CN1209481A - Method for making paper pulp without discharging of waste liquid - Google Patents
Method for making paper pulp without discharging of waste liquid Download PDFInfo
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- CN1209481A CN1209481A CN 98112196 CN98112196A CN1209481A CN 1209481 A CN1209481 A CN 1209481A CN 98112196 CN98112196 CN 98112196 CN 98112196 A CN98112196 A CN 98112196A CN 1209481 A CN1209481 A CN 1209481A
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Abstract
The present invention discloses a pulping method free from discharge of waste liquor, including fibrous raw materials and cooking agent. It is characterized by that its cooking agent is acetic acid or propionic acid, and under the condition of inorganic acid as catalyst and 80-130 deg.C said materials are reacted. Said invention possesses the advantages of saving energy source, eliminating environmental pollution, extensive raw material source and simple and easy to implement technological process.
Description
The invention belongs to a kind of method of making paper pulp, belong to a kind of method for making paper pulp that does not produce waste liquid with waste sludge discharge especially.
The method of existing chemistry system paper pulp has sulfate process and sulphite process, and representational is sulfate legal system paper pulp.This method is under certain conditions, and fibrous raw material and caustic soda, vulcanized sodium are reacted in container.This pulping process produces the foul gas of sulfur-bearing in digestion process, atmospheric environment is produced have a strong impact on; Produce in the production by force to cancer material organic chloride, swallow, water environment has been caused have a strong impact on as Er Evil; And use complicated, huge equipment, investment is high; Energy consumption is very high.
Some organic solvent matter has selectively dissolved lignin and part half fine plain characteristic, thereby lignin is separated with cellulose, and solvent is recycled through distillation, remaining nearly solid shape lignin and hemicellulose or as industrial chemicals and agricultural goods, materials and equipments, or send boiler combustion, utilize its heat energy.Representational solvent pulp-making method has alcohols medicament pulp-making method, phenols medicament pulp-making method and organic acid medicament pulp-making method etc.The alcohols pulp-making method makes a large amount of fresh ethanol contact with raw material, and energy consumption is very high.Slurrying is to carry out under High Temperature High Pressure, and is quite tight to the requirements such as sealing of equipment; When phenols slurrying is used, might cause the toxicity problem of phenol in large-scale production.It is difficult and to problems such as equipment corrosion are serious that formic acid slurrying exists containing the high coniferous wood delignification of lignin.
Japanese patent laid-open 4-300379 employing hydrochloric acid is that the propionic acid solution of the 80-97% concentration of catalyst carries out the slurrying of fibrous raw material delignification.This method need make the lignin precipitation with a large amount of water, and hemicellulose is dissolved in the solution and separates, on technology, used a large amount of acetone solns, reclaim trouble, and consumes energy has been big, cooking waste liquor concentrating and separating lignin, produce a large amount of rare propionic acid solution, recycled the energy consumption height, used hydrochloric acid to be catalyst, make equipment corrosion serious, big to environmental hazard.
The purpose of this invention is to provide a kind of is steaming preparation with the organic solvent, and the method for high yield chemical pulp is produced in energy-conservation no waste liquid, toxic emission under temperate condition.This not only can solve the pollution of paper mill to atmospheric environment, water environment, can reduce energy consumption, reagent consumption, the water consumption of slurrying again.
The objective of the invention is to realize by following measure:
Steaming preparation is: acetate or propionic acid,, be preferably under 80～130 ℃ as catalyst at inorganic acid, and be more preferably under 100～120 ℃, best is to react at 103～116 ℃.
Fibrous raw material is under boiling solvent acetic acid or propionic acid and catalytic condition, carry out boiling, make lignin and the stripping of hemicellulose part extremely a little more than after the fiber separation, is paper pulp through slight mechanical treatment to help frotation, the characteristics of utilizing solvent to be easy to volatilize again, through distillation the organic solvent in the solution is separated, and recycle.
Acetate or propionic acid play the effect of lignin remover, and it can dissolve lignin and part hemicellulose in the fibrous raw material, and cellulose is separated with hemicellulose with lignin.The concentration (weight percent concentration) of acetate in steaming preparation is preferably 65～97%, and is more preferably 70～95%; The concentration (weight percent concentration) of propionic acid in steaming preparation is preferably 65～98%, and is more preferably 75～95%.
Inorganic acid plays the effect of catalyst in organic solvent.Catalyst in this method is preferably selected sulfuric acid for use, can also select phosphoric acid or hydrochloric acid for use except that sulfuric acid.
Sulfuric acid and concentration of phosphoric acid (percentage by weight) are preferably 0.05～0.5%, are more preferably 0.05～0.35%.
The present invention carries out under environmental pressure, and the reaction time is preferably 30～120 minutes, is more preferably 70～100 minutes.
The used fibrous raw material of the present invention can adopt careless class material, as straw, bamboo chip and rice bar etc., also can adopt wood type.
The present invention uses organic acid boiling fibrous raw material to make catalyst with sulfuric acid, and the slurrying condition is 103-116 ℃, and 0.75-2 hour, because the organic acid heat of vaporization is low, so boiling energy consumption of the present invention and medicament reclaimed distillation, evaporation energy consumption all far below sulfate pulping.The present invention does not use medicaments such as sulfide, so does not have foul gass such as hydrogen sulfide, mercaptan in the digestion process and discharge.Cooking waste liquor is after distillation reclaims organic solvent, and lignin and hemicellulose are collected with solid form, no longer includes the black liquor discharging, reduces that greatly the waters is polluted; Collect solid slag in drier bottom, send the boiler room to do the fuel use, or make industrial chemicals and can make full use of discarded object based on lignin and hemicellulose.The organic acid conditions of cooking is gentle, and the sex change of lignin is little, and slurry washs easily, has reduced the water consumption, and hemicellulose has 50% to remain in the thick slurry approximately under this conditions of cooking simultaneously, be easier to so pull an oar, and pulp yield is also higher; In the organic acid boiling, ash elements such as the silicon in the fibrous raw material can stripping in black liquor, handle black liquor and do not have problems such as silicon interference, therefore, the present invention both had been applicable to the wood type raw material, more be applicable to grass as raw material, raw material is applied widely.
The present invention is described further below by embodiment.
Embodiment 1.
In 50 liters of stainless steel boiling vessels (jacket steam heating), add the bamboo chip (moisture 11.6%) of 2.5 kilograms of 10-25 millimeters long, inject 25 liters of propionic acid cooking liquors, contain propionic acid 950 grams in every hydrargyrum oxydatum crudum liquid, sulfuric acid 3 grams.Under 115 ℃, boiling 120 minutes to distiller, adds 20 liters of not vitriolated propionic acid solution (propionic acid content 950g/l), 115 ℃ of following boilings 30 minutes with cooking waste liquor (pitchy) force feed again in boiling vessel.With cooking waste liquor (light brown) force feed to distiller.Superheated steam to 180 ℃ of boiling vessel feedings fully steams propionic acid residual in the crude pulp.The propionic acid that steams reclaims through condenser condenses.
The fibrous material of the above-mentioned processing of process is dried after hot water fully washs and is weighed, and gets 1.30 kilograms of crude pulps, and yield is 58.8%.The sampling chemical analysis, its lignin content is 12.7%, hemicellulose level is 13.2%.
Cooking waste liquor reclaims propionic acid through distillation.The overall recovery of overall process propionic acid is: 42.63 kilograms (with 100% purity meter), the propionic acid of per kilogram crude pulp (100%) consumption is 0.092 kilogram.
Embodiment 2.
In 50 liters of stainless steel boiling vessels (jacket steam heating), add the straw (moisture: 12.3%), inject 25 liters of acetate cooking liquors of 2.5 kilograms of 10-30 millimeters long.Contain acetate 750 grams in every hydrargyrum oxydatum crudum liquid, sulfuric acid 3 grams.Boiling is 90 minutes under 103 ℃ of temperature, with the cooking waste liquor force feed to distiller.In boiling vessel, add 20 liters again and contain acetate 750g/l and not vitriolated soup, 103 ℃ of boilings 20 minutes.With the cooking waste liquor force feed to distiller.Feed 180 ℃ of superheated steams to boiling vessel and fully steam acetate residual in the crude pulp.The acetate that steams reclaims through condenser condenses.
Dry after hot water fully washs through the fibrous raw material of above-mentioned processing and to weigh, 1.21 kilograms of crude pulps, yield is 55.2%, the sampling chemical analysis, its lignin content is 10.3%, hemicellulose level is 12.6%.
Cooking waste liquor reclaims acetate through distillation.The overall recovery of overall process acetate (100%) is 33.61 kilograms, and the acetate consumption of per kilogram crude pulp is: 0.116 kilogram.
Embodiment 3.
In 50 liters of stainless steel boiling vessels (jacket steam heating), add the rice straw (moisture: 13.1%) of 2.5 kilograms of 10-30 millimeters long.Inject 25 liters of acetate cooking liquors, contain acetate 850 grams in every hydrargyrum oxydatum crudum liquid, sulfuric acid 2 grams were 105 ℃ of temperature boilings 60 minutes.With the cooking liquor force feed to distiller.In boiling vessel, add 20 liters again and contain acetate 850g/l and not vitriolated soup, 105 ℃ of boilings 15 minutes.With the cooking waste liquor force feed to distiller.Feed 180 ℃ of superheated steams to boiling vessel and fully steam acetate residual in the crude pulp.The acetate that steams reclaims through condensation.
Dry after hot water fully washs through the fibrous raw material of above-mentioned processing and to weigh, 1.28 kilograms of crude pulps, yield is 58.9%.The sampling chemical analysis, its lignin content is 9.6%, hemicellulose level is 10.8%.
Cooking waste liquor reclaims acetate through distillation.The overall recovery of overall process acetate is 38.11 kilograms, and the acetate consumption of per kilogram crude pulp is 0.118 kilogram.
Claims (7)
1. a method for making paper pulp that does not have discharging of waste liquid comprises fibrous raw material and steaming preparation, it is characterized in that steaming preparation is: acetate or propionic acid,, react under 80-130 ℃ as catalyst at inorganic acid.
2. the method for making paper pulp of no discharging of waste liquid according to claim 1 is characterized in that the concentration (percentage by weight) of steaming preparation acetic acid solution is 65～97%.
3. the method for making paper pulp of no discharging of waste liquid according to claim 1 is characterized in that the concentration (percentage by weight) of steaming preparation propionic acid solution is 65～98%.
4. the method for making paper pulp of no discharging of waste liquid according to claim 1, the concentration that it is characterized in that sulfuric acid solution is 0.05～0.5%.
5. the method for making paper pulp of no discharging of waste liquid according to claim 1 is characterized in that fibrous raw material and steaming preparation ratio are 1: 8～17.
6. the method for making paper pulp of no discharging of waste liquid according to claim 1 is characterized in that described being reflected at carried out under the environmental pressure 30～120 minutes.
7. the method for making paper pulp of no discharging of waste liquid according to claim 1 is characterized in that described inorganic acid can be H
2SO
4, H
3PO
4Or HCl.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98112196 CN1209481A (en) | 1998-08-19 | 1998-08-19 | Method for making paper pulp without discharging of waste liquid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98112196 CN1209481A (en) | 1998-08-19 | 1998-08-19 | Method for making paper pulp without discharging of waste liquid |
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| Publication Number | Publication Date |
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| CN1209481A true CN1209481A (en) | 1999-03-03 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 98112196 Pending CN1209481A (en) | 1998-08-19 | 1998-08-19 | Method for making paper pulp without discharging of waste liquid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9296180B2 (en) | 2010-11-17 | 2016-03-29 | Nippon Stell & Sumikin Materials Co., Ltd. | Metal foil for base material |
| CN108867132A (en) * | 2018-08-21 | 2018-11-23 | 青岛科技大学 | The method that platinum-phosphotungstic acid catalyst of zirconium oxide load extracts ginger rod fibers element |
-
1998
- 1998-08-19 CN CN 98112196 patent/CN1209481A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9296180B2 (en) | 2010-11-17 | 2016-03-29 | Nippon Stell & Sumikin Materials Co., Ltd. | Metal foil for base material |
| CN108867132A (en) * | 2018-08-21 | 2018-11-23 | 青岛科技大学 | The method that platinum-phosphotungstic acid catalyst of zirconium oxide load extracts ginger rod fibers element |
| CN108867132B (en) * | 2018-08-21 | 2021-03-02 | 青岛科技大学 | Method for extracting ginger stem cellulose by using zirconium oxide loaded platinum-phosphotungstic acid catalyst |
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