CN101700479A - Method for preparing novel water-coal slurry dispersing agent by utilizing papermaking black liquor - Google Patents
Method for preparing novel water-coal slurry dispersing agent by utilizing papermaking black liquor Download PDFInfo
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- CN101700479A CN101700479A CN200910229871A CN200910229871A CN101700479A CN 101700479 A CN101700479 A CN 101700479A CN 200910229871 A CN200910229871 A CN 200910229871A CN 200910229871 A CN200910229871 A CN 200910229871A CN 101700479 A CN101700479 A CN 101700479A
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Abstract
The invention discloses a method for preparing a novel water-coal slurry dispersing agent by utilizing papermaking black liquor. The method comprises the following steps: filtering waste black liquor, separating filtrate by using a semipermeable membrane, washing precipitate which is lignin and is blocked with 2-4 times weight of water, adding caustic soda, introducing SO2 at 130-150 DEG C, drying in water bath to obtain sodium lignin sulfonate, then adding ethanediol, water and concentrated sulfuric acid, and reacting for 2h under normal temperature and pressure to obtain the finished product. The method for preparing the novel water-coal slurry dispersing agent by utilizing the papermaking black liquor not only carries out effective reclamation treatment and utilization to the papermaking black liquor, but also obtains the novel water-coal slurry dispersing agent, and has wide raw material source, low manufacturing cost and broad application prospect in the reclamation treatment of the papermaking black liquor.
Description
Technical field
The present invention relates to a kind of recycling processing method of black liquid, relate in particular to a kind of method of utilizing black liquid to prepare novel water-coal slurry dispersing agent.
Background technology
Paper industry is that an energy, industrial chemicals consume high, big, the with serious pollution industry of water consumption, the paper field pulping and paper-making small scale of China, quantity is many, it is wide to distribute, lack effective pollution control, and China's pulping raw material is based on wheat straw fiber, raw material availability is low, and black liquor complicated component, lignin are the accessory substances of paper industry, it is contained in the black liquor of pulp-making method papermaking as main component, cheap, the source is abundant, and is non-renewable living resources, annual 5000000000 tons of the black liquids that produce of China's paper industry, wherein lignin contains 4,300,000 tons approximately.At present most ofly directly discharge with paper waste, both wasted important resource as refuse, again severe contamination environment, therefore the efficient resource processing to black liquor seems extremely important.
To extensive method alkali recovery technology and the lignin acidizing separation technology that adopts of administration of papermaking black liquid, acid-precipitation method is a kind of black liquor processing method that is suitable for middle-size and small-size paper plant, the principle of this method is that the solubility of lignin (mainly containing in the black liquor organic pollutants) descends along with the decline of pH value, generally drop to 5.0 and will separate out when following, generally drop to 5.0 and will separate out when following in the pH value in the pH value.Although certain effect is arranged, to invest greatlyyer, operating cost is too high, and alkali is recouped the investment more than 5,000 ten thousand yuan, and use in the paper mill that only is fit to produce per year more than 30,000 tons.The content of silicon is higher in the careless class black liquor simultaneously, and to reducing the alkali cost recovery, it is also unsatisfactory to improve alkali recovery on technology, and lignin acidizing separation can make lignin products be reclaimed, but the lignin market outlet is not smooth.
Summary of the invention
The present invention is for solving at present the problem to the treatment technology deficiency of black liquid, a kind of method that black liquid can be carried out effectively recycling treatment is provided, product after the one-step optimization black liquor of going forward side by side is handled is used as the dispersant of water-coal-slurry, thereby realize the recycling of black liquid, turn waste into wealth.
For achieving the above object, the present invention adopts following scheme:
The method of utilizing black liquid to prepare novel water-coal slurry dispersing agent of the present invention comprises the steps:
(1) be the moto-vibro screen filtration papermaking waste black liquor of 100-300 μ m with the aperture, filtrate is separated after pellicle, and the precipitate that does not see through is lignin, and the solution that sees through with the electrolysis of single stage membrane electric dialyzator, is promptly separated out caustic soda at negative pole again; Wherein the one pole film is that high shear dynamic film, shear strength are 140000-160000s
-1, the electrode voltage of electric dialyzator is 6-20V;
(2), add step (1) gained caustic soda, then in stirring 130-150 ℃ of feeding SO down with after the water washing of step (1) gained lignin with 2-4 times of weight
2To pH=5.0-6.0, reaction finishes the back and uses drying with water bath, promptly gets sodium lignin sulfonate; Wherein the mol ratio of caustic soda and lignin is 1.5: 1-3: 1;
(3) add ethylene glycol, water and the concentrated sulfuric acid in step (2) gained sodium lignin sulfonate, normal temperature and pressure promptly obtains novel coal water slurry dispersing agent after reacting 2h down; Wherein the mol ratio of sodium lignin sulfonate and ethylene glycol is 1: 2-1: 5, and the amount of water is 3-5 a times of sodium lignin sulfonate weight, the weight of the concentrated sulfuric acid is the 1-3% of sodium lignin sulfonate weight.
For making processing method of the present invention reach best, the mechanical oscillation mesh size is preferably 200 μ m described in the step (1), and the single stage membrane shear strength is 150000s
-1, the electrode voltage of electric dialyzator is 12-15V; The mol ratio of caustic soda and lignin is 2: 1 described in the step (2); The mol ratio of sodium lignin sulfonate and ethylene glycol is 1: 3 described in the step (3).
The method of utilizing black liquid to prepare novel water-coal slurry dispersing agent of the present invention, both the papermaking waste black liquor recycling treatment and utilization had effectively been carried out, a kind of novel coal water slurry dispersing agent of having got back, the preparation raw material sources are extensive, cost of manufacture is low, has broad application prospects in the recycling treatment of black liquid.
The specific embodiment
Embodiment 1
(1) be the moto-vibro screen filtration papermaking waste black liquor of 200 μ m with the aperture, filtrate is separated after pellicle, and the precipitate that does not see through is lignin (mean molecule quantity 2400), and the solution that sees through is that 12V, shear strength are 150000s again with the electrode voltage
-1The electrolysis of single stage membrane electric dialyzator, promptly separate out caustic soda at negative pole;
(2) with step (1) gained lignin 100g (about 0.042mol) with after the 200g water washing, add step (1) gained caustic soda 3.36g (0.084mol), feed SO in stirring down 130-150 ℃ then
2To pH=5.0-6.0, reaction finishes the back and uses drying with water bath, promptly gets 96.5g (about 0.039mol) sodium lignin sulfonate;
(3) add 7.3g (about 0.117mol) ethylene glycol, 300g water and the 2g concentrated sulfuric acid in step (2) gained sodium lignin sulfonate, normal temperature and pressure promptly obtains novel coal water slurry dispersing agent after reacting 2h down.
Embodiment 2
(1) be the moto-vibro screen filtration papermaking waste black liquor of 300 μ m with the aperture, filtrate is separated after pellicle, and the precipitate that does not see through is lignin (mean molecule quantity 2400), and the solution that sees through is that 6V, shear strength are 160000s again with the electrode voltage
-1The electrolysis of single stage membrane electric dialyzator, promptly separate out caustic soda at negative pole;
(2) with step (1) gained lignin 100g (about 0.042mol) with after the 400g water washing, add step (1) gained caustic soda 2.52g (0.063mol), feed SO in stirring down 130-150 ℃ then
2To pH=5.0-6.0, reaction finishes the back and uses drying with water bath, promptly gets 94.6g (about 0.038mol) sodium lignin sulfonate;
(3) add 4.7g (about 0.076mol) ethylene glycol, 300g water and the 1g concentrated sulfuric acid in step (2) gained sodium lignin sulfonate, normal temperature and pressure promptly obtains novel coal water slurry dispersing agent after reacting 2h down.
Embodiment 3
(1) be the moto-vibro screen filtration papermaking waste black liquor of 100 μ m with the aperture, filtrate is separated after pellicle, and the precipitate that does not see through is lignin (mean molecule quantity 2400), and the solution that sees through is that 20V, shear strength are 140000s again with the electrode voltage
-1The electrolysis of single stage membrane electric dialyzator, promptly separate out caustic soda at negative pole;
(2) with step (1) gained lignin 100g (about 0.042mol) with after the 200g water washing, add step (1) gained caustic soda 5.04g (about 0.126mol), then in stirring 130-150 ℃ of feeding SO down
2To pH=5.0-6.0, reaction finishes the back and uses drying with water bath, promptly gets 93g (about 0.037mol) sodium lignin sulfonate;
(3) add 11.5g (about 0.185mol) ethylene glycol, 450g water and the 2.5g concentrated sulfuric acid in step (2) gained sodium lignin sulfonate, normal temperature and pressure promptly obtains novel coal water slurry dispersing agent after reacting 2h down.
Claims (4)
1. a method of utilizing black liquid to prepare novel water-coal slurry dispersing agent is characterized in that comprising the steps:
(1) be the moto-vibro screen filtration papermaking waste black liquor of 100-300 μ m with the aperture, filtrate is separated after pellicle, and the precipitate that does not see through is lignin, and the solution that sees through with the electrolysis of single stage membrane electric dialyzator, is promptly separated out caustic soda at negative pole again; The one pole film is that high shear dynamic film, shear strength are 140000-160000s
-1, the electrode voltage of electric dialyzator is 6-20V;
(2), add step (1) gained caustic soda, then in stirring 130-150 ℃ of feeding SO down with after the water washing of step (1) gained lignin with 2-4 times of weight
2To pH=5.0-6.0, reaction finishes the back and uses drying with water bath, promptly gets sodium lignin sulfonate; The mol ratio of described caustic soda and lignin is 1.5: 1-3: 1;
(3) add ethylene glycol, water and the concentrated sulfuric acid in step (2) gained sodium lignin sulfonate, normal temperature and pressure promptly obtains novel coal water slurry dispersing agent after reacting 2h down; The mol ratio of described sodium lignin sulfonate and ethylene glycol is 1: 2-1: 5, and the amount of water is 3-5 a times of sodium lignin sulfonate weight, the weight of the concentrated sulfuric acid is the 1-3% of sodium lignin sulfonate weight.
2. according to the described method of utilizing black liquid to prepare novel water-coal slurry dispersing agent of claim 1, it is characterized in that mechanical oscillation mesh size described in the step (1) is 200 μ m, the single stage membrane shear strength is 150000s
-1, the electrode voltage of electric dialyzator is 12-15V.
3. according to the described method of utilizing black liquid to prepare novel water-coal slurry dispersing agent of claim 1, it is characterized in that the mol ratio of caustic soda described in the step (2) and lignin is 2: 1.
4. according to the described method of utilizing black liquid to prepare novel water-coal slurry dispersing agent of claim 1, it is characterized in that the mol ratio of sodium lignin sulfonate described in the step (3) and ethylene glycol is 1: 3.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103045317A (en) * | 2012-12-26 | 2013-04-17 | 中国东方电气集团有限公司 | Lignin serial coal water slurry dispersing agent and preparation method thereof |
| 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 |
| CN103819686A (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-sulphur coal and fiber hydrolysis residues |
| CN104357114A (en) * | 2014-11-21 | 2015-02-18 | 湖南科技大学 | Lignin-series water-coal-slurry composite additive as well as preparation method and application thereof |
| CN115348894A (en) * | 2020-03-30 | 2022-11-15 | 东洋纺株式会社 | Semipermeable polyphenylene-based membrane and process for producing the same |
-
2009
- 2009-11-17 CN CN200910229871XA patent/CN101700479B/en active Active
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103045317A (en) * | 2012-12-26 | 2013-04-17 | 中国东方电气集团有限公司 | Lignin serial coal water slurry dispersing agent and preparation method thereof |
| CN103045317B (en) * | 2012-12-26 | 2014-08-27 | 中国东方电气集团有限公司 | Lignin serial coal water slurry dispersing agent and preparation method thereof |
| 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 |
| CN103819686A (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-sulphur coal and fiber hydrolysis residues |
| CN103819686B (en) * | 2014-03-21 | 2016-02-03 | 河南省科学院化学研究所有限公司 | High sulphur coal and fiber hydrolysis residue is utilized to produce the method for sodium lignosulfonate |
| CN103819687B (en) * | 2014-03-21 | 2016-02-03 | 河南省科学院化学研究所有限公司 | A kind of method utilizing high sulphur coal to produce sodium lignosulfonate |
| CN104357114A (en) * | 2014-11-21 | 2015-02-18 | 湖南科技大学 | Lignin-series water-coal-slurry composite additive as well as preparation method and application thereof |
| CN104357114B (en) * | 2014-11-21 | 2016-07-20 | 湖南科技大学 | A kind of Lignins water-coal-slurry compound additive and preparation method thereof and utilization |
| CN115348894A (en) * | 2020-03-30 | 2022-11-15 | 东洋纺株式会社 | Semipermeable polyphenylene-based membrane and process for producing the same |
| CN115348894B (en) * | 2020-03-30 | 2024-04-09 | 东洋纺株式会社 | Polyphenylene semipermeable membrane and process for producing the same |
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