CN105601943A - Method used for preparing sulfonated lignin from sulfate papermaking waste water - Google Patents
Method used for preparing sulfonated lignin from sulfate papermaking waste water Download PDFInfo
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- CN105601943A CN105601943A CN201510773227.4A CN201510773227A CN105601943A CN 105601943 A CN105601943 A CN 105601943A CN 201510773227 A CN201510773227 A CN 201510773227A CN 105601943 A CN105601943 A CN 105601943A
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- lignosulfonate
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Abstract
The invention discloses a method used for preparing sulfonated lignin from sulfate papermaking waste water. The method comprises following steps: firstly, papermaking waste liquid membrane is treated so as to obtain a membrane concentrate, and the membrane concentrate is subjected to sulfonation and condensation successively so as to obtain sulfonated lignin. The method is capable of changing waste into valuables, and reducing environmental pollution; at the same time technology step is simplified, production period is shortened, and production efficiency is increased; the obtained sulfonated lignin is high in thermal stability, and excellent in contamination resistance and hydrophilic performance.
Description
Technical field
The present invention relates to a kind of sulfate papermaking wastewater and prepare the method for lignosulfonate.
Background technology
Paper-making industry is the heavy polluted industry of China, and wherein most important reason is exactly the processing of black liquid. Under normal circumstances, enterprise generally adopts two kinds of methods to black liquor treatment: one is that black liquor is concentrated to burning; Another kind is to utilize black liquor exploitation lignin product. Front kind of method black liquor, through condensed combustion, although can reclaim alkali and the part calorific value in black liquor, is that a kind of low value utilizes mode concerning alkali lignin, and equipment investment large, consume energy high. A kind of rear method is by alkali lignin is carried out to chemical modification, and exploitation lignin chemical products, improve its high added value, are the good methods of rationally utilizing alkali lignin.
The patent No. is: 201310082509.0, patent name is: a kind of method of utilizing black liquid to prepare lignin, the problems such as its manufacturing process exists complex process, the production cycle is long, production efficiency is low, and the lignin simultaneously obtaining exists heat endurance low, and hydrophily is poor.
Summary of the invention
The object of the present invention is to provide a kind of sulfate papermaking wastewater to prepare the method for lignosulfonate, its twice laid, when reducing environmental pollution, simplify processing step, shortened the production cycle, improve production efficiency, the lignosulfonate heat endurance obtaining is high, contamination is good, good hydrophilic property.
In order to achieve the above object, technical scheme of the present invention is:
Sulfate papermaking wastewater is prepared a method for lignosulfonate, comprises the steps: first papermaking wastewater to be obtained to film concentrate through film processing, thereby then film concentrate is obtained to lignosulfonate by sulfonation, condensation successively.
Described papermaking wastewater carries out pretreatment to papermaking wastewater before film is processed, and removes water-insoluble particle and fibrous impurity.
Described pretreatment can leave standstill more than 5 minutes by precipitation, thereby filter filters or water-insoluble particle and fibrous impurity are removed in centrifugal separating device centrifugation.
Thereby described film processing can adopt rolled film, tubular membrane or board-like film to process polymeric alkali lignin to papermaking wastewater and be trapped within film surface, accumulation, the concentrated film concentrate that obtains.
Described film concentrate carries out oxidation processes to film concentrate before sulfonation, thereby the pH value of acquisition film concentrate is 8-13. The process of oxidation processes can reduce its reproducibility, increases dispersed.
Described oxidation processes can adopt airoxidation or oxidant oxidation processes, and oxidant can adopt ozone or hydrogen peroxide.
Described film concentrate is by sulfur dioxide sulfonating reaction, sodium hydrogensulfite sulfonating reaction, or sulfuric acid, sodium sulfite sulfonating reaction. The process of sulfonating reaction can improve its hydrophily, dispersiveness.
Described film concentrate passes through formaldehyde condensation reaction. The process of condensation reaction can increase its molecular weight, improves its heat endurance and contamination.
Described film concentrate makes concentrate acid out obtain large molecule rugose wood element precipitation by sulfuric acid, hydrochloric acid or carbon dioxide before sulfonation, thereby then large molecule rugose wood element precipitation is obtained to lignosulfonate by sulfonation, condensation successively.
The invention has the beneficial effects as follows: a kind of sulfate papermaking wastewater is prepared the method for lignosulfonate, its twice laid, when reducing environmental pollution, simplify processing step, shortened the production cycle, improve production efficiency, the lignosulfonate heat endurance obtaining is high, contamination is good, good hydrophilic property.
Detailed description of the invention
Embodiment 1
A kind of sulfate papermaking wastewater is prepared the method for lignosulfonate, comprise the steps: first papermaking wastewater to be obtained to film concentrate through film processing, thereby described film processing can adopt rolled film or board-like film to process and make polymeric alkali lignin be trapped within film surface papermaking wastewater, accumulation, the concentrated film concentrate that obtains.
Described papermaking wastewater carries out pretreatment to papermaking wastewater before film is processed, and removes water-insoluble particle and fibrous impurity. Described pretreatment can be by staticly settling more than 5 minutes, thereby filter filters or water-insoluble particle and fibrous impurity are removed in centrifugal separating device centrifugation.
Described film concentrate makes concentrate acid out obtain large molecule rugose wood element precipitation by sulfuric acid, hydrochloric acid or carbon dioxide before sulfonation.
Then thereby large molecule rugose wood element is obtained to lignosulfonate by sulfonation, condensation successively. Described large molecule rugose wood element precipitation is by sulfur dioxide sulfonating reaction. Described film concentrate passes through formaldehyde condensation reaction.
A kind of sulfate papermaking wastewater of the present embodiment is prepared the method for lignosulfonate, and its twice laid has been simplified processing step when reducing environmental pollution, shortened the production cycle, improve production efficiency, the lignosulfonate heat endurance obtaining is high, and contamination is good, good hydrophilic property.
Embodiment 2
A kind of sulfate papermaking wastewater is prepared the method for lignosulfonate, comprise the steps: first papermaking wastewater to be obtained to film concentrate through film processing, thereby described film processing can adopt rolled film, tubular membrane or board-like film to process polymeric alkali lignin to papermaking wastewater and be trapped within film surface, accumulation, the concentrated film concentrate that obtains.
Described papermaking wastewater carries out pretreatment to papermaking wastewater before film is processed, and removes water-insoluble particle and fibrous impurity. Described pretreatment can be passed through to leave standstill, precipitate more than 5 minutes, thereby filter filters or water-insoluble particle and fibrous impurity are removed in centrifugal separating device centrifugation.
Described film concentrate carries out oxidation processes to film concentrate before sulfonation, is 8-13 thereby make the pH value of film concentrate. Described oxidation processes can adopt airoxidation or oxidant oxidation processes, and oxidant can adopt ozone or hydrogen peroxide or other oxidants.
Then thereby the film concentrate after oxidation processes is obtained to lignosulfonate by sulfonation, condensation successively. Described film concentrate is by sodium hydrogensulfite sulfonating reaction. Described film concentrate passes through formaldehyde condensation reaction.
A kind of sulfate papermaking wastewater of the present embodiment is prepared the method for lignosulfonate, and its twice laid has been simplified processing step when reducing environmental pollution, shortened the production cycle, improve production efficiency, the lignosulfonate heat endurance obtaining is high, and contamination is good, good hydrophilic property.
Embodiment 3
A kind of sulfate papermaking wastewater is prepared the method for lignosulfonate, comprise the steps: that first processing obtains film concentrate to papermaking wastewater film, thereby described film processing can adopt rolled film, tubular membrane or board-like film to process polymeric alkali lignin to papermaking wastewater and be trapped within film surface, accumulation, the concentrated film concentrate that obtains.
Described papermaking wastewater carries out pretreatment to papermaking wastewater before film is processed, and removes water-insoluble particle and fibrous impurity. Described pretreatment can be passed through to leave standstill, precipitate more than 5 minutes, thereby filter filters or water-insoluble particle and fibrous impurity are removed in centrifugal separating device centrifugation.
Described film concentrate carries out oxidation processes to film concentrate before sulfonation, thereby the pH value of acquisition film concentrate is 8-13. Described oxidation processes can adopt airoxidation or oxidant oxidation processes, and oxidant can adopt ozone or hydrogen peroxide.
Then, in the concentrate after oxidation processes, add sulfuric acid acid out to obtain large molecule rugose wood element precipitation, thereby then obtain lignosulfonate by sulfonation, condensation successively obtaining large molecule rugose wood element precipitation. Described film concentrate is by sodium sulfite sulfonating reaction. Described film concentrate passes through formaldehyde condensation reaction.
A kind of sulfate papermaking wastewater of the present embodiment is prepared the method for lignosulfonate, and its twice laid has been simplified processing step when reducing environmental pollution, shortened the production cycle, improve production efficiency, the lignosulfonate heat endurance obtaining is high, and contamination is good, good hydrophilic property.
Embodiment 4
A kind of sulfate papermaking wastewater is prepared the method for lignosulfonate, comprise the steps: that first processing obtains film concentrate to papermaking wastewater film, thereby described film processing can adopt rolled film, tubular membrane or board-like film to process polymeric alkali lignin to papermaking wastewater and be trapped within film surface, accumulation, the concentrated film concentrate that obtains.
Then thereby film concentrate is obtained to lignosulfonate by sulfonation, condensation successively. Described film concentrate is by sulfur dioxide sulfonating reaction. Described film concentrate passes through formaldehyde condensation reaction.
A kind of sulfate papermaking wastewater of the present embodiment is prepared the method for lignosulfonate, and its twice laid has been simplified processing step when reducing environmental pollution, shortened the production cycle, improve production efficiency, the lignosulfonate heat endurance obtaining is high, and contamination is good, good hydrophilic property.
Embodiment 5
Sulfate papermaking wastewater is prepared a method for lignosulfonate, thereby comprises the steps: papermaking wastewater to obtain lignosulfonate by sulfonation, condensation successively. Described film concentrate is by sulfur dioxide sulfonating reaction. Described film concentrate passes through formaldehyde condensation reaction.
A kind of sulfate papermaking wastewater of the present embodiment is prepared the method for lignosulfonate, and its twice laid has been simplified processing step when reducing environmental pollution, shortened the production cycle, improve production efficiency, the lignosulfonate heat endurance obtaining is high, and contamination is good, good hydrophilic property.
Claims (9)
1. sulfate papermaking wastewater is prepared a method for lignosulfonate, it is characterized in that comprising the steps: first sulfate papermaking wastewater being obtained to film concentrate through film processing, thereby then film concentrate is obtained to lignosulfonate by sulfonation, condensation successively.
2. a kind of sulfate papermaking wastewater according to claim 1 is prepared the method for lignosulfonate, it is characterized in that: described papermaking wastewater carries out pretreatment to papermaking wastewater before film is processed, and removes water-insoluble particle and fibrous impurity.
3. a kind of sulfate papermaking wastewater according to claim 2 is prepared the method for lignosulfonate, it is characterized in that: described pretreatment can leave standstill more than 5 minutes by precipitation, thereby filter filters or water-insoluble particle and fibrous impurity are removed in centrifugal separating device centrifugation.
4. a kind of sulfate papermaking wastewater according to claim 1 is prepared the method for lignosulfonate, it is characterized in that: be trapped within film surface thereby described film processing can adopt rolled film, tubular membrane or board-like film to process polymeric alkali lignin to papermaking wastewater, accumulation, the concentrated film concentrate that obtains.
5. a kind of sulfate papermaking wastewater according to claim 1 is prepared the method for lignosulfonate, it is characterized in that: described film concentrate carries out oxidation processes to film concentrate before sulfonation, thereby the pH value of acquisition film concentrate is 8-13.
6. a kind of sulfate papermaking wastewater according to claim 5 is prepared the method for lignosulfonate, it is characterized in that: described oxidation processes can adopt airoxidation or oxidant oxidation processes, and oxidant can adopt ozone or hydrogen peroxide.
7. a kind of sulfate papermaking wastewater according to claim 1 is prepared the method for lignosulfonate, it is characterized in that: described film concentrate is by sulfur dioxide sulfonating reaction, sodium hydrogensulfite sulfonating reaction, or sodium sulfite sulfonating reaction.
8. a kind of sulfate papermaking wastewater according to claim 1 is prepared the method for lignosulfonate, it is characterized in that: described film concentrate passes through formaldehyde condensation reaction.
9. a kind of sulfate papermaking wastewater according to claim 1 is prepared the method for lignosulfonate, it is characterized in that: described film concentrate makes concentrate acid out obtain large molecule rugose wood element precipitation by sulfuric acid, hydrochloric acid or carbon dioxide before sulfonation, thereby then large molecule rugose wood element precipitation is obtained to lignosulfonate by sulfonation, condensation successively.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108314789A (en) * | 2017-10-18 | 2018-07-24 | 海南金海浆纸业有限公司 | A method of preparing lignosulfonate using black liquid |
| CN108456572A (en) * | 2018-05-18 | 2018-08-28 | 萧县沃德化工科技有限公司 | Air-liquid two-phase sulfonation soda pulping process spent lye prepares slurries additive agent |
| CN108864442A (en) * | 2017-12-14 | 2018-11-23 | 济宁明升新材料有限公司 | A method of lignosulphonates are prepared using dissolving pulp pre-cooked waste liquid |
| CN109179845A (en) * | 2018-11-16 | 2019-01-11 | 河南省科学院化学研究所有限公司 | A kind of disposal of resources method of sulfate method pulp black liquor |
| CN109251322A (en) * | 2018-11-16 | 2019-01-22 | 河南省科学院化学研究所有限公司 | Utilize the method for sulfate pulping black liquor production sodium lignin sulfonate |
| CN109384938A (en) * | 2018-10-31 | 2019-02-26 | 张飞 | The method and its application of sodium lignin sulfonate are prepared using black liquid |
| CN109679113A (en) * | 2018-12-12 | 2019-04-26 | 上海昶法新材料有限公司 | A kind of preparation method of low contamination lignosulfonates |
| CN114000369A (en) * | 2021-09-28 | 2022-02-01 | 山东格瑞兰德添加剂有限公司 | Method for preparing anionic surfactant from ultrafiltration sulfate pulping black liquor |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108314789A (en) * | 2017-10-18 | 2018-07-24 | 海南金海浆纸业有限公司 | A method of preparing lignosulfonate using black liquid |
| CN108314789B (en) * | 2017-10-18 | 2020-10-30 | 海南金海浆纸业有限公司 | Method for preparing sulfonated lignin by using papermaking black liquor |
| CN108864442A (en) * | 2017-12-14 | 2018-11-23 | 济宁明升新材料有限公司 | A method of lignosulphonates are prepared using dissolving pulp pre-cooked waste liquid |
| CN108456572A (en) * | 2018-05-18 | 2018-08-28 | 萧县沃德化工科技有限公司 | Air-liquid two-phase sulfonation soda pulping process spent lye prepares slurries additive agent |
| CN109384938A (en) * | 2018-10-31 | 2019-02-26 | 张飞 | The method and its application of sodium lignin sulfonate are prepared using black liquid |
| CN109179845A (en) * | 2018-11-16 | 2019-01-11 | 河南省科学院化学研究所有限公司 | A kind of disposal of resources method of sulfate method pulp black liquor |
| CN109251322A (en) * | 2018-11-16 | 2019-01-22 | 河南省科学院化学研究所有限公司 | Utilize the method for sulfate pulping black liquor production sodium lignin sulfonate |
| CN109179845B (en) * | 2018-11-16 | 2021-06-25 | 河南省科学院化学研究所有限公司 | Resourceful treatment method for sulfate process wood pulp black liquor |
| CN109679113A (en) * | 2018-12-12 | 2019-04-26 | 上海昶法新材料有限公司 | A kind of preparation method of low contamination lignosulfonates |
| CN114000369A (en) * | 2021-09-28 | 2022-02-01 | 山东格瑞兰德添加剂有限公司 | Method for preparing anionic surfactant from ultrafiltration sulfate pulping black liquor |
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Application publication date: 20160525 |