CN106967387B - A method of the water-fast dust suppressant of soft film type is prepared using black liquid - Google Patents
A method of the water-fast dust suppressant of soft film type is prepared using black liquid Download PDFInfo
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Abstract
The invention discloses a kind of methods for preparing the water-fast dust suppressant of soft film type using black liquid, belong to environmental protection technical field.Lignosulfonates are made as dust suppression core by raw material of black liquid in the present invention, utilize hydroxyl contained in lignosulfonate molecules structure, sulfonic group isoreactivity group can be in conjunction with coal particles, cured layer, which is formed, on surface reaches dust suppression purpose, by warm milk, lipochondrion floats to form fine and close skin on boiled milk to the cold again, glycerol and fatty acid are resolved into lipase enzymatic hydrolysis skin on boiled milk again, it uses glycerol as plasticizer and improves product film forming, lignosulfonates and acrylic acid are finally passed through into water solution polymerization process graft copolymerization, improve the stability of dust suppressant, sodium methyl silicate again improves the water resistance of dust suppressant, the water-fast dust suppressant stability of soft film type produced by the present invention is strong, after use cured layer can be formed in coal surface, it is non-breakable after concussion, anti-dust effect is good, water resistance is good, it has broad application prospects.
Description
Technical field
The invention discloses a kind of methods for preparing the water-fast dust suppressant of soft film type using black liquid, belong to environmental protection skill
Art field.
Background technique
Railway Coal transport is generally used open-top car and transports, since roadbed, track switch and rail facility cause in transportational process
The wind pressure to jolt and when train operation generates, especially form the strong disturbance air-flow of moment, meeting as the train moves into the tunnel
Make the coal grain on surface by the car body that blows off, falls and be spread across ground, and ecological environment of the coal dust blown off not only to along causes seriously
Pollution, and certain destruction will also result in equipment such as railway roadbed in route, railway signal and contact power grids, considerably increase
Maintenance cost, while also resulting in the no small wasting of resources.So solving the problems, such as that Railway Coal dust pollution is very urgent.
Currently, the method for preventing coal from being scattered is mainly include the following types: 1, capping method.Car body capping can effectively prevent coal dust
Be scattered, but its higher cost, the sequence of operations such as Er Qiekai, lid can disguise coal to existing machinery, process of unloading coal generate it is larger
It influences, is difficult to match with existing automatic production line；2, tarpaulin covering method.With tarpaulin body perimeter and vertical or horizontal
Rope binds the method on compartment mouth.It effectively prevents coal dust or other powder things to fly out out of compartment with the wind, but due to
Along Railway high degree of automation, vehicle flowrate are big, and operating speed is fast, need a large amount of manpowers that could complete；3, watering method.Watering is
Prevent and treat the most common method of dust pollution, but natural conditions are dry, in environment of train high-speed cruising, inevitably result in evaporation
Amount is big, and sprinkling is frequent, and the difficult requirement for reaching environmental quality；4, chemical dust suppression method.Dust suppressant is sprayed in coal surface, it is applied
Work is easy, and dust-proof effect is preferable, and does not have any influence to coal burning.
Dust suppressant is composed of novel and multifunctional high molecular polymer.The degree of cross linking between polymer molecule will form net
Shape structure, at the same it is intermolecular there are various ionic groups, stronger affinity can be generated between ion.Its mechanism of action is
It by capture, absorption, reunion dust particle, is rigidly fastened within reticular structure, plays wet, bonding, condensation, moisture absorption, prevents
Dirt, anti-etch and antiscour effect.But the waterproof effect of dust suppressant is mostly poor at present, during transportation, once it meets
It will result in a large amount of coal dust loss to rainfall, and commercially available dust suppressant is mostly hard-shell type, during Coal Transport, by
Therefore easy fragmentation after to concussion, with railway transportation raising speed by a large scale, develops a kind of film strength to lose dust suppression effect
Big and with certain waterproof ability coal dust depressor has become one of urgent problem at this stage.
Summary of the invention
Present invention mainly solves the technical issues of: be mostly hard-shell type for presently commercially available dust suppressant, after being shaken
Easy fragmentation, to lose dust suppression effect, and the defect of waterproof effect difference provides a kind of utilization black liquid and prepares soft film type
The method of water-fast dust suppressant.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
(1) it collects black liquid and filtrate is obtained by filtration, filtrate and water are mixed to get mixed liquor, hydrogen is added into mixed liquor
Calcium oxide, heating boil 30~35min, obtain calcifying solution, and calcifying solution is staticly settled to be separated by filtration after 10~12h and is filtered
Slag；
(2) it is stirred to react 20~30min after sulfuric acid being added into above-mentioned filter residue, sulfuric acid calcium precipitate is filtered off, obtains pre-
Filtrate is handled, then sodium carbonate is added into pretreatment filtrates, 2~3h is stirred to react at 90~95 DEG C, after filtering removal precipitates
Obtain filtered fluid, by filtered fluid be concentrated into the 1/3 of its original volume concentrate, then under conditions of concentrate is placed on 4~6 DEG C it is cold
But it crystallizes, crystal is obtained by filtration, it is spare；
(3) warm milk is poured into stainless steel pallet immediately when naturally cooling to 80~82 DEG C after taking whole milk heating to boil
In, then pallet is put into refrigerator and stands 20~30min at 2~4 DEG C, pallet is taken out, is formed with tweezers tweezer tray surface
Fine and close skin on boiled milk；
(4) skin on boiled milk obtained above is fitted into enzymatic vessel, then lipase and deionized water is added into tank, be stirred
After 10~15min will enzymatic vessel move into insulating box in digest, after enzymatic hydrolysis by zymolyte take out and stratification 20~
30min, isolated lower layer's glycerine water solution；
(5) it weighs 10~20g acrylic acid to be fitted into dropping funel, is that 30% sodium hydroxide solution adjusts third with mass fraction
Olefin(e) acid degree of neutralization is to 68~72%, then weighs the spare crystal of 15~25g step (2) and be fitted into three-necked flask, and 50~60mL is added
Water heats 30~40min at 60~70 DEG C, then the acrylic acid in dropping funel is instilled in three-necked flask, then toward three-necked flask
Middle addition 0.1~0.2g potassium peroxydisulfate after being stirred to react 1~2h continues that 1~2gN, N '-di-2-ethylhexylphosphine oxide are added into three-necked flask
8~10g glycerine water solution obtained above and 3~4g methyl are added into three-necked flask after the reaction was continued 3~4h for acrylamide
Sodium metasilicate, discharging is after being warming up to 75~80 DEG C the reaction was continued 1~2h to get the water-fast dust suppressant of soft film type.
The mass ratio of filtrate as described in step (1) and water is 1:1, and the additional amount of calcium hydroxide is mixed liquor quality
10%。
Sulphuric acid described in step (2) is 5~6 times of filter residue quality, and the mass fraction of sulfuric acid is 10%, carbonic acid
The additional amount of sodium is equal with filter residue quality.
The additional amount of lipase described in step (4) is the 1% of skin on boiled milk quality, and the additional amount of deionized water is milk cortex
1~2 times of amount, the temperature of insulating box are 30~40 DEG C, and enzymolysis time is 6~8h
The beneficial effects of the present invention are:
(1) present invention generates wood by the hydroxy combining in sulphite and lignin molecule using black liquid as raw material
Mahogany sulfonate, using lignosulfonates as dust suppression core, using hydroxyl contained in lignosulfonate molecules structure,
Sulfonic group isoreactivity group can reach dust suppression purpose in the cured layer that surface forms crosslinking net in conjunction with coal particles,
Formed crosslinking net cured layer film formation time is short, and film strength is big, and the continuity and excellent tenacity of the caudacoria that forms a film were being transported
It is non-breakable by shaking in journey；
(2) by warm milk, lipochondrion floats to form fine and close skin on boiled milk the present invention to the cold, then digests skin on boiled milk with lipase
Glycerol and fatty acid are resolved into, plasticizer is used glycerol as and improves product film forming, finally by lignosulfonates and propylene
Acid improves the stability of dust suppressant, sodium methyl silicate again mentions the water resistance of dust suppressant by water solution polymerization process graft copolymerization
Height solves the problems, such as that traditional dust suppressant waterproof effect is poor.
Specific embodiment
Filtrate is obtained by filtration in collection 50~60L black liquid first, is mixed after filtrate and water are mixed by equal mass ratioes
Liquid to be closed, mixed liquor is moved into reaction kettle and the calcium hydroxide of mixed liquor quality 10% is added into kettle, 30~35min is boiled in heating,
Calcifying solution is obtained, is separated by filtration to obtain filter residue after calcifying solution is staticly settled 10~12h, 5~6 times of its quality is added into filter residue
Mass fraction is to be stirred to react 20~30min after 10% sulfuric acid, filters off sulfuric acid calcium precipitate, obtains pretreatment filtrates, then to pre-
The sodium carbonate that the quality such as filter residue are added in filtrate is handled, moves into water-bath and is stirred to react 2~3h at 90~95 DEG C, filter off
Except obtaining filtered fluid after precipitating, by filtered fluid be put into concentrated by rotary evaporation in Rotary Evaporators to its original volume 1/3 concentrate, then
Concentrate is put into refrigerator crystallisation by cooling at 4~6 DEG C, crystal is obtained by filtration, then measure 2~3L whole milk heating boil after
Warm milk is poured in stainless steel pallet immediately when naturally cooling to 80~82 DEG C, then that pallet is put into refrigerator is quiet at 2~4 DEG C
It sets 20~30min, takes out pallet, be fitted into enzymatic vessel with the skin on boiled milk of tweezers tweezer tray surface densification, then by skin on boiled milk, then to tank
The middle lipase and 1~2 times of skin on boiled milk quality of deionized water that skin on boiled milk quality 1% is added will digest after being stirred 10~15min
Tank moves into and digests 6~8h in 30~40 DEG C of insulating box, takes out zymolyte and 20~30min of stratification after enzymatic hydrolysis,
Isolated lower layer's glycerine water solution；It weighs 10~20g acrylic acid to be fitted into dropping funel, is 30% hydroxide with mass fraction
Sodium solution adjusts acrylic acid degree of neutralization to 68~72%, then weighs 15~25g crystal and is fitted into three-necked flask, 50~60mL of addition
Water heats 30~40min at 60~70 DEG C, then the acrylic acid in dropping funel is instilled in three-necked flask, then toward three-necked flask
Middle addition 0.1~0.2g potassium peroxydisulfate after being stirred to react 1~2h continues that 1~2gN, N '-di-2-ethylhexylphosphine oxide are added into three-necked flask
8~10g glycerine water solution and 3~4g sodium methyl silicate are added into three-necked flask after the reaction was continued 3~4h, rises for acrylamide
Discharging is after temperature to 75~80 DEG C of the reaction was continued 1~2h to get the water-fast dust suppressant of soft film type.
Example 1
Filtrate is obtained by filtration in collection 50L black liquid first, obtains mixed liquor after filtrate and water are mixed by equal mass ratioes,
Mixed liquor is moved into reaction kettle and the calcium hydroxide of mixed liquor quality 10% is added into kettle, heating boils 30min, obtains calcification
Liquid is separated by filtration to obtain filter residue after calcifying solution is staticly settled 10h, and it is 10% sulphur that 5 times of mass fractions of its quality are added into filter residue
It is stirred to react 20min after acid, filters off sulfuric acid calcium precipitate, obtains pretreatment filtrates, then filter residue is added into pretreatment filtrates
Etc. quality sodium carbonate, move into water-bath and be stirred to react 2h at 90 DEG C, obtain filtered fluid after filtering removal precipitating, will filter
Liquid be put into concentrated by rotary evaporation in Rotary Evaporators to its original volume 1/3 concentrate, then that concentrate is put into refrigerator is cold at 4 DEG C
But it crystallizes, crystal is obtained by filtration, then measure and immediately rush warm milk when naturally cooling to 80 DEG C after the heating of 2L whole milk is boiled
Enter in stainless steel pallet, then pallet is put into refrigerator and stands 20min at 2 DEG C, takes out pallet, caused with tweezers tweezer tray surface
Close skin on boiled milk, then skin on boiled milk is fitted into enzymatic vessel, then the lipase of skin on boiled milk quality 1% and 1 times of skin on boiled milk quality go are added into tank
Ionized water will digest 6h in 30 DEG C of enzymatic vessel immigration of insulating box after being stirred 10min, take out zymolyte after enzymatic hydrolysis
And stratification 20min, isolated lower layer's glycerine water solution weigh 10g acrylic acid and are fitted into dropping funel, use mass fraction
Acrylic acid degree of neutralization is adjusted to 68% for 30% sodium hydroxide solution, then is weighed 15g crystal and is fitted into three-necked flask, addition 50mL water
30min is heated at 60 DEG C, then the acrylic acid in dropping funel is instilled in three-necked flask, then 0.1g is added into three-necked flask
Potassium peroxydisulfate after being stirred to react 1h continues that 1gN is added into three-necked flask, N '-methylene-bisacrylamide, after the reaction was continued 3h
8g glycerine water solution and 3g sodium methyl silicate are added into three-necked flask, discharging is after being warming up to 75 DEG C the reaction was continued 1h to get soft
Membranous type is water-fast dust suppressant.
Example 2
Filtrate is obtained by filtration in collection 55L black liquid first, obtains mixed liquor after filtrate and water are mixed by equal mass ratioes,
Mixed liquor is moved into reaction kettle and the calcium hydroxide of mixed liquor quality 10% is added into kettle, heating boils 33min, obtains calcification
Liquid is separated by filtration to obtain filter residue after calcifying solution is staticly settled 11h, and it is 10% sulphur that 5 times of mass fractions of its quality are added into filter residue
It is stirred to react 25min after acid, filters off sulfuric acid calcium precipitate, obtains pretreatment filtrates, then filter residue is added into pretreatment filtrates
Etc. quality sodium carbonate, move into water-bath and be stirred to react 2h at 93 DEG C, obtain filtered fluid after filtering removal precipitating, will filter
Liquid be put into concentrated by rotary evaporation in Rotary Evaporators to its original volume 1/3 concentrate, then that concentrate is put into refrigerator is cold at 5 DEG C
But it crystallizes, crystal is obtained by filtration, then measure and immediately rush warm milk when naturally cooling to 81 DEG C after the heating of 2L whole milk is boiled
Enter in stainless steel pallet, then pallet is put into refrigerator and stands 25min at 3 DEG C, takes out pallet, caused with tweezers tweezer tray surface
Close skin on boiled milk, then skin on boiled milk is fitted into enzymatic vessel, then the lipase of skin on boiled milk quality 1% and 1 times of skin on boiled milk quality go are added into tank
Ionized water will digest 7h in 35 DEG C of enzymatic vessel immigration of insulating box after being stirred 13min, take out zymolyte after enzymatic hydrolysis
And stratification 25min, isolated lower layer's glycerine water solution weigh 15g acrylic acid and are fitted into dropping funel, use mass fraction
Acrylic acid degree of neutralization is adjusted to 70% for 30% sodium hydroxide solution, then is weighed 20g crystal and is fitted into three-necked flask, addition 55mL water
35min is heated at 65 DEG C, then the acrylic acid in dropping funel is instilled in three-necked flask, then 0.1g is added into three-necked flask
Potassium peroxydisulfate after being stirred to react 1h continues that 1gN is added into three-necked flask, N '-methylene-bisacrylamide, after the reaction was continued 3h
9g glycerine water solution and 3g sodium methyl silicate are added into three-necked flask, discharging is after being warming up to 78 DEG C the reaction was continued 1h to get soft
Membranous type is water-fast dust suppressant.
Example 3
Filtrate is obtained by filtration in collection 60L black liquid first, obtains mixed liquor after filtrate and water are mixed by equal mass ratioes,
Mixed liquor is moved into reaction kettle and the calcium hydroxide of mixed liquor quality 10% is added into kettle, heating boils 35min, obtains calcification
Liquid is separated by filtration to obtain filter residue after calcifying solution is staticly settled 12h, and it is 10% sulphur that 6 times of mass fractions of its quality are added into filter residue
It is stirred to react 30min after acid, filters off sulfuric acid calcium precipitate, obtains pretreatment filtrates, then filter residue is added into pretreatment filtrates
Etc. quality sodium carbonate, move into water-bath and be stirred to react 3h at 95 DEG C, obtain filtered fluid after filtering removal precipitating, will filter
Liquid be put into concentrated by rotary evaporation in Rotary Evaporators to its original volume 1/3 concentrate, then that concentrate is put into refrigerator is cold at 6 DEG C
But it crystallizes, crystal is obtained by filtration, then measure and immediately rush warm milk when naturally cooling to 82 DEG C after the heating of 3L whole milk is boiled
Enter in stainless steel pallet, then pallet is put into refrigerator and stands 30min at 4 DEG C, takes out pallet, caused with tweezers tweezer tray surface
Close skin on boiled milk, then skin on boiled milk is fitted into enzymatic vessel, then the lipase of skin on boiled milk quality 1% and 2 times of skin on boiled milk quality go are added into tank
Ionized water will digest 8h in 40 DEG C of enzymatic vessel immigration of insulating box after being stirred 15min, take out zymolyte after enzymatic hydrolysis
And stratification 30min, isolated lower layer's glycerine water solution weigh 20g acrylic acid and are fitted into dropping funel, use mass fraction
Acrylic acid degree of neutralization is adjusted to 72% for 30% sodium hydroxide solution, then is weighed 25g crystal and is fitted into three-necked flask, addition 60mL water
40min is heated at 70 DEG C, then the acrylic acid in dropping funel is instilled in three-necked flask, then 0.2g is added into three-necked flask
Potassium peroxydisulfate after being stirred to react 2h continues that 2gN is added into three-necked flask, N '-methylene-bisacrylamide, after the reaction was continued 4h
10g glycerine water solution and 4g sodium methyl silicate are added into three-necked flask, discharging is after being warming up to 80 DEG C the reaction was continued 2h to get soft
Membranous type is water-fast dust suppressant.
The water-fast dust suppressant of soft film type made from example 1~3 and commercially available compound dust suppressant are subjected to live use respectively, and
Dust suppressant property is detected with performance, specifically used method are as follows: 1:500 in mass ratio stirs dust suppressant and water mixed
60s is closed, and uniformly mixed dust suppressant aqueous solution is injected in sprinkler, by 1.2L/m2Dosage, dust suppressant aqueous solution is equal
It is even to be sprayed at scattered coal heap surface layer, it finally stands and air-dries.
In conclusion the water-fast dust suppressant stability of soft film type produced by the present invention is strong, can be formed in coal surface after use
Cured layer, non-breakable after concussion, anti-dust effect is good, and water resistance is good, has broad application prospects.
Claims (4)
1. a kind of method for preparing the water-fast dust suppressant of soft film type using black liquid, it is characterised in that specific preparation step are as follows:
(1) it collects black liquid and filtrate is obtained by filtration, filtrate and water are mixed to get mixed liquor, hydroxide is added into mixed liquor
Calcium, heating boil 30~35min, obtain calcifying solution, be separated by filtration to obtain filter residue after calcifying solution is staticly settled 10~12h；
(2) it is stirred to react 20~30min after sulfuric acid being added into above-mentioned filter residue, sulfuric acid calcium precipitate is filtered off, is pre-processed
Filtrate, then sodium carbonate is added into pretreatment filtrates, it is stirred to react 2~3h at 90~95 DEG C, is obtained after filtering removal precipitating
Filtered fluid, 1/3 that filtered fluid is concentrated into its original volume obtains concentrate, then cools down knot under conditions of concentrate is placed on 4~6 DEG C
Crystal is obtained by filtration in crystalline substance, spare；
(3) warm milk is poured in stainless steel pallet immediately when naturally cooling to 80~82 DEG C after taking whole milk heating to boil,
Pallet is put into refrigerator again and stands 20~30min at 2~4 DEG C, takes out pallet, the densification formed with tweezers tweezer tray surface
Skin on boiled milk；
(4) skin on boiled milk obtained above is fitted into enzymatic vessel, then lipase and deionized water is added into tank, it is stirred 10~
After 15min will enzymatic vessel move into insulating box in digest, after enzymatic hydrolysis by zymolyte take out and stratification 20~
30min, isolated lower layer's glycerine water solution；
(5) it weighs 10~20g acrylic acid to be fitted into dropping funel, is that 30% sodium hydroxide solution adjusts acrylic acid with mass fraction
Degree of neutralization is to 68~72%, then weighs the spare crystal of 15~25g step (2) and be fitted into three-necked flask, be added 50~60mL water in
30~40min is heated at 60~70 DEG C, then the acrylic acid in dropping funel is instilled in three-necked flask, then is added into three-necked flask
Enter 0.1~0.2g potassium peroxydisulfate, after being stirred to react 1~2h continues that 1~2gN, N '-methylene bisacrylamide are added into three-necked flask
Amide is separately added into 8~10g glycerine water solution obtained above and 3~4g methyl into three-necked flask after the reaction was continued 3~4h
Sodium metasilicate, discharging is after being warming up to 75~80 DEG C the reaction was continued 1~2h to get the water-fast dust suppressant of soft film type.
2. a kind of method for preparing the water-fast dust suppressant of soft film type using black liquid according to claim 1, feature exist
In: the mass ratio of filtrate as described in step (1) and water is 1:1, and the additional amount of calcium hydroxide is the 10% of mixed liquor quality.
3. a kind of method for preparing the water-fast dust suppressant of soft film type using black liquid according to claim 1, feature exist
In: sulphuric acid described in step (2) is 5~6 times of filter residue quality, and the mass fraction of sulfuric acid is 10%, and sodium carbonate adds
It is equal with filter residue quality to enter amount.
4. a kind of method for preparing the water-fast dust suppressant of soft film type using black liquid according to claim 1, feature exist
In: the additional amount of lipase described in step (4) is the 1% of skin on boiled milk quality, and the additional amount of deionized water is the 1 of skin on boiled milk quality
~2 times, the temperature of insulating box is 30~40 DEG C, and enzymolysis time is 6~8h.
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| CN108219749A (en) * | 2017-12-12 | 2018-06-29 | 王敏 | A kind of preparation method of anti-freezing type road dust inhibitor |
| CN108251062A (en) * | 2017-12-30 | 2018-07-06 | 唐林元 | A kind of preparation method of long-acting stable water proof type dust suppressant |
| CN110105920B (en) * | 2019-06-04 | 2022-03-08 | 中国葛洲坝集团易普力股份有限公司 | Green high-efficiency mine pavement dust suppressant and preparation method thereof |
| CN110372883B (en) * | 2019-08-14 | 2021-01-01 | 南京工业大学 | Method for extracting lignin and silicic acid from black liquor |
| CN111574963A (en) * | 2020-06-29 | 2020-08-25 | 天津科技大学 | Degradable dust suppressant and preparation method thereof |
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| CN101638570A (en) * | 2008-07-28 | 2010-02-03 | 吉仁塔布 | Preparation method of binding agent capable of restraining swirling coal powder of coal train |
| CN101747866A (en) * | 2009-12-17 | 2010-06-23 | 中铁西北科学研究院有限公司 | Coal dust depressor and preparation method thereof |
| CN105950116A (en) * | 2016-05-04 | 2016-09-21 | 山东科技大学 | Environmentally-friendly coal transporting and stockpiling dust inhibitor and preparation method thereof |
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| US8066448B2 (en) * | 2009-03-31 | 2011-11-29 | Midwest Industrial Supply, Inc. | Dust suppression agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101638570A (en) * | 2008-07-28 | 2010-02-03 | 吉仁塔布 | Preparation method of binding agent capable of restraining swirling coal powder of coal train |
| CN101747866A (en) * | 2009-12-17 | 2010-06-23 | 中铁西北科学研究院有限公司 | Coal dust depressor and preparation method thereof |
| CN105950116A (en) * | 2016-05-04 | 2016-09-21 | 山东科技大学 | Environmentally-friendly coal transporting and stockpiling dust inhibitor and preparation method thereof |
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