CN1032378C - Method for recycling and fully recovering alkaline straw pulp papermaking black liquor - Google Patents
Method for recycling and fully recovering alkaline straw pulp papermaking black liquor Download PDFInfo
- Publication number
- CN1032378C CN1032378C CN 93118743 CN93118743A CN1032378C CN 1032378 C CN1032378 C CN 1032378C CN 93118743 CN93118743 CN 93118743 CN 93118743 A CN93118743 A CN 93118743A CN 1032378 C CN1032378 C CN 1032378C
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- CN
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- Prior art keywords
- black liquor
- lignin
- calcium
- filtrate
- acidifying
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Abstract
The method comprises the steps of acidifying the alkaline papermaking black liquor by using sulfur dioxide as an acidifying agent to separate lignin, using calcium hydroxide as a neutralizing agent to convert acidic filtrate into alkalinity, precipitating and separating calcium sulfite, and reusing the alkaline filtrate for pulping or evaporating to concentrate into calcium saccharate slurry containing multiple components or drying into calcium saccharate powder, thereby completely converting the papermaking black liquor into a product.
Description
The present invention relates to the full method that reclaims of alkaline straw pulp paper black liquid resource.
It is reported, family surplus the existing middle-size and small-size paper ten thousand of China, most factories do not add processing to black liquid promptly discharges, both serious environment pollutions, the heavy damage ecological balance again.
With traditional black liquor recovery method, at first cost of investment is big, and middle-size and small-size paper mill is difficult to bear, secondly, because annual production is little, make the existing problems without interruption of black liquor, this also is a problem, moreover, because silicone content height in the straw pulp black liquor, therefore, along with the silicon accumulation, with blocking pipe, therefore, the traditional firing method alkali of this kind reclaims, and still has some technical problems for the recovery of the high black liquor of silicon content.
Another kind of black liquor processing method is with hydrochloric acid or sulfuric acid and black liquor reaction, to generate the lignin precipitation, but sodium chloride in the filtrate after separating or sodium sulphate are recycled and are worth not quite, therefore, this method makes NaOH be transformed into low NaCl and the Na of value when reclaiming lignin
2SO
4
The applicant's CN891066942 Chinese patent discloses a kind of method with acidifying process of paper black liquid with sulphur dioxide, this method comprises uses the SO 2 acidifying black liquor, under heat tracing, precipitate lignin, with the acid filtrate behind the separating lignin with NaOH neutralization and evaporation, crystallization to reclaim sodium sulfite.Yet evaporative crystallization not only needs more equipment investment, and Na
2SO
3Market prospects are little.
The processing method that the purpose of this invention is to provide a kind of alkaline straw-pulp black liquid, it can also reclaim calcium sulfite and sodium hydroxide solution when reclaiming lignin, reclaim entirely to reach paper-mill black liquor and development as resource.And recovery method is simple and easy to do, CaSO
3Extensive market.
Method of the present invention is applicable to alkaline straw-pulp black liquid, alkaline wheat straw pulp particularly, and typical black liquor composition is: content of lignin＞2%, Baume degrees 5-7, pH＞7.5～12, ash content＜5%.
Method of the present invention is to realize like this, at first make the black liquor acidifying with sulfur dioxide, under heat tracing, precipitate lignin, isolated by filtration lignin and contain the acid filtrate of inferior sulfate radical then, the pH of black liquor acidifying is below 4, Baume degrees≤7, and temperature is 50～70 ℃, in acid solution, add calcium hydroxide at last, obtain calcium sulfite precipitation and alkaline solution.This solution can be back to slurrying, or inspissation becomes calcium carbohydrate pulp, dry back saccharogenesis calcium powder.
The main reaction process of each one is as follows in the said method:
R is a lignin in the formula.
Acid solution behind the separating lignin adds Ca (OH)
2Generate CaSO
3Precipitation.
Alkaline solution behind the separation calcium sulfite is back to slurrying or inspissation becomes calcium carbohydrate pulp, dry back saccharogenesis calcium powder.
The preferred embodiments of the invention are:
1. roasting pyrite (also available coal troilite, sulphur or the sulfur dioxide liquid of containing gasifies) produces sulfur dioxide gas;
2. make its water-soluble acid solution that contains sulfurous acid that becomes, the alkaline black liquor or directly feed sulfur dioxide in black liquor of neutralizing then forms the solution system that contains sulfurous acid, makes pH＜4 precipitation lignin;
3. reaction black liquid wave hairdressing＜7 of acid precipitation lignin and in 50～70 ℃ of heating;
4. isolated by filtration lignin, with dry after the hot wash lignin product;
5. in acid filtrate, add 4～5% Ca (OH)
2,, be settled out CaSO in 60～90 ℃ of heating
3, and filter to isolate solid-state CaSO
3
6. isolate solid CaSO
3After alkaline filtrate be back to slurrying or inspissation becomes dried calcium carbohydrate pulp, or dry saccharogenesis calcium powder.
(as CN89106694) compares with prior art, and the advantage and the good effect of the inventive method are:
1. with calcium sulfite products substitution sodium sulfite product, produce light building material with it, market is very wide, thereby can avoid having limited because of produce market is saturated the popularization of resource technology;
2. replace in the NaOH with calcium hydroxide (or lime) and separating lignin after acid solution, thereby production cost is reduced greatly;
3. separate calcium sulfite with the precipitation method and replace refrigeration and Crystallization Separation sodium sulfite repeatedly, thereby simplified equipment, reduced investment.
4. alkaline filtrate is back to slurrying after separating inferior calcium, or inspissation, is dried to powder and obtains the 3rd product.
This method is to obtain the calcium sulfite product with acid filtrate in the calcium hydroxide, and reaction condition is simple, and product separates easily; Solution changes into alkalescence and also contains carbohydrate and calcium constituent, can be back to slurrying or inspissation, dry saccharogenesis calcium powder.
This method has following characteristics:
(1) simple, the small investment of equipment;
(2) with low cost;
(3) processing ease, cycle weak point;
(4) moisture content is removed when evaporation drying in the black liquor, and all the other compositions all change three products over to, no longer include discharge of wastewater, and pollution control is thorough, satisfies environmental requirement fully, reaches the ideal environment benefit, and excellent economic is arranged.
Claims (5)
1. full recovery method of alkaline straw pulp paper black liquid resource, comprise with sulfur dioxide and make the black liquor acidifying, under heat tracing, precipitate lignin, and isolated by filtration lignin and acid filtrate, it is characterized in that, combine with inferior sulfate radical in the acid filtrate with calcium hydroxide behind the separating lignin, generate the calcium sulfite precipitation, and separate that to obtain that the calcium sulfite precipitation reaches with NaOH be the filtrate of main component.
2. method according to claim 1 is characterized in that black liquor acidifying pH value below 4, Baume degrees≤7.
3. method according to claim 1 and 2 is characterized in that the temperature of lignin flocculation sediment is≤50～70 ℃
4. method according to claim 1 and 2, the Baume degrees of wherein said black liquor are≤7.
5. method according to claim 3, the Baume degrees of wherein said black liquor are≤7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93118743 CN1032378C (en) | 1993-10-25 | 1993-10-25 | Method for recycling and fully recovering alkaline straw pulp papermaking black liquor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93118743 CN1032378C (en) | 1993-10-25 | 1993-10-25 | Method for recycling and fully recovering alkaline straw pulp papermaking black liquor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1102227A CN1102227A (en) | 1995-05-03 |
| CN1032378C true CN1032378C (en) | 1996-07-24 |
Family
ID=4992620
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 93118743 Expired - Lifetime CN1032378C (en) | 1993-10-25 | 1993-10-25 | Method for recycling and fully recovering alkaline straw pulp papermaking black liquor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1032378C (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1059482C (en) * | 1996-09-10 | 2000-12-13 | 刘友会 | Alkali process for treating black liquor |
| CN1115435C (en) * | 1998-09-15 | 2003-07-23 | 中南工业大学 | Acidifying sulfate pulp-making process |
| CN1075574C (en) * | 1999-07-15 | 2001-11-28 | 孙连超 | Process for preparing sodium xylose from paper-making black liquor and recovering caustic soda by dry combustion |
| CN1093581C (en) * | 2000-09-25 | 2002-10-30 | 孙连超 | Process for reclaiming neutral ammonium sulfite liquor to produce more lignin products |
| CN104153232A (en) * | 2014-08-06 | 2014-11-19 | 广西星岛科技发展有限公司 | Method for treating pulping black liquor through alkali cooking method taking gramineous plants as materials |
| CN106634904A (en) * | 2016-11-10 | 2017-05-10 | 仇颖超 | Preparation method of high-temperature and high-salinity water shutoff agent special for oil well |
| CN117684409A (en) * | 2023-12-29 | 2024-03-12 | 佛山市昊舜德聚合物科技有限公司 | A resource treatment method for papermaking black liquor |
-
1993
- 1993-10-25 CN CN 93118743 patent/CN1032378C/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| CN1102227A (en) | 1995-05-03 |
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