CN102559305A - Compound efficient coal water slurry additive and preparation method thereof - Google Patents
Compound efficient coal water slurry additive and preparation method thereof Download PDFInfo
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- CN102559305A CN102559305A CN2011103532834A CN201110353283A CN102559305A CN 102559305 A CN102559305 A CN 102559305A CN 2011103532834 A CN2011103532834 A CN 2011103532834A CN 201110353283 A CN201110353283 A CN 201110353283A CN 102559305 A CN102559305 A CN 102559305A
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Abstract
The invention discloses a compound efficient coal water slurry additive and a preparation method thereof. The preparation method comprises the steps that 5 parts of lignosulfonate powder is added to 10 parts of water, a pH (potential of hydrogen) value is regulated to 9 to 10, 5 parts of aldehydes are added to the water, and then a hydroxymethylation reaction is conducted, so as to obtain an intermediate I; afterwards, 5 parts of lignosulfonate powder is dissolved in 10 parts of water, 5 parts of ketones are added to the water, and an intermediate II is obtained after a reaction; and the obtained intermediate I is mixed with the obtained intermediate II, a pH value is regulated to 5 to 6 by using dilute sulphuric acid, the temperature is controlled within a range of 80 DEG C to 90 DEG C, a graft copolymerization reaction is conducted, and then the compound efficient coal water slurry additive is obtained after a reaction product is cooled to room temperature. The coal water slurry additive prepared by adopting the method has the advantages of low production cost, high lignin utilization rate, steady performance and high efficiency.
Description
Technical field
The present invention relates to a kind of additive of coal water slurry, exactly relate to a kind of composite highly effective slurries additive agent and preparation method thereof.
Background technology
Coal water slurry comes from the world oil energy dilemma of the seventies in last century.It is by about 70% coal; The formulated a kind of coal-water mixture of water about 30% and a spot of chemicaladditives (about 1%); Be a kind of slurry New-type fuel, have good flowability and stable, can carry out pumping, atomizing, storage and stable burning as oil.The water coal slurry replacing oil combustion technology is in the fuel-economizing clean coal technology promoted of China very important one.Coal water slurry is the change row fluid fuel of coal; Have fuel efficiency height, low, the low cost and other advantages of pollutant emission; Can be widely used in boiler of power plant, Industrial Boiler, Industrial Stoves previous generation oil, for gas, for coal combustion, developing water coal slurry industrial application meets the Energy policy of China; Meet China's energy development strategy, satisfy the energy substitution demand.
Each character of coal water slurry is mainly regulated and control through additive.Different by its effect, normally used slurries additive agent comprises dispersion agent, stablizer and some other assistant chemical medicaments.Anionic dispersing agent mainly contains naphthalenesulfonate, sulfonated humic acid salt etc.Wherein naphthalenesulfonate series anionic type additive be use at present more a kind of.Though this type additive good dispersivity, the dehesion effect is strong, the slurry good fluidity, and slurry stability is poor, and bleed produces hard-caked sediment easily, and on the high side, increases the slurrying cost.The non-ionic type additive mainly contains T 46155 and polyoxy ethane series; This type additive is that mainly the amphipathic property of molecule and relative molecular mass are easy to regulate and control; Do not receive the influence of solvend in water quality and the coal; But cost an arm and a leg, and need skimmer, be difficult for the preparation high-concentration coal-water slurry.
Xylogen slurries additive agent raw material sources are abundant, nontoxic, cheap, and it is imperative that its research and extension is used.Exist aromatic base, phenolic hydroxyl group, alcoholic extract hydroxyl group, carbon back conjugated double bond isoreactivity group in the lignin molecule in the structure; Therefore can carry out many chemical reactions such as acidolysis methoxyl group, Suo Ji, phthaleinization, sulfonation, alkylation, polycondensation or graft copolymerization, have the possibility that makes good additive.But in present research, production technique, low and technical process is complicated to the utilization ratio of xylogen, the additive effects on slurry making that obtains is undesirable.
Summary of the invention
The purpose of this invention is to provide a kind of composite highly effective slurries additive agent and preparation method thereof, the slurries additive agent production cost that adopts this kind method to make is low, the xylogen utilization ratio is high and the slurries additive agent stable performance that makes, efficient.
Composite highly effective slurries additive agent of the present invention is made up of following component by weight:
10 parts of sulfonated lignin; 20 parts in water; 25%NaOH solution; Dilute sulphuric acid; 5 parts of aldehydes; 5 parts of ketone things.
The method for preparing composite highly effective slurries additive agent of the present invention is made up of following steps successively:
(1) 5 parts of sulfonated lignin powder is added in 10 parts of water, regulate ph value to 9～10, add 5 parts of aldehydes, under 80～90 ℃, carried out hydroxymethylation 1～1.5 hour, get intermediate compound I with NaOH;
(2) 5 parts of sulfonated lignin powder are dissolved in 10 parts of water, add 5 parts of ketone things, reacted 30 minutes down, get intermediate II at 45～50 ℃;
(3) intermediate compound I that obtains and intermediate II are mixed, using dilute sulphuric acid to regulate the ph value is 5～6, and 80～90 ℃ of controlled temperature carried out graft copolymerization 3 hours, and reaction finishes postcooling to room temperature, obtains slurries additive agent solution.
The slurries additive agent solution that makes is promptly made powder-like product through super-dry.
In the said components, aldehydes refers to: formaldehyde, acetaldehyde, oxalic dialdehyde, one or more mixtures of propionic aldehyde, butyraldehyde, LUTARALDEHYDE;
The ketone thing refers to: one or more mixtures in methyl ethyl diketone, pimelinketone, methyl phenyl ketone, the ketene.
The present invention compared with prior art has following outstanding advantage and effect:
1, production process of the present invention is carried out under atmospheric low-temperature, has the advantage that technology is simple, efficient is high, production cost is low.The product good water solubility, no strange taste, nontoxic, belong to green chemical;
2, the suitable coal scope of efficient slurries additive agent of the present invention is wide, has good dispersion and falls glutinous usefulness and slurry stability;
3, efficient slurries additive agent of the present invention is a main raw material with the papermaking wastewater regenerant, and production technique is simple, and is cheap, can be used as slurries additive agent and uses separately, also can be used with other additives.Adopt preparation method of the present invention, improved the utility value of pulping and paper-making sub product, have environmental protection and economic double effect.
Embodiment
Table one: the coal water slurry performance of product of the present invention and other additive preparation relatively
[embodiment 1]
Get dry sulfonated lignin 100 grams; Add in the 200 gram water, adding concentration again and be 25% NaOH solution modulation ph value is 10, is heated to certain service temperature while stirring; Service temperature is 90 degree, drips formaldehyde 25 grams in this process and carries out hydroxymethylation 1 hour; Get dry ligninsulfonate 50 grams, adding 100 gram water stirring and dissolving are warming up to 45 degree, add methyl ethyl diketone 40 grams, react half a hour; Two kinds of reaction intermediates of top gained are mixed, and adding 30% dilution heat of sulfuric acid while stirring, to regulate ph value be 5, is warming up to 90 degree, in this process, drips formaldehyde 20 and restrain and carry out polycondensation, reacted 3 hours.Obtain efficient slurries additive agent liquid product after the cooling, can get the solid, powdery product through drying again.
[embodiment 2]
Get dry sulfonated lignin 100 grams; Add in the 200 gram water, adding concentration again and be 25% NaOH solution modulation ph value is 9, is heated to certain service temperature while stirring; Service temperature is 90 degree, drips oxalic dialdehyde 25 grams in this process and carries out hydroxymethylation 1 hour; Get dry ligninsulfonate 50 grams, adding 100 gram water stirring and dissolving are warming up to 45 degree, add ketene 40 grams, react half a hour; Two kinds of reaction intermediates of top gained are mixed, and adding 30% dilution heat of sulfuric acid while stirring, to regulate ph value be 5.5, is warming up to 85 degree, in this process, drips oxalic dialdehyde 20 and restrain and carry out polycondensation, reacted 3 hours.Obtain efficient slurries additive agent liquid product after the cooling, can get the solid, powdery product through drying again.
[embodiment 3]
Get dry sulfonated lignin 100 grams; Add in the 200 gram water, adding concentration again and be 25% NaOH solution modulation ph value is 10, is heated to certain service temperature while stirring; Service temperature is 85 degree, drips propionic aldehyde 25 grams in this process and carries out hydroxymethylation 1 hour; Get dry ligninsulfonate 50 grams, adding 100 gram water stirring and dissolving are warming up to 45 degree, add methyl ethyl diketone and pimelinketone 40 grams, react half a hour; Two kinds of reaction intermediates of top gained are mixed, and adding 30% dilution heat of sulfuric acid while stirring, to regulate ph value be 5, is warming up to 90 degree, in this process, drips propionic aldehyde 20 and restrain and carry out polycondensation, reacted 3 hours.Obtain efficient slurries additive agent liquid product after the cooling, can get the solid, powdery product through drying again.
[embodiment 4]
Get dry sulfonated lignin 100 grams; Add in the 200 gram water, adding concentration again and be 25% NaOH solution modulation ph value is 9.5, is heated to certain service temperature while stirring; Service temperature is 90 degree, drips isobutyric aldehyde 25 grams in this process and carries out hydroxymethylation 1 hour; Get dry ligninsulfonate 50 grams, adding 100 gram water stirring and dissolving are warming up to 45 degree, add pimelinketone 40 grams, react half a hour; Two kinds of reaction intermediates of top gained are mixed, and adding 30% dilution heat of sulfuric acid while stirring, to regulate ph value be 5, is warming up to 85 degree, in this process, drips isobutyric aldehyde 20 and restrain and carry out polycondensation, reacted 3 hours.Obtain efficient slurries additive agent liquid product after the cooling, can get the solid, powdery product through drying again.
Table one is that embodiment product and each performance of prior art products compare
Annotate: flowability: A continuous flow B discontinuous flow
Be higher than naphthalene sulfonic salt formaldehyde mixture by the slurry static stability that can find out product prepn of the present invention in the table one, and the dispersion of coal water slurry is fallen glutinous effect obviously.The present invention has good dispersion and falls glutinous usefulness and slurry stability.
The present invention is a raw material with the recovery sub product sulfonated lignin of pulp and paper industry; Prepare efficient slurries additive agent through methylolation, graft copolymerization; Both realized that coal water slurry was dispersed and stable preferably; Greatly reduce production cost again, improve enterprises comprehensive and utilize xylogen and solve the enthusiasm that pulping back liquor pollutes, have good environmental protection and economy benefit and social benefit.
Claims (4)
1. a composite highly effective slurries additive agent is characterized in that, is made up of following component by weight: 10 parts of sulfonated lignin; 20 parts in water; 25%NaOH solution; Dilute sulphuric acid; 5 parts of aldehydes; 5 parts of ketone things.
2. the preparation method of a composite highly effective slurries additive agent is characterized in that, is made up of following steps successively:
(1) 5 parts of sulfonated lignin powder is added in 10 parts of water, regulate ph value to 9～10, add 5 parts of aldehydes, under 80～90 ℃, carried out hydroxymethylation 1～1.5 hour, get intermediate I with NaOH;
(2) 5 parts of sulfonated lignin powder are dissolved in 10 parts of water, add 5 parts of ketone things, reacted 30 minutes down, get the midbody II at 45～50 ℃;
(3) intermediate I that obtains and midbody II are mixed, using dilute sulphuric acid to regulate the ph value is 5～6, and 80～90 ℃ of controlled temperature carried out graft copolymerization 3 hours, and reaction finishes postcooling to room temperature, obtains slurries additive agent solution.
The slurries additive agent solution that makes is promptly made powder-like product through super-dry.
3. the preparation method of a kind of composite highly effective slurries additive agent according to claim 2 is characterized in that, in the said components, and aldehydes nail aldehyde, acetaldehyde, oxalic dialdehyde, one or more mixtures of propionic aldehyde, butyraldehyde, LUTARALDEHYDE.
4. the preparation method of a kind of composite highly effective slurries additive agent according to claim 2 is characterized in that, in the said components, the ketone thing refers to one or more mixtures in methyl ethyl diketone, pimelinketone, methyl phenyl ketone, the ketene.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106243141A (en) * | 2016-08-01 | 2016-12-21 | 常州聚博节能科技有限公司 | Inorganic hybridization methylolated lignin and preparation method thereof |
| CN106281513A (en) * | 2015-10-19 | 2017-01-04 | 刘剑锋 | A kind of modified aliphatic slurries additive agent and preparation method thereof |
| CN111704725A (en) * | 2020-06-30 | 2020-09-25 | 金陵科技学院 | Preparation method of modified natural bio-based lignin sulfonate high-efficiency water reducing agent |
| CN113817177A (en) * | 2021-07-16 | 2021-12-21 | 兖矿新疆煤化工有限公司 | Modified lignosulfonate dispersant, preparation method and application in coal water slurry |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63199793A (en) * | 1987-02-16 | 1988-08-18 | Kubota Ltd | Production of coal-water slurry |
| CN1404912A (en) * | 2002-11-08 | 2003-03-26 | 华南理工大学 | Modified lignin sulfosalt dispersant of water coal slurry |
| CN1818041A (en) * | 2006-03-08 | 2006-08-16 | 华南理工大学 | Hydrophilous slurry additive with mediben lignin and production thereof |
-
2011
- 2011-11-10 CN CN2011103532834A patent/CN102559305A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63199793A (en) * | 1987-02-16 | 1988-08-18 | Kubota Ltd | Production of coal-water slurry |
| CN1404912A (en) * | 2002-11-08 | 2003-03-26 | 华南理工大学 | Modified lignin sulfosalt dispersant of water coal slurry |
| CN1818041A (en) * | 2006-03-08 | 2006-08-16 | 华南理工大学 | Hydrophilous slurry additive with mediben lignin and production thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106281513A (en) * | 2015-10-19 | 2017-01-04 | 刘剑锋 | A kind of modified aliphatic slurries additive agent and preparation method thereof |
| CN106243141A (en) * | 2016-08-01 | 2016-12-21 | 常州聚博节能科技有限公司 | Inorganic hybridization methylolated lignin and preparation method thereof |
| CN111704725A (en) * | 2020-06-30 | 2020-09-25 | 金陵科技学院 | Preparation method of modified natural bio-based lignin sulfonate high-efficiency water reducing agent |
| CN111704725B (en) * | 2020-06-30 | 2022-01-25 | 金陵科技学院 | Preparation method of modified natural bio-based lignin sulfonate high-efficiency water reducing agent |
| CN113817177A (en) * | 2021-07-16 | 2021-12-21 | 兖矿新疆煤化工有限公司 | Modified lignosulfonate dispersant, preparation method and application in coal water slurry |
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Application publication date: 20120711 |