CN102635011B - Recycling comprehensive utilization technology for pulping black liquor or red liquor - Google Patents
Recycling comprehensive utilization technology for pulping black liquor or red liquor Download PDFInfo
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- CN102635011B CN102635011B CN 201210106232 CN201210106232A CN102635011B CN 102635011 B CN102635011 B CN 102635011B CN 201210106232 CN201210106232 CN 201210106232 CN 201210106232 A CN201210106232 A CN 201210106232A CN 102635011 B CN102635011 B CN 102635011B
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- black liquor
- red liquid
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- sludge cake
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Abstract
The invention belongs to the field of paper-making pulping and relates to a recycling comprehensive utilization technology for pulping black liquor or red liquor. The recycling comprehensive utilization technology is characterized by comprising the following steps in turn: pre-treating; dehydrating (reusing water after being treated); treating a sludge cake; burdening; pre-forming; forming; polishing; trimming; and forming an end product of a building material. According to the invention, solid and water in the black liquor or red liquor are separated by adopting a compound flocculation technology; after the separated water is treated, the water is reused for pulping; the separated solid is used for producing the building material, so that the environmental pollution caused by the black liquor or red liquor is thoroughly eliminated and a large amount of water for production is saved; the treating cost of the black liquor or red liquor is low; the equipment investment is less; the produced building material belongs to the comprehensive utilization of wastes; and the economic benefit is increased.
Description
Technical field
The invention belongs to the paper-making pulping field, the circulation comprehensive that is specifically related to black liquor of pulp making or red liquid utilizes technique.
Background technology
Black liquor, the waste liquid of gained is dark brown after the soda pulping process boiling, is called black liquor.Inorganic matter comprises free NaOH, sodium metasilicate, sodium thiosulfate, vulcanized sodium, sodium sulfite, sodium carbonate etc. in the black liquor.Organic matter in the black liquor comprises the phenol organic matter of alkali lignin, sulfuration lignin, VFA, other modified lignin and trace etc.Black liquor directly enters rivers and can pollute, and should process.Processing method is first evaporation and concentration, again through burning, recyclable alkali.
Red liquid, the waste liquid of gained is brownish red after the sulfite pulping boiling, is called red liquid.Organic matter in the red liquid mainly is lignosulfonates, also contains carbohydrate, organic acid, volatile acid, resin, pigment etc.Inorganic matter in the red liquid is mainly the materials such as sodium sulphate, vulcanized sodium, silica, magnesia, and directly discharging can cause public hazards, should recycle.General recovery and treatment method is: with red liquid evaporation and concentration (solid matter content reaches 50%～60%), spray in the combustion furnace and burn, generate sulfur dioxide, magnesia, soda ash etc.
Black (red) liquid burning absorption method is adopted in the at present processing of black (red) liquid of slurrying both at home and abroad basically.There is following shortcoming in the method:
One, complex process.
Existing black (red) liquid is processed by black (red) liquid and is extracted, black (red) liquid preliminary treatment, black (red) liquid evaporation enrichment, black (red) liquid burning, reclaims heat energy and the technical process such as the cooking liquor of regenerating are finished.
Its two, black (red) liquid treatment facility investment is large.
Existing black (red) liquid treatment facility investment accounts for paper-making pulping gross investment 1/3rd.
Its three, cause secondary pollution.
Existing black (red) liquid produces a large amount of pernicious gases such as H in combustion process
2S etc. cause serious secondary pollution to air.
Its four, intractability is large.
At present the waste liquid that discharges every year of China's paper-making pulping reaches 40.77 hundred million m
3, COD content reaches 128.8 ten thousand tons in the waste water, accounts for 31.82% of COD in the national waste water, and black (red) liquid in the waste liquid accounts for 1,000,000,000 m
3, wherein solid content about 13%, about 1.3 hundred million tons of every annual.
This shows that the treatment technology technique of black (red) liquid of existing slurrying falls behind, investment is large, complex process, causes secondary pollution, waste large water gaging and sludge resource and (produce 1.3 hundred million tons of dewatered sludges every year and consume 39.47 hundred million m
3Water), disposal cost is high.
Summary of the invention
For existing black liquor of pulp making or the existing problem of red liquor treating process, the new technology of a kind of black liquor or the comprehensive utilization capable of circulation of red liquid is proposed, utilize the composite flocculation technology make solid content in black liquor or the red liquid and moisture from.The water of separating is supplied with after treatment slurrying and is recycled, and the solid content of separating is for the production of building materials, thereby thoroughly eradicated the pollution that black liquor of pulp making or red liquid cause environment, and save a large amount of industrial waters, black liquor or red liquid processing cost are low, equipment investment is few, and the building materials of producing belong to comprehensive utilization of waste materials, have increased economic benefit.
Technical scheme of the present invention is:
Black liquor of pulp making or red liquid can be divided into four-stage " black liquor or red liquid flocculation dewatering " " remaining water treatment " " grass meal preparation " " building materials moulding ", and accompanying drawing 1 is seen in the technological process that black liquor of pulp making or red liquid are processed.
The treatment formulations of black liquor of pulp making or red liquid:
Flocculant: the cationic polyacrylamide graft starch, be called for short the CPAM graft starch
Oxidant: peroxosulphuric (H
2SO
5), peroxide calcium carbonate (2CaCO
33H
2O
2)
Chelating agent: diethylene triamine pentamethylene phosphonic, be called for short DTPMPA
Neutralizer: H
2SO
4Ca (OH)
2CaCO
3
Adhesive: polyvinyl alcohol graft copolymerized starch (PVA graft starch), isocyanates-5(MDI-5)
The circulation comprehensive of a kind of black liquor of pulp making or red liquid utilizes technique, may further comprise the steps:
Preliminary treatment: in black liquor or red liquid, add the cationic polyacrylamide graft starch as flocculant, consumption is the 2%-3% of black liquor or red liquid quality, stir after 8-15 minute, add again oxidant, consumption is the 2%-5% of black liquor or red liquid quality, stirred 8-15 minute, and made the solid content flocculation, get pretreatment fluid; The oxidant that adds in the described black liquor is peroxosulphuric; The oxidant that adds in the described red liquid is peroxide calcium carbonate;
Dehydration: above-mentioned pretreatment fluid is sent in the filter pressing dehydrator, made the solid content press filtration in the pretreatment fluid become sludge cake, sludge cake moisture content 60%-70%, the water of deviating from is sent into water treating pond;
Water treatment: add neutralizer and transfer pH to 6.5-7.5 in water treating pond, add the chelating agent diethylene triamine pentamethylene phosphonic again, consumption is the 0.1%-0.2% of the quality of deviating from, and the water confession slurrying after the processing recycles; The neutralizer that adds in the described black liquor is calcium carbonate; The neutralizer that adds in the described red liquid is sulfuric acid;
Sludge cake is processed: add neutralizer and stir in sludge cake, transfer pH to 6.5-7.5, get the sludge cake after the neutralization; The neutralizer that adds in the described black liquor is calcium hydroxide; The neutralizer that adds in the described red liquid is sulfuric acid;
The grass meal preparation: non-wood type string is pulverized, and crossing sieve diameter is the 3mm-6mm sieve plate, gets grass meal;
Batching: grass meal is dropped in the mixer, add polyvinyl alcohol graft copolymerized starch, consumption is the 8%-12% of grass meal over dry quality, stirs evenly, and adds isocyanates-5 again, and consumption is the 4%-8% of grass meal over dry quality, stirs evenly, and adds at last the sludge cake after neutralizing; The over dry mass ratio of the sludge cake after the neutralization and grass meal is 1:0.8-1.2, stirs evenly, and gets compound;
Preformed: usefulness preformed spreading machine by product specification requirement preformed, gets preform with compound;
Moulding: on the building materials heat pressing forming machines preform is carried out thermocompression forming, pressure is 0.8 MPa-1.2MPa, and temperature is 105 ℃-115 ℃, and the time is pressed building materials THICKNESS CALCULATION 0.8 min/mm-1.2min/mm, the material of must finalizing the design.
Then the building materials finished product polishes above-mentioned typing material and cuts edge after processing to get.
The flocculant consumption is preferably the 2.5%-3% of black liquor or red liquid quality in the described preprocessing process, and the oxidant consumption is preferably the 3%-3.5% of black liquor or red liquid quality.
During processing, described water treatment and sludge cake transfer pH to be preferably 7.
Polyvinyl alcohol graft copolymerized starch consumption is preferably 10% of grass meal over dry quality in the described blending process; Isocyanates-5 consumption is preferably 6% of grass meal over dry quality; The over dry mass ratio of the sludge cake after the neutralization and grass meal is preferably 1:1.
The pressure of thermocompression forming is preferably 1.0MPa in the described forming process, and temperature is preferably 110 ℃, and the time is preferably 1min/mm by the building materials THICKNESS CALCULATION.
Non-wood type string in the described grass meal preparation is preferably selected from straw, kaoliang stalk, wheat straw, cornstalk, reed or bagasse.
Below the present invention will be further explained and the explanation:
Principle of the present invention is: the present invention utilize the composite flocculation technology make solid content in black liquor or the red liquid and moisture from, then carry out subsequent treatment:
In preprocessing process:
For the black liquor of soda pulping process, H
2SO
5In organic matter and inorganic matter in the unnecessary oxygen atom oxidation solid content, eliminate its chemism, make it stable in properties, and H
2SO
5In H
2SO
4The nuisances such as catechol, talan are carried out sulfonated processing, and its however, residual base that neutralizes, the water material is separated, get black liquor pretreatment liquid.
For the red liquid of acid polishing, 2CaCO
33H
2O
2In H
2O
2Organic matter and inorganic matter in the oxidation solid content are eliminated its chemism, make it stable in properties, and 2CaCO
33H
2O
2In CaCO
3The neutralize acidity of red liquid makes solid content carry out the sedimentation flocculation simultaneously, and the water material separates, and gets red liquid pretreatment fluid.
In the sludge cake processing procedure:
Sludge cake after the dehydration is sent in the rustless steel container of belt stirrer.For the black liquor sludge cake, its PH3 adds Ca (OH)
2In and the acidity of sludge cake, be adjusted to pH7, make simultaneously Sulfonated poisonous benzene, aldehydes matter further be combined to the nontoxic materials such as paratoluenesulfonic acid sodium salt, thereby eliminated the harmful substance in the sludge cake.For the sludge cake of red liquid, its pH9 then adds H
2SO
4Neutralize, be adjusted to PH7.Because CaCO
3, H
2SO
4, Ca (OH)
2, H
2O
2Acting in conjunction, eliminated the noxious material in black (red) liquid, make the sludge cake become nontoxic raw material.
Compared with prior art, advantage of the present invention is:
1, the present invention proposes the New Process for Treatment of black (red) liquid of a cover slurrying through the more than ten years theory and practice, has thoroughly eliminated the pollution that black (red) liquid of slurrying causes environment.
2, the equipment investment processed of black (red) liquid of slurrying is few, only be equivalent to the current device investment pact half.
3, save great lot of water resources, annually after deceiving (red) liquid water treatment, can provide slurrying with about 6.3 hundred million m of recirculated water
3
4, provide 1.3 hundred million tons of building materials raw materials.
5, increase by 2.6 hundred million tons of the useless comprehensive utilization of environment-friendly type building materials, by 1500 yuan/tons, annual income reaches 3,900 hundred million yuan.
Description of drawings
Fig. 1 is the process chart that black liquor of pulp making of the present invention or red liquid are processed.
The specific embodiment
The present invention will be further explained and explanation below in conjunction with specific embodiment.Consumption described in the embodiment all refers to the quality consumption.
Embodiment 1: the processing of black liquor
Take northeast, paper mill, Yueyang Korean pine soda pulping process as example, its black liquor is realized the comprehensive utilization processing through following technique.
Preliminary treatment: in black liquor pond (band low-speed agitator), add the CPAM graft starch, consumption is 2.5% of black liquor amount, and stirring at low speed adds H after 10 minutes again
2SO
5, consumption is 3% of black liquor amount, stirring at low speed 10 minutes makes the solid content flocculation in the black liquor, gets pretreatment fluid.
Dehydration: pretreatment fluid is sent among the filter pressing dehydrator ZQWY-50, made the solid content press filtration of having flocculated in the pretreatment fluid become sludge cake, the water of deviating from is sent into water treating pond.
Water treatment: in water treating pond, add CaCO
3Be adjusted to pH7, add chelating agent DTPMPA again, consumption is 0.1% of the water yield, and the water after the processing recycles for slurrying, and merges with sludge cake after the sludge collection.
Sludge cake is processed: sludge cake is sent in the rustless steel container of belt stirrer, added Ca (OH)
2Be adjusted to pH7, for subsequent use.
The grass meal preparation: with beater disintegrating machine 9FQ40-20 non-wood type string is pulverized, crossed diameter and be the sieve plate of 4mm, for subsequent use.
Batching: grass meal is dropped in the mixer, add PVA graft starch glue, consumption is that the 10%(grass meal of grass meal is by oven-dry weight), stir evenly, add again MDI-50, consumption is 6% of grass meal, (grass meal is by oven-dry weight) stirs evenly, and adds at last sludge cake.Sludge cake (over dry): grass meal (over dry)=1:1, stir evenly, get compound.
Preformed: usefulness preformed spreading machine by product specification requirement preformed, gets preform with compound.
Moulding: on the building materials heat pressing forming machines preform is carried out thermocompression forming, pressure is 1.0MPa, and temperature is 110 ℃ ± 3 ℃, and the time is pressed the building materials THICKNESS CALCULATION, 1min/mm, the material of must finalizing the design.
Polish: will finalize the design with polishing machine and expect surface finish, and get polishing material.
Cut edge: neat with cutting around the polishing material with bead cutter, get the building materials finished product.
Embodiment 2: the processing of red liquid
Take Yueyang Co., Ltd of good luck paper technology research institute sulfite pulping as example, its red liquid is realized the comprehensive utilization processing through following technique.
Preliminary treatment: in red liquid pool (band low-speed agitator), add the CPAM graft starch, consumption is 3% of black liquor amount, and stirring at low speed adds 2CaCO after 10 minutes again
33H
2O
2, consumption is 3.5% of black liquor amount, stirring at low speed 10 minutes makes the solid content flocculation in the black liquor, gets pretreatment fluid.
Dehydration: pretreatment fluid is sent among the filter pressing dehydrator ZQWY-50, made the solid content press filtration of having flocculated in the pretreatment fluid become sludge cake, the water of deviating from is sent into water treating pond.
Water treatment: in water treating pond, add sulfuric acid and be adjusted to pH7, add chelating agent DTPMPA again, consumption is 0.1% of the water yield, and the water after the processing recycles for slurrying, and merges with sludge cake after the sludge collection.
Sludge cake is processed: sludge cake sent in the rustless steel container of belt stirrer, added sulfuric acid and be adjusted to pH7, and for subsequent use.
The grass meal preparation: usefulness beater disintegrating machine 9FQ40-20 pulverizes non-wood type string, and the mistake diameter is that the sieve plate of 4mm is for subsequent use.
Batching: grass meal is dropped in the mixer, add PVA graft starch glue, consumption is that the 10%(grass meal of grass meal is by oven-dry weight), stir evenly, add again MDI-50, consumption is 6% of grass meal, (grass meal is by oven-dry weight) stirs evenly, and adds at last sludge cake.Sludge cake (over dry): grass meal (over dry)=1:1, stir evenly, get compound.
Preformed: usefulness preformed spreading machine by product specification requirement preformed, gets preform with compound.
Moulding: on the building materials heat pressing forming machines preform is carried out thermocompression forming, pressure is 1.0MPa, and temperature is 110 ℃ ± 3 ℃, and the time is pressed the building materials THICKNESS CALCULATION, 1min/mm, the material of must finalizing the design.
Polish: will finalize the design with polishing machine and expect surface finish, and get polishing material.
Cut edge: neat with cutting around the polishing material with bead cutter, get the building materials finished product.
Claims (7)
1. the circulation comprehensive of a black liquor of pulp making or red liquid utilizes technique, it is characterized in that, may further comprise the steps:
Preliminary treatment: in black liquor or red liquid, add the cationic polyacrylamide graft starch as flocculant, consumption is the 2%-3% of black liquor or red liquid quality, stir after 8-15 minute, add again oxidant, consumption is the 2%-5% of black liquor or red liquid quality, stirred 8-15 minute, and made the solid content flocculation, get pretreatment fluid; The oxidant that adds in the described black liquor is peroxosulphuric; The oxidant that adds in the described red liquid is peroxide calcium carbonate;
Dehydration: above-mentioned pretreatment fluid is sent in the filter pressing dehydrator, made the solid content press filtration in the pretreatment fluid become sludge cake, sludge cake moisture content 60%-70%, the water of deviating from is sent into water treating pond;
Water treatment: add neutralizer and transfer pH to 6.5-7.5 in water treating pond, add the chelating agent diethylene triamine pentamethylene phosphonic again, consumption is the 0.1%-0.2% of the quality of deviating from, and the water confession slurrying after the processing recycles; The neutralizer that adds in the described black liquor is calcium carbonate; The neutralizer that adds in the described red liquid is sulfuric acid;
Sludge cake is processed: add neutralizer and stir in sludge cake, transfer pH to 6.5-7.5, get the sludge cake after the neutralization; The neutralizer that adds in the described black liquor is calcium hydroxide; The neutralizer that adds in the described red liquid is sulfuric acid;
The grass meal preparation: non-wood type string is pulverized, and crossing sieve diameter is the 3mm-6mm sieve plate, gets grass meal;
Batching: grass meal is dropped in the mixer, add polyvinyl alcohol graft copolymerized starch, consumption is the 8%-12% of grass meal over dry quality, stirs evenly, and adds MDI-50 again, and consumption is the 4%-8% of grass meal over dry quality, stirs evenly, and adds at last the sludge cake after neutralizing; The over dry mass ratio of the sludge cake after the neutralization and grass meal is 1:0.8-1.2, stirs evenly, and gets compound;
Preformed: usefulness preformed spreading machine by product specification requirement preformed, gets preform with compound;
Moulding: on the building materials heat pressing forming machines preform is carried out thermocompression forming, pressure is 0.8 MPa-1.2MPa, and temperature is 105 ℃-115 ℃, and the time is pressed building materials THICKNESS CALCULATION 0.8 min/mm-1.2min/mm, the material of must finalizing the design.
2. the circulation comprehensive of described a kind of black liquor of pulp making or red liquid utilizes technique according to claim 1, it is characterized in that, to the processing of polishing and cut edge of described typing material, gets the building materials finished product.
3. the circulation comprehensive of described a kind of black liquor of pulp making or red liquid utilizes technique according to claim 1 and 2, it is characterized in that, the flocculant consumption is the 2.5%-3% of black liquor or red liquid quality in the described preprocessing process, and the oxidant consumption is the 3%-3.5% of black liquor or red liquid quality.
4. the circulation comprehensive of described a kind of black liquor of pulp making or red liquid utilizes technique according to claim 1 and 2, it is characterized in that, transfers pH to 7 during described water treatment and sludge cake are processed.
5. the circulation comprehensive of described a kind of black liquor of pulp making or red liquid utilizes technique according to claim 1 and 2, it is characterized in that, polyvinyl alcohol graft copolymerized starch consumption is 10% of grass meal over dry quality in the described blending process; The MDI-50 consumption is 6% of grass meal over dry quality; The over dry mass ratio of the sludge cake after the neutralization and grass meal is 1:1.
6. the circulation comprehensive of described a kind of black liquor of pulp making or red liquid utilizes technique according to claim 1 and 2, it is characterized in that, the pressure of thermocompression forming is 1.0MPa in the described forming process, and temperature is 110 ℃, and the time is pressed building materials THICKNESS CALCULATION 1min/mm.
7. the circulation comprehensive of described a kind of black liquor of pulp making or red liquid utilizes technique according to claim 1 and 2, it is characterized in that, the non-wood type string in the described grass meal preparation is selected from straw, kaoliang stalk, wheat straw, cornstalk, reed or bagasse.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210106232 CN102635011B (en) | 2012-04-12 | 2012-04-12 | Recycling comprehensive utilization technology for pulping black liquor or red liquor |
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|---|---|---|---|
| CN 201210106232 CN102635011B (en) | 2012-04-12 | 2012-04-12 | Recycling comprehensive utilization technology for pulping black liquor or red liquor |
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| CN102635011A CN102635011A (en) | 2012-08-15 |
| CN102635011B true CN102635011B (en) | 2013-10-23 |
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| CN104878636B (en) * | 2015-04-23 | 2017-08-25 | 中国制浆造纸研究院 | A kind of purified cotton preparation and its method for pollutant control |
| CN106915894B (en) * | 2017-05-15 | 2019-07-16 | 沈夏磊 | A kind of compound addition reagent of mud-water separation and preparation method thereof and application method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0117529A3 (en) * | 1983-02-25 | 1986-12-30 | Dieter J. Dipl.-Chem. Becker | Process for the purification of waste water originating from the production of cellulose, especially from bleaching with chlorine |
| CN1262359A (en) * | 2000-03-17 | 2000-08-09 | 中国科学院生态环境研究中心 | Cyclic process for treating black paper-making liquid of alkali pulping to recover useful resource |
| CN1397684A (en) * | 2001-07-13 | 2003-02-19 | 阮键华 | Process for treating and reclaiming black paper-making liquid generated by alkali pulping |
| CN1587077A (en) * | 2003-08-26 | 2005-03-02 | 山东泉林纸业有限责任公司 | Process for extracting lignin by acid separation |
-
2012
- 2012-04-12 CN CN 201210106232 patent/CN102635011B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0117529A3 (en) * | 1983-02-25 | 1986-12-30 | Dieter J. Dipl.-Chem. Becker | Process for the purification of waste water originating from the production of cellulose, especially from bleaching with chlorine |
| CN1262359A (en) * | 2000-03-17 | 2000-08-09 | 中国科学院生态环境研究中心 | Cyclic process for treating black paper-making liquid of alkali pulping to recover useful resource |
| CN1397684A (en) * | 2001-07-13 | 2003-02-19 | 阮键华 | Process for treating and reclaiming black paper-making liquid generated by alkali pulping |
| CN1587077A (en) * | 2003-08-26 | 2005-03-02 | 山东泉林纸业有限责任公司 | Process for extracting lignin by acid separation |
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