenol-contaminated soil and reparation method of organic phenol-contaminated soil |
| CN102220135B (en) * | 2011-05-31 | 2013-04-24 | 苏州大学 | Leaching liquid for repairing organic phenol-contaminated soil and reparation method of organic phenol-contaminated soil |
| CN102277391A (en) * | 2011-08-25 | 2011-12-14 | 温志明 | Comprehensive utilization method of straw raw materials |
| CN102277391B (en) * | 2011-08-25 | 2014-04-16 | 温志明 | Comprehensive utilization method of straw raw materials |
| CN102425075A (en) * | 2011-12-06 | 2012-04-25 | 南京大学 | Device and method for extracting and separating lignin in papermaking black liquor |
| CN102425075B (en) * | 2011-12-06 | 2013-10-09 | 南京大学 | Device and method for extracting and separating lignin in papermaking black liquor |
| CN106794425A (en) * | 2014-10-03 | 2017-05-31 | 斯道拉恩索公司 | Undergo the method that electric field purifies lignin by making the slurry containing lignin |
| CN105152458A (en) * | 2015-07-18 | 2015-12-16 | 常州大学 | Method for separating and recovering lignin in paper-making wastewater |
| CN105268461A (en) * | 2015-11-04 | 2016-01-27 | 高大元 | Method for recovering lignin from straw pulp black liquid to prepare lignin carbon carrier catalyst |
| CN108951252A (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 soda pulping cooking liquor |
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