CN108531231A - A kind of preparation method of low metal responsive type coal water slurry dispersing agent - Google Patents
A kind of preparation method of low metal responsive type coal water slurry dispersing agent Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of low metal responsive type coal water slurry dispersing agent, belong to coal mine field of material technology.Technical solution of the present invention prepares humic acid and modified coal water slurry dispersing agent using potassium humate, due to a large amount of negative electrical charges of coal grain surface hydrophilic region band, when effective dispersant agent molecule is in coal grain adsorption, coal water slurry dispersing agent can not only be closed by hydrophobic effect in coal burl, Cationic functional groups on its strand can also be strongly adsorbed in by electrostatic force on coal grain surface, aligning more closely can be formed on coal grain surface, improve coal grain surface hydrophilicity, coal grain is separated by means of hydration shell, to reduce the viscosity of water-coal-slurry, improve the dispersion performance of coal water slurry dispersing agent.
Description
Technical field
The present invention relates to a kind of preparation methods of low metal responsive type coal water slurry dispersing agent, belong to coal mine material technology neck
Domain.
Background technology
In the preparation process of water-coal-slurry, add a small amount of dispersant can play the role of it is vital.Dispersant can
By changing coal particle surface property, can be homogeneously dispersed in slurry, to make water-coal-slurry with lower apparent
Viscosity and good rheological characteristic.Its mechanism of action can be illustrated by following three aspects：
For the effect of 1 wetting and dispersing since coal is mainly a kind of nonpolar hydrocarbon, surface has strong hydrophobicity.This
Outside, since the surface tension of water is more much larger than coal surface tension, two aspect factors, which combine, causes coal grain cannot
It is fully soaked, can not be uniformly dispersed.Dispersant molecule hydrophobic effect by hydrophobic side and coal grain surface in conjunction in a manner of and
It is adsorbed on coal grain surface, water-wet side is then aligned and combined with water, is turned hydrophobic to be hydrophilic, is formed simultaneously one layer of hydration shell.
The hydration shell can be effectively reduced coal-water interfacial tension, and coal grain is separated, to reduce the viscosity of water-coal-slurry.
2 electrostatic repulsion dehesions effect dlvo theory thinks, the Van der Waals force between charged colloidal particle and electrostatic repulsion it
Between magnitude relationship determine its can stable dispersion, if Van der Waals force be less than electrostatic repulsion if it is colloid-stabilised, otherwise it is unstable.
There are a variety of oxygen-containing functional groups such as hydroxyl, carboxyl on coal surface, and dissociation is so that coal shows elecrtonegativity, Zeta potential one in water
As be -15~-20mv.Anionic dispersing agent, which is adsorbed on coal grain surface, can effectively enhance its electrostatic repulsion, promote coal grain
It is better dispersed in water.
3 steric hindrance dehesion effects are hydrophilic in molecule when dispersant adsorption is aligned in coal particle surface presentation
End can form one layer of three-dimensional hydration shell on coal surface.When coal particle is moved close to each other, hydration shell, which is squeezed, to be deformed, and is passed through
Mechanical elasticity promotes coal grain is evenly dispersed to come.In addition, dispersant itself, which is formed by adsorption layer, has certain thickness, when two
Close to when squeezing, the free movement of the molecule in adsorption layer is affected complex coal particle, reduces the entropy of coal slurry system.
Chemical thermodynamics thinks that the entropy of isolated blob is carried out towards the direction of growth always.So promoting that extrusion cladding coal grain occurs again
It is secondary separated, cause the dispersion of coal grain to suspend.
The water-coal-slurry for reaching commercial Application demand need to have high concentration, low apparent viscosity and outstanding rheological characteristic, stabilization
The performance characteristics such as property.In the preparation process of water-coal-slurry, adds a small amount of dispersant and extremely key is played to the performance of water-coal-slurry
Effect.Currently, what is be most widely used in the market is naphthalene sulfonate system dispersant, although such dispersant has good point
Dissipate performance, excellent dehesion effect and it is applied widely the advantages that, but its slurrying stability is poor.China's humic acid resource is extremely
Abundant, humic acid system coal water slurry dispersing agent is primarily referred to as humate and its modified product, its main feature is that raw material be easy to get it is inexpensive, and
The problems such as slurrying favorable dispersibility, can be used alone, but that equally there is also slurry stabilities is poor, more sensitive to metal ion.
Therefore how in the case where ensuring good dehesion effect, the emphasis that stability is existing coal water slurry dispersing agent research is improved.
Invention content
The technical problems to be solved by the invention：It is poor for existing coal water slurry dispersing agent stability of material, to metal ion
Sensitive issue provides a kind of preparation method of low metal responsive type coal water slurry dispersing agent.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
（1）In mass ratio 1:8, corrosive acid potassium is added in hydrochloric acid solution, stirs mixed rear and stands, filter and collect filter residue,
Washing, drying, grind to obtain modified particles；Nitrogen is passed through to absolute ethyl alcohol, leads to nitrogen treatment, obtains modification liquid；
（2）Count in parts by weight, respectively weigh 45~50 parts of modification liquids, 10~15 parts of deionized waters, 25~30 parts of absolute ethyl alcohols,
10~15 parts of tetraethoxysilanes are placed in three-necked flask, and insulation reaction obtains mixed liquor and by volume 1:8, by γ-aminopropyl
Tetraethoxysilane is added dropwise in mixed liquor, and after being added dropwise to complete, heating in water bath for reaction collects to obtain reaction solution；
（3）It places reaction liquid into dialysis membrane, dialysed using absolute ethyl alcohol and collects dialysis modification liquid, in mass ratio 1:5, by alkene
Propyl sulfonic acid sodium is stirred and adjusts pH to 9.0 with dodecyl trimethyl ammonium chloride, obtains matrix liquid；
（4）It counts in parts by weight, weighs 45~50 parts of matrix liquid, 10~15 parts of dialysis modification liquids, 15~20 parts of modifications respectively
Grain and 3~5 parts of polyvinyl alcohol are placed in beaker, are stirred and are adjusted pH to 9.0, obtain modified mixed liquor；
（5）Modified mixed liquor is placed in three-necked flask, at 75~85 DEG C, in mass ratio 1:15, ammonium persulfate solution is dripped
It adds in modified mixed liquor, after being added dropwise to complete, insulation reaction, standing is cooled to room temperature, ultrasonic disperse, you can be prepared into described
Low metal responsive type coal water slurry dispersing agent.
Step（1）It is 25~30mL/min that the nitrogen, which is passed through rate,.
Step（2）The γ-aminopropyl tetraethoxysilane drop rate is 2~3mL/min.
Compared with other methods, advantageous effects are the present invention：
（1）Technical solution of the present invention there is excellent sensitive property to change metal ion by modifying silicon Nano sol and preparing
Property agent, technical solution of the present invention adequately adsorbs metal ion by the sensitive decorative layer on Ludox surface, to have
Effect reduces jamming performance of the metal ion to the metal ion of effective dispersant agent material, to improve in technical solution of the present invention
The stability of coal water slurry dispersing agent；
（2）Technical solution of the present invention prepares humic acid and modified coal water slurry dispersing agent using potassium humate, due to coal grain surface parent
The a large amount of negative electrical charges of water area band, when effective dispersant agent molecule is in coal grain adsorption, coal water slurry dispersing agent can not only lead to
It crosses hydrophobic effect to close in coal burl, the Cationic functional groups on strand can also be strongly adsorbed in by electrostatic force
On coal grain surface, aligning more closely can be formed on coal grain surface, improve coal grain surface hydrophilicity, borrow hydration shell will
Coal grain separates, and to reduce the viscosity of water-coal-slurry, improves the dispersion performance of coal water slurry dispersing agent.
Specific implementation mode
In mass ratio 1:8, corrosive acid potassium is added in 1% hydrochloric acid solution of mass fraction, stir it is mixed after and stand 20~
For 24 hours, filter residue is filtered and collects, it is 7.0 to be rinsed to cleaning solution pH with deionized water, then dry 3~5h at 75~80 DEG C, grinding
Obtain modified particles；Nitrogen is passed through to absolute ethyl alcohol, it is 25~30mL/min that control nitrogen, which is passed through rate, nitrogen to be led to 25~
30min obtains modification liquid, then counts in parts by weight, weighs 45~50 parts of modification liquids, 10~15 parts of deionized waters, 25~30 respectively
Part absolute ethyl alcohol, 10~15 parts of tetraethoxysilanes are placed in three-necked flask, at 45~50 DEG C after 3~5h of insulation reaction, are obtained
Mixed liquor and by volume 1:8, γ-aminopropyl tetraethoxysilane is added dropwise in mixed liquor, control drop rate be 2~
3mL/min, after being added dropwise to complete, then at 75~85 DEG C react 10~12h, collect reaction solution is placed in dialysis membrane, adopt
It is dialysed with absolute ethyl alcohol and collects dialysis modification liquid；In mass ratio 1:5, by Sodium Allyl Sulfonate and trimethyl chlorination
Ammonium is stirred and 1% sodium hydroxide solution of mass fraction is used to adjust pH to 9.0, obtains matrix liquid and counts in parts by weight, respectively
It weighs 45~50 parts of matrix liquid, 10~15 parts of dialysis modification liquids, 15~20 parts of modified particles and 3~5 parts of polyvinyl alcohol and is placed in burning
It in cup, is stirred and adjusts pH to 9.0 with 1% sodium hydroxide solution of mass fraction, obtain modified mixed liquor, by modified mixed liquor
It is placed in three-necked flask, at 75~85 DEG C, in mass ratio 1:15,1% ammonium persulfate solution of mass fraction is added dropwise to modification
In mixed liquor, control ammonium persulfate drop rate is 2~3mL/min, after being added dropwise to complete, then the insulation reaction at 75~85 DEG C
3~5h, standing are cooled to room temperature, then 10~15min of ultrasonic disperse at 200~300W, you can are prepared into the low metal
Responsive type coal water slurry dispersing agent.
Example 1
In mass ratio 1:8, corrosive acid potassium is added in 1% hydrochloric acid solution of mass fraction, stirs mixed rear and stands 20h, filter
And filter residue is collected, it is 7.0 to be rinsed to cleaning solution pH with deionized water, then the dry 3h at 75 DEG C, grinds to obtain modified particles；To nothing
Water-ethanol is passed through nitrogen, and it is 25mL/min that control nitrogen, which is passed through rate, and nitrogen 25min to be led to obtains modification liquid, then in parts by weight
Meter weighs 45 parts of modification liquids, 10 parts of deionized waters, 25 parts of absolute ethyl alcohols, 10 parts of tetraethoxysilanes and is placed in three-necked flask respectively
In, at 45 DEG C after insulation reaction 3h, obtain mixed liquor and by volume 1:8, γ-aminopropyl tetraethoxysilane is added dropwise to mixed
It closes in liquid, control drop rate is 2mL/min, after being added dropwise to complete, then reacts 10h at 75 DEG C, collects to obtain reaction solution juxtaposition
In dialysis membrane, is dialysed using absolute ethyl alcohol and collect dialysis modification liquid；In mass ratio 1:5, by Sodium Allyl Sulfonate and 12
Alkyl trimethyl ammonium chloride is stirred and 1% sodium hydroxide solution of mass fraction is used to adjust pH to 9.0, obtains matrix liquid and by weight
Number meter is measured, 45 parts of matrix liquid, 10 parts of dialysis modification liquids, 15 parts of modified particles and 3 parts of polyvinyl alcohol is weighed respectively and is placed in beaker
In, it is stirred and adjusts pH to 9.0 with 1% sodium hydroxide solution of mass fraction, obtain modified mixed liquor, modified mixed liquor is set
In three-necked flask, at 75 DEG C, in mass ratio 1:15,1% ammonium persulfate solution of mass fraction is added dropwise to modified mixed liquor
In, control ammonium persulfate drop rate is 2mL/min, and after being added dropwise to complete, then the insulation reaction 3h at 75 DEG C, standing are cooled to
Room temperature, then the ultrasonic disperse 10min at 200W, you can be prepared into the low metal responsive type coal water slurry dispersing agent.
Example 2
In mass ratio 1:8, corrosive acid potassium is added in 1% hydrochloric acid solution of mass fraction, stirs mixed rear and stands 22h, filter
And filter residue is collected, it is 7.0 to be rinsed to cleaning solution pH with deionized water, then the dry 4h at 77 DEG C, grinds to obtain modified particles；To nothing
Water-ethanol is passed through nitrogen, and it is 27mL/min that control nitrogen, which is passed through rate, and nitrogen 27min to be led to obtains modification liquid, then in parts by weight
Meter weighs 47 parts of modification liquids, 12 parts of deionized waters, 27 parts of absolute ethyl alcohols, 12 parts of tetraethoxysilanes and is placed in three-necked flask respectively
In, at 47 DEG C after insulation reaction 4h, obtain mixed liquor and by volume 1:8, γ-aminopropyl tetraethoxysilane is added dropwise to mixed
It closes in liquid, control drop rate is 2mL/min, after being added dropwise to complete, then reacts 11h at 80 DEG C, collects to obtain reaction solution juxtaposition
In dialysis membrane, is dialysed using absolute ethyl alcohol and collect dialysis modification liquid；In mass ratio 1:5, by Sodium Allyl Sulfonate and 12
Alkyl trimethyl ammonium chloride is stirred and 1% sodium hydroxide solution of mass fraction is used to adjust pH to 9.0, obtains matrix liquid and by weight
Number meter is measured, 47 parts of matrix liquid, 12 parts of dialysis modification liquids, 17 parts of modified particles and 4 parts of polyvinyl alcohol is weighed respectively and is placed in beaker
In, it is stirred and adjusts pH to 9.0 with 1% sodium hydroxide solution of mass fraction, obtain modified mixed liquor, modified mixed liquor is set
In three-necked flask, at 77 DEG C, in mass ratio 1:15,1% ammonium persulfate solution of mass fraction is added dropwise to modified mixed liquor
In, control ammonium persulfate drop rate is 2mL/min, and after being added dropwise to complete, then the insulation reaction 4h at 80 DEG C, standing are cooled to
Room temperature, then the ultrasonic disperse 12min at 250W, you can be prepared into the low metal responsive type coal water slurry dispersing agent.
Example 3
In mass ratio 1:8, corrosive acid potassium is added in 1% hydrochloric acid solution of mass fraction, stirs mixed rear and stands for 24 hours, filtering
And filter residue is collected, it is 7.0 to be rinsed to cleaning solution pH with deionized water, then the dry 5h at 80 DEG C, grinds to obtain modified particles；To nothing
Water-ethanol is passed through nitrogen, and it is 30mL/min that control nitrogen, which is passed through rate, and nitrogen 30min to be led to obtains modification liquid, then in parts by weight
Meter weighs 50 parts of modification liquids, 15 parts of deionized waters, 30 parts of absolute ethyl alcohols, 15 parts of tetraethoxysilanes and is placed in three-necked flask respectively
In, at 50 DEG C after insulation reaction 5h, obtain mixed liquor and by volume 1:8, γ-aminopropyl tetraethoxysilane is added dropwise to mixed
It closes in liquid, control drop rate is 3mL/min, after being added dropwise to complete, then reacts 12h at 85 DEG C, collects to obtain reaction solution juxtaposition
In dialysis membrane, is dialysed using absolute ethyl alcohol and collect dialysis modification liquid；In mass ratio 1:5, by Sodium Allyl Sulfonate and 12
Alkyl trimethyl ammonium chloride is stirred and 1% sodium hydroxide solution of mass fraction is used to adjust pH to 9.0, obtains matrix liquid and by weight
Number meter is measured, 50 parts of matrix liquid, 15 parts of dialysis modification liquids, 20 parts of modified particles and 5 parts of polyvinyl alcohol is weighed respectively and is placed in beaker
In, it is stirred and adjusts pH to 9.0 with 1% sodium hydroxide solution of mass fraction, obtain modified mixed liquor, modified mixed liquor is set
In three-necked flask, at 85 DEG C, in mass ratio 1:15,1% ammonium persulfate solution of mass fraction is added dropwise to modified mixed liquor
In, control ammonium persulfate drop rate is 3mL/min, and after being added dropwise to complete, then the insulation reaction 5h at 85 DEG C, standing are cooled to
Room temperature, then the ultrasonic disperse 15min at 300W, you can be prepared into the low metal responsive type coal water slurry dispersing agent.
1,2,3 pairs of water-coal-slurry of example prepared by the present invention are added, control additive amount is 0.75%, and to water coal
Slurry is tested for the property, and specific test result is as follows shown in table table 1：
1 performance test table of table
As seen from the above table, the present invention, which prepares coal water slurry dispersing agent, has excellent dispersion performance and resistance to metal ion disturbance performance.
Claims (3)
1. a kind of preparation method of low metal responsive type coal water slurry dispersing agent, it is characterised in that specifically preparation process is：
（1）In mass ratio 1:8, corrosive acid potassium is added in hydrochloric acid solution, stirs mixed rear and stands, filter and collect filter residue,
Washing, drying, grind to obtain modified particles；Nitrogen is passed through to absolute ethyl alcohol, leads to nitrogen treatment, obtains modification liquid；
（2）Count in parts by weight, respectively weigh 45~50 parts of modification liquids, 10~15 parts of deionized waters, 25~30 parts of absolute ethyl alcohols,
10~15 parts of tetraethoxysilanes are placed in three-necked flask, and insulation reaction obtains mixed liquor and by volume 1:8, by γ-aminopropyl
Tetraethoxysilane is added dropwise in mixed liquor, and after being added dropwise to complete, heating in water bath for reaction collects to obtain reaction solution；
（3）It places reaction liquid into dialysis membrane, dialysed using absolute ethyl alcohol and collects dialysis modification liquid, in mass ratio 1:5, by alkene
Propyl sulfonic acid sodium is stirred and adjusts pH to 9.0 with dodecyl trimethyl ammonium chloride, obtains matrix liquid；
（4）It counts in parts by weight, weighs 45~50 parts of matrix liquid, 10~15 parts of dialysis modification liquids, 15~20 parts of modifications respectively
Grain and 3~5 parts of polyvinyl alcohol are placed in beaker, are stirred and are adjusted pH to 9.0, obtain modified mixed liquor；
（5）Modified mixed liquor is placed in three-necked flask, at 75~85 DEG C, in mass ratio 1:15, ammonium persulfate solution is dripped
It adds in modified mixed liquor, after being added dropwise to complete, insulation reaction, standing is cooled to room temperature, ultrasonic disperse, you can be prepared into described
Low metal responsive type coal water slurry dispersing agent.
2. a kind of preparation method of low metal responsive type coal water slurry dispersing agent according to claim 1, it is characterised in that：Step
Suddenly（1）It is 25~30mL/min that the nitrogen, which is passed through rate,.
3. a kind of preparation method of low metal responsive type coal water slurry dispersing agent according to claim 1, it is characterised in that：Step
Suddenly（2）The γ-aminopropyl tetraethoxysilane drop rate is 2~3mL/min.
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| CN201810372355.1A CN108531231A (en) | 2018-04-24 | 2018-04-24 | A kind of preparation method of low metal responsive type coal water slurry dispersing agent |
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| CN103951836A (en) * | 2014-04-18 | 2014-07-30 | 陕西科技大学 | Method for preparing sulfonation condensation polymerization modified humic acid water-coal-slurry dispersing agent |
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| CN105542886A (en) * | 2014-11-03 | 2016-05-04 | 太原市天鼎恒砼外加剂科技发展有限公司 | Coal water slurry dispersant and preparation method thereof |
| CN105567354A (en) * | 2014-10-13 | 2016-05-11 | 太原市天鼎恒硂外加剂科技发展有限公司 | Dispersant for coal water slurry and preparation method thereof |
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