CN1262359A - Cyclic process for treating black paper-making liquid of alkali pulping to recover useful resource - Google Patents
Cyclic process for treating black paper-making liquid of alkali pulping to recover useful resource Download PDFInfo
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- CN1262359A CN1262359A CN 00103238 CN00103238A CN1262359A CN 1262359 A CN1262359 A CN 1262359A CN 00103238 CN00103238 CN 00103238 CN 00103238 A CN00103238 A CN 00103238A CN 1262359 A CN1262359 A CN 1262359A
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Abstract
A cyclic process for treating the black paper-making liquid of alkali pulping to recover useful resource include such steps as regulating concentration of black liquid, feeding the fume generated by calcining sulfur or troilite or from flue, or liquefied SO2 into system, reaction on black liquid to generate acidifying agent, separating lignin, regulating filtrate with sodium hydroxide and/or sodium carbonate for returning it back to pulping step, preparing lignin sulfonate with recovered liquid, and recovering acidifying agent as pulping chemical and being transformed into lignin sulfonate component. Its advantages are less investment, low cost and high properties of recovered substances.
Description
The invention provides a kind of process of black paper-making liquid of alkali pulping benign cycle recycling treatment.20,000 tons/year of suitable especially slurrying production scale less thaies, grass fiber raw material paper mill black liquor are handled.Subordinate environmental pollution treatment technology of the present invention field.
The pulping back liquor discharging causes serious environmental to pollute, its main cause is that the fibrous raw material utilization rate is low, account for industrial chemicals and the industrial water formation high consistency pulping black liquor such as alkali that add in lignin, hemicellulose and the pulping process of fibrous raw material amount about 50%, enter environment, both form serious environmental and polluted, caused a large amount of wastings of resources simultaneously.
At present, the processing method of black paper-making liquid of alkali pulping mainly comprises: alkali recycling method, flocculation sediment facture, evaporation concentration method, anaerobic bio-treated method etc.
Silvola recovery abroad is the pulping and paper-making factory of raw material with timber, pollutional load is accounted for pulping and paper-making produce the method that the processing of the black digestion liquid of total emission volumn about 90% adopts alkali to reclaim more.Big at China's alkali recovery technology to scale, be that the solution of soda pulping process factory black liquor pollution problem of raw material is respond well with timber.But to numerous be that the pulping and paper-making factory black liquor pollution of raw material, scale deficiency is administered with the grass fiber, be difficult to the effect that reaches desirable.Grass fiber raw pulp black liquor silicone content height, viscosity are big, are difficult to it is concentrated to the concentration requirement that is fit to the alkali recovery furnace burning; The straw pulp black liquor calorific value is low than wood pulp, usually needs to add auxiliary fuel such as heavy oil etc. and could guarantee the alkali recovery furnace normal combustion, increases the cost that reclaims alkali greatly.In addition, to the paper mill of slurrying small scale, there is not abundant black liquor to move continuously for alkali recovery furnace.Huge investment makes alkali recovery technology be expected unreachable to the not strong numerous paper mills genus of financial strength.
This method of flocculent precipitation is primarily aimed at pulping and paper-making factory comprehensive wastewater and adopts flocculation, precipitation, filtration, method of separating deposit to handle.The later waste liquid of sediment separate out carries out advanced treating through anaerobic biological process again.Contaminated wastewater after processing load obviously descends, part reuse or all dischargings, but be difficult to the processing target that reaches desirable.These class methods are handled the high consistency pulping black liquor and are not suitable for, and construction investment and operating cost are higher.In the sediment of separating, the flocculant that component of effluent and processing procedure add etc. mixes, and complicated component is difficult to effectively be utilized, and does not reach the purpose that resource reclaims, utilizes.
This method of evaporation concentration method directly is concentrated to certain concentration with black liquor of pulp making earlier, carries out drying and dehydrating again and makes black powder.This method only by concentrate, seasoning removes black liquor moisture, both needed large-area evaporimeter and more energy consumption, the intensity of drying and dehydrating is also big, causes that equipment investment is big, energy consumption is high.Simultaneously, black liquor composition non-modified, whole organic and inorganic thing component packings wherein, complicated component, using value is little.
The pulping back liquor processing method that patent of invention 89106694.2 provides, the lignin purity height of recovery, steady quality have good application foundation.But, reclaiming the later liquid of lignin and further reclaim sodium sulfite, process conditions and equipment require high, and the sodium sulfite elaboration rate of recovery is low, cost is high, and economic benefit of engineering is poor.
The lime process pulping black liquor that the suitable boiling degree of this method of anaerobic biological process is lower is handled.With burning subtract, vulcanized sodium, sodium sulfite be the black liquor that produces of main medicament slurrying than lime method black liquid consistency height, lignin etc. are difficult to a large amount of existence of degradable chemical, make anaerobic process COD clearance low as counterfeit substrate.The salinity of higher concentration such as silicon, (Asia) sulfate, sodium etc. produce serious inhibitory action to biologically active in the black liquor.Waste water behind the producing methane also need carry out advanced treating just may be up to standard, and the mud value of generation is low.Low temperature makes anaerobic fermentation system biologically active difference and has a strong impact on treatment effect.The northern area that the long-term temperature of China is lower is difficult to make anaerobic fermentation system to remain on the temperature levels of suitable (middle temperature 35-40 ℃, high temperature 52-55 ℃).This method limitation is big.
The objective of the invention is to effectively administer black liquor of pulp making and pollute, simultaneously black liquor solid and moisture are all changed into form recovery, the reuse of product and reuse liquid.After the feedstock conversion of using in the processing procedure is back to slurrying production as pulp-making agent, further become the active principle of regenerant.The present invention is fit to the processing of various scales, multiple fibrous raw material black paper-making liquid of alkali pulping, and technology is brief, construction investment is economized, processing cost is low, and adaptability is strong.The regenerant application performance is good, and the liquid reuse is effective.The treatment mechanism of black liquor processing of setting up and recovery, reuse good combination is the important foundation that the present invention has good benefits in environment and economic benefit.Can realize that black liquor pollution is administered thoroughly, resource reclaims sufficient double goal.
The present invention's purpose realizes as follows:
1. alkaline pulping black liquor extracts lignin
Regulating alkaline pulping black liquor concentration is Be ° of 1-13 (20 ℃), with SO
2Introduce treatment system, generate the sulfurous acid acidulant with the black liquor reaction of moisture.Black liquor is acidified to pH2-5.5 and separates out lignin.With liquid heat, insulation, make lignin coacervation precipitation and filter to isolate lignin.
2. filtrate is transferred alkali system reuse liquid
Liquid behind the separating lignin with solid or liquid sodium hydroxide or (with) sodium carbonate regulates the pH value, acidulant is transformed into the main component of pulp-making agent, liquid becomes reuse liquid.
3. the white liquid reuse of synthetic paper-pulp production slurrying is produced
Reuse liquid is synthesized neutrality or the white liquid of alkaline sulfite pulp production, be back to slurrying production.
4. gained reclaims liquid through modulation, concentrated, the dry product lignosulfonates that obtain after the reuse slurrying.
Wood invented technology flow chart is seen accompanying drawing.Cyclic process for treating black paper-making liquid of alkali pulping to recover useful resource embodiment is as follows:
Embodiment 1
Alkaline pulping black liquor 50kg is adjusted to Be ° of 4 (20 ℃), and acidifying makes liquid pH2.5 separate out lignin.Be heated to 65 ℃ of temperature, insulation coacervation 3.0 hours, isolated by filtration solid lignin.Liquid behind the separating lignin is adjusted to pH12 with NaOH and sodium carbonate becomes slurrying reuse liquid.Slurrying reuse liquid is transferred to effective alkali 16%, sulfiting degree 0.4, be back to pulping and paper-making.Gained reuse liquid through modulation, concentrate, drying becomes lignosulfonates.
Embodiment 2-5 treatment step is with embodiment 1, and implementation condition is listed in table 1.
Table 1. embodiment 1-5 implementation condition
| Embodiment NO. | Black liquor | Acidifying pH | Reaction | Liquid is transferred pH | Reuse liquid | |||
| ????Kg | ???Be·(20℃) | ??℃ | ??h | Effective alkali | The sulfiting degree | |||
| ????1 | ????45 | ????4.0 | ??2.5 | ??65 | ??3.0 | ??12 | ??16 | ????0.4 |
| ????2 | ????50 | ????6.5 | ??4.0 | ??80 | ??2.0 | ??10 | ??12 | ????0.6 |
| ????3 | ????50 | ????7.0 | ??3.5 | ??90 | ??1.5 | ??9.0 | ??14 | ????0.6 |
| ????4 | ????55 | ????3.0 | ??3.6 | ??85 | ??2.5 | ??9.5 | ??15 | ????0.8 |
| ????5 | ????30 | ????10.5 | ??3.5 | ?75 | ??2.5 | ??8.5 | ??9 | ????0.45 |
Table 2. embodiment experimental result
| ??NO. | Project | Index | ??NO. | Project | Index |
| ??1 | The lignin yield | ??0.7-2.8％ | ??5 | Unscreened yield | ??54-67％ |
| ??2 | Reuse liquid reclamation rate | ??100％ | ??6 | Screened yield | ??42-53％ |
| ??3 | The lignosulphonates yield | ??4-18.5％ | ??7 | Become the lateral lattice | ??60-80g/m 2 |
| ??4 | Lignin purity | ??80-85％ | ??8 | Become the paper whiteness | The 70-85 degree |
Claims (7)
1. cyclic process for treating black paper-making liquid of alkali pulping to recover useful resource is that the black liquor that produces with alkaline process, neutrality, alkaline sulfite legal system slurry is handled, and recovery, reuse black liquor solid and slurrying industrial water also reclaim the raw material that uses in the black liquor processing procedure.The invention is characterized in and may further comprise the steps:
Alkaline pulping black liquor extracts lignin
Filtrate is transferred alkali system reuse liquid
The white liquid reuse of synthetic paper-pulp production slurrying is produced
Gained reclaims liquid and makes lignosulfonates through modulate, concentrate, drying etc. after the reuse slurrying.
2. cyclic process for treating black paper-making liquid of alkali pulping to recover useful resource as claimed in claim 1 is characterized in that used acidulant is to burn sulphur or roasting pyrite or flue gas or liquefaction SO
2The sulfurous acid that generates with reaction of moisture in the black liquor.
3. cyclic process for treating black paper-making liquid of alkali pulping to recover useful resource as claimed in claim 1, the concentration that it is characterized in that handling black liquor is Be ° of 1-13 (20 ℃), black liquor acidifying pH value is 2-5.5, and precipitate coacervation temperature is 40-90 ℃, and the liquid temperature retention time is 1/3-5 hour.
4. cyclic process for treating black paper-making liquid of alkali pulping to recover useful resource as claimed in claim 1 is characterized in that the medicine component sodium sulfite in the slurrying reuse liquid is synthetic with black liquor of pulp making extraction lignin acidulant employed.
5. cyclic process for treating black paper-making liquid of alkali pulping to recover useful resource as claimed in claim 1, it is characterized in that behind the separating lignin liquid with NaOH or (with) sodium carbonate is modulated into the slurrying reuse liquid of pH7-14.Concentration with the white liquid of pulp production of reuse liquid modulation is effective alkali 8-16%, sulfiting degree 0.4-0.85.
6. cyclic process for treating black paper-making liquid of alkali pulping to recover useful resource as claimed in claim 1, the sulfonating agent that it is characterized in that preparing lignosulfonates are to extract the used acidulant of lignin with black liquor of pulp making to be transformed.
7. cyclic process for treating black paper-making liquid of alkali pulping to recover useful resource as claimed in claim 1 is characterized in that acidulant reclaims and the lignin sulfonation is finished in digestion process.
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| CN00103238A CN1087045C (en) | 2000-03-17 | 2000-03-17 | Cyclic process for treating black paper-making liquid of alkali pulping to recover useful resource |
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| CN00103238A CN1087045C (en) | 2000-03-17 | 2000-03-17 | Cyclic process for treating black paper-making liquid of alkali pulping to recover useful resource |
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| CN1087045C CN1087045C (en) | 2002-07-03 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102140261A (en) * | 2011-01-18 | 2011-08-03 | 延边石岘白麓纸业股份有限公司 | Method for preparing dye dispersing agent based on sulfite pulping waste liquid and dye combination |
| 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 |
| CN103665390A (en) * | 2012-09-25 | 2014-03-26 | 潘增强 | Method for extracting sodium lignin sulfonate from papermaking black liquor employing sulphur treatment |
| CN103819687A (en) * | 2014-03-21 | 2014-05-28 | 河南省科学院化学研究所有限公司 | Method for producing sodium lignin sulfonate by using high-sulfur coal |
| CN112169753A (en) * | 2020-09-21 | 2021-01-05 | 张家港市杨舍丝印工艺厂 | Heavy metal adsorbent and preparation process thereof |
| CN112708144A (en) * | 2020-11-30 | 2021-04-27 | 山东华泰纸业股份有限公司 | Method for producing lignin by using sulfur mud |
| CN116590945A (en) * | 2023-03-02 | 2023-08-15 | 广西大学 | Pulping method for improving pulp yield by circularly steaming fiber raw materials through black liquor acidification filtrate |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1037183A (en) * | 1988-04-19 | 1989-11-15 | 四川农业大学 | The sulfate process black liquid is handled in Chemical Decomposition |
| CN1017077B (en) * | 1989-09-04 | 1992-06-17 | 中国科学院环境评价部 | Acidifying process of paper black liquid with sulphur dioxide |
| SE465039B (en) * | 1989-11-23 | 1991-07-15 | Chemrec Ab | MADE TO MAKE SUBSTANCES WITH HIGH SULFIDITY BEFORE SULFAT PREPARATION |
| CN1030537C (en) * | 1990-11-21 | 1995-12-20 | 何柱生 | Non-pollution technology for comprehensive utilization of alkaline straw-pulp black liquid |
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2000
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102140261A (en) * | 2011-01-18 | 2011-08-03 | 延边石岘白麓纸业股份有限公司 | Method for preparing dye dispersing agent based on sulfite pulping waste liquid and dye combination |
| 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 |
| CN103665390A (en) * | 2012-09-25 | 2014-03-26 | 潘增强 | Method for extracting sodium lignin sulfonate from papermaking black liquor employing sulphur treatment |
| CN103819687A (en) * | 2014-03-21 | 2014-05-28 | 河南省科学院化学研究所有限公司 | Method for producing sodium lignin sulfonate by using high-sulfur coal |
| CN112169753A (en) * | 2020-09-21 | 2021-01-05 | 张家港市杨舍丝印工艺厂 | Heavy metal adsorbent and preparation process thereof |
| CN112169753B (en) * | 2020-09-21 | 2023-08-29 | 北京伟创力科技股份有限公司 | Heavy metal adsorbent and preparation process thereof |
| CN112708144A (en) * | 2020-11-30 | 2021-04-27 | 山东华泰纸业股份有限公司 | Method for producing lignin by using sulfur mud |
| CN116590945A (en) * | 2023-03-02 | 2023-08-15 | 广西大学 | Pulping method for improving pulp yield by circularly steaming fiber raw materials through black liquor acidification filtrate |
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| CN1087045C (en) | 2002-07-03 |
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