CN102923990A - Preparation method of lignin polysulfonate high-efficiency water reducing agent - Google Patents
Preparation method of lignin polysulfonate high-efficiency water reducing agent Download PDFInfo
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- CN102923990A CN102923990A CN2012104280229A CN201210428022A CN102923990A CN 102923990 A CN102923990 A CN 102923990A CN 2012104280229 A CN2012104280229 A CN 2012104280229A CN 201210428022 A CN201210428022 A CN 201210428022A CN 102923990 A CN102923990 A CN 102923990A
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Abstract
The invention discloses a preparation method of a lignin polysulfonate high-efficiency water reducing agent, which comprises the following steps: (1) dissolving sulfite in water in a reaction kettle, and carrying out sulfonation reaction with acetone for 20-60 minutes; (2) adding papermaking black liquor into the reaction kettle, and reacting for 20-60 minutes; (3) dropwisely adding 10-20% formaldehyde, and carrying out polycondensation reaction for 120-360 minutes; and (4) adding sulfite and formaldehyde, and reacting for 60-120 minutes, thereby obtaining the liquid product. The method is simple and easy to implement; when being used in concrete, the lignin polysulfonate high-efficiency water reducing agent can reduce the water consumption of concrete, save the cement by 20-30%, and increase the flowability and workability of the concrete, thereby enhancing the strength and durability of the concrete; and when being used in coal water slurry, the lignin polysulfonate high-efficiency water reducing agent can enable the coal powder particle surface to be hydrophilic and negatively charged, so that the coal powder can be easily mixed and dissolved in water, and the coal water slurry has low viscosity and favorable flowability.
Description
Technical field
The present invention relates to a kind of building and industrial auxiliary agent, refer more particularly to a kind of preparation method of the high efficiency water reducing agent for concrete and coal water slurry.
Background technology
High efficiency water reducing agent can increase considerably the concrete mix workability, satisfying pumping or preparation self-compacting concrete needs, or is keeping significantly reducing the mixing water amount under the concrete work degree permanence condition; Be used for coal water slurry, can make coal dust and water miscible, reduce viscosity in aqueous coal slurries, make it have good flowing property.High efficiency water reducing agent commonly used has naphthalene series high-efficiency water-reducing agent and aliphatic high-efficiency water reducing agent at present, naphthalene series high-efficiency water-reducing agent is under 165 ℃ NAPTHALENE FLAKES. (INDUSTRIAL GRADE） to be carried out sulfonation with the vitriol oil, again the hydrolysis and and formaldehyde condensation, make with the alkali neutralization, exist in the manufacture craft and pollute the drawback high, that energy consumption is high, and the water reducer of producing exists water-reducing rate low, the shortcomings such as bleeding; It is simple that aliphatic high-efficiency water reducing agent has the preparation method than naphthalene series high-efficiency water-reducing agent, and energy consumption is low, the characteristics such as environmental protection, but exist water-reducing rate low in use properties, easy bleeding, the shortcomings such as concrete color intensification.
Summary of the invention
The object of the present invention is to provide a kind of technique simple, environmental protection, easy to implement, and can improve the poly-sulfonic acid high efficiency water reducing agent preparation method of xylogen of water reducer performance.
For realizing above-mentioned technical purpose, the present invention realizes by the following technical solutions: xylogen gathers sulfonic acid high efficiency water reducing agent preparation method, comprises the steps;
(1) first the sulphite of total mass 10%-20% is dissolved in water in reactor, again with the acetone of 5%-20% 38 ℃-40 ℃ lower sulfonation reaction 20-60 minute;
(2) black liquid that 20%-50% is contained xylogen joined in the reactor, in 40 ℃-60 ℃ lower reactions 20-60 minute;
(3) formaldehyde of dropping 10%-20%, temperature slowly raises naturally, is warming up to 80 ℃-100 ℃, carried out polycondensation 120-360 minute,
(4) add the sulphite of 5%-10%, the formaldehyde of 5%-10% reacts and made liquid product in 60-120 minute, and the mass percent of above component is to roll over hundred calculating.
The present invention has following beneficial effect: the poly-sulfonic acid main chain of xylogen is the aliphatics straight chain, adsorption group is sulfonic group, xylogen is combined on the main chain, increased electrostatic repulsion and sterically hindered effect, be applied to play above the concrete low-dosage, water-reducing rate is high, reach more than 30%, far above water reducers such as naphthalene system and aliphatics, and the slump keeps, and has the not advantage of bleeding of not emanating; Be used on the coal water slurry, can make the pulverized coal particle surface hydrophilic, electronegative, thus make coal dust and water miscible, so that viscosity in aqueous coal slurries is low, have good flowing property; Present method is simple, implements easily.
Embodiment
Embodiment one
(1) sulphite of first 1kg is dissolved in water in reactor, again with 2kg acetone 38 ℃ of lower sulfonation reactions 60 minutes;
(2) black liquid that 5kg is contained xylogen joined in the reactor, in 40 ℃ of lower reactions 60 minutes;
(3) drip 1kg formaldehyde, temperature slowly raises naturally, is warming up to 80 ℃, carries out polycondensation 360 minutes;
(4) add 0.5kg sulphite, 0.5kg formaldehyde reacts and made liquid product in 60 minutes.
Embodiment two
(1) first 2kg sulphite is dissolved in water in reactor, again with 0.5kg acetone 40 ℃ of lower sulfonation reactions 20 minutes;
(2) black liquid that 3.5kg is contained xylogen joined in the reactor, in 60 ℃ of lower reactions 20 minutes;
(3) drip 2kg formaldehyde, temperature slowly raises naturally, is warming up to and carries out polycondensation 120 minutes under 100 ℃;
(4) add 1kg sulphite, 1kg formaldehyde reacts and made liquid product in 120 minutes.
Embodiment three
(1) first 2kg sulphite is dissolved in water in reactor, again with 2kg acetone 39 ℃ of lower sulfonation reactions 40 minutes;
(2) black liquid that 2kg is contained xylogen joined in the reactor, in 50 ℃ of lower reactions 40 minutes;
(3) drip 2kg formaldehyde, temperature slowly raises naturally, and be warming up to and carry out polycondensation 200 minutes between 90 ℃,
(4) add 1kg sulphite, 1kg formaldehyde reacts and made liquid product in 100 minutes.
Claims (1)
1. the poly-sulfonic acid high efficiency water reducing agent preparation method of xylogen is characterized in that it comprises the steps;
(1) first the sulphite of total mass 10%-20% is dissolved in water in reactor, again with the acetone of 5%-20% 38 ℃-40 ℃ lower sulfonation reaction 20-60 minute;
(2) black liquid that 20%-50% is contained xylogen joined in the reactor, in 40 ℃-60 ℃ lower reactions 20-60 minute;
(3) formaldehyde of dropping 10%-20%, temperature slowly raises naturally, is warming up to 80 ℃-100 ℃, carried out polycondensation 120-360 minute,
(4) add the sulphite of 5%-10%, the formaldehyde of 5%-10% reacts and made liquid product in 60-120 minute.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2012104280229A CN102923990A (en) | 2012-10-19 | 2012-10-19 | Preparation method of lignin polysulfonate high-efficiency water reducing agent |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012104280229A CN102923990A (en) | 2012-10-19 | 2012-10-19 | Preparation method of lignin polysulfonate high-efficiency water reducing agent |
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| CN102923990A true CN102923990A (en) | 2013-02-13 |
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| CN2012104280229A Pending CN102923990A (en) | 2012-10-19 | 2012-10-19 | Preparation method of lignin polysulfonate high-efficiency water reducing agent |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104558632A (en) * | 2014-12-30 | 2015-04-29 | 山东龙力生物科技股份有限公司 | Method for preparing lignin derivative products from industrial fiber waste residues |
| CN106188554A (en) * | 2016-07-04 | 2016-12-07 | 武汉理工大学 | A kind of twice-modified high efficiency water reducing agent and preparation method thereof |
| CN112646101A (en) * | 2021-01-14 | 2021-04-13 | 福州大学 | Lignin degradation product-sulfonated acetone-formaldehyde polycondensate dispersant and preparation method thereof |
Citations (5)
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|---|---|---|---|---|
| US4551151A (en) * | 1984-04-16 | 1985-11-05 | Westvaco Corporation | Dyestuff composition: disperse or vat dye and lignin sulphonate |
| CN101531484A (en) * | 2009-01-21 | 2009-09-16 | 福州大学 | Sulfonated acetone-formaldehyde high-efficiency water reducing agent modified by enzymatic hydrolysis lignin or by derivatives thereof, and preparation method thereof |
| CN101665337A (en) * | 2009-09-03 | 2010-03-10 | 南京林业大学 | Modified aliphatic high-efficiency water-reducing agent by utilizing lignosulfonate and preparation method thereof |
| CN102140174A (en) * | 2011-03-08 | 2011-08-03 | 延边石岘白麓纸业股份有限公司 | Preparation method for lignosulfonate |
| CN102320768A (en) * | 2011-06-20 | 2012-01-18 | 河北久强建材有限公司 | Method for preparing modified aliphatic water reducing agent |
-
2012
- 2012-10-19 CN CN2012104280229A patent/CN102923990A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4551151A (en) * | 1984-04-16 | 1985-11-05 | Westvaco Corporation | Dyestuff composition: disperse or vat dye and lignin sulphonate |
| CN101531484A (en) * | 2009-01-21 | 2009-09-16 | 福州大学 | Sulfonated acetone-formaldehyde high-efficiency water reducing agent modified by enzymatic hydrolysis lignin or by derivatives thereof, and preparation method thereof |
| CN101665337A (en) * | 2009-09-03 | 2010-03-10 | 南京林业大学 | Modified aliphatic high-efficiency water-reducing agent by utilizing lignosulfonate and preparation method thereof |
| CN102140174A (en) * | 2011-03-08 | 2011-08-03 | 延边石岘白麓纸业股份有限公司 | Preparation method for lignosulfonate |
| CN102320768A (en) * | 2011-06-20 | 2012-01-18 | 河北久强建材有限公司 | Method for preparing modified aliphatic water reducing agent |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104558632A (en) * | 2014-12-30 | 2015-04-29 | 山东龙力生物科技股份有限公司 | Method for preparing lignin derivative products from industrial fiber waste residues |
| CN106188554A (en) * | 2016-07-04 | 2016-12-07 | 武汉理工大学 | A kind of twice-modified high efficiency water reducing agent and preparation method thereof |
| CN106188554B (en) * | 2016-07-04 | 2017-11-24 | 武汉理工大学 | A kind of twice-modified high efficiency water reducing agent and preparation method thereof |
| CN112646101A (en) * | 2021-01-14 | 2021-04-13 | 福州大学 | Lignin degradation product-sulfonated acetone-formaldehyde polycondensate dispersant and preparation method thereof |
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Application publication date: 20130213 |