CN107794048A - A kind of attapulgite/lignite compounding absorbent-type soil oxygenation agent and preparation method thereof - Google Patents
A kind of attapulgite/lignite compounding absorbent-type soil oxygenation agent and preparation method thereof Download PDFInfo
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- CN107794048A CN107794048A CN201710887645.5A CN201710887645A CN107794048A CN 107794048 A CN107794048 A CN 107794048A CN 201710887645 A CN201710887645 A CN 201710887645A CN 107794048 A CN107794048 A CN 107794048A
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- C09K17/40—Soil-conditioning materials or soil-stabilising materials containing mixtures of inorganic and organic compounds
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Abstract
The invention provides a kind of attapulgite/lignite compounding absorbent-type soil oxygenation agent and preparation method thereof, it is by after the oxidized ammonolysis reaction processing of lignite, extract lignite humic acid, then sulfonation processing is carried out to lignite humic acid using sodium sulfite as sulfonating agent, afterwards using acrylic acid, acrylamide and lignite sulfonated humic acid as raw material, lignite sulfonated humic acid base high hydroscopic resin has been synthesized using water solution polymerization process;Concave-convex clay rod and SODIUM PERCARBONATE are pressed into particle, is coated afterwards using above-mentioned high hydroscopic resin, obtains soil oxygenation agent.
Description
Technical field
The invention belongs to agriculture and forestry means of production preparation field, and in particular to a kind of attapulgite/lignite compounding absorbent-type
Soil oxygenation agent and preparation method thereof.
Technical background
Lignite is the low-order coal that degree of coalification is only above peat, is characterized in moisture height, and carbon content is low, and oxygen content is high, hair
Heat is low, and chemical reactivity is strong, and mechanical strength is low.The main distinction of lignite and other coals is that lignite contains to some extent
There is humic acid, particularly primary humic acid.Humic acid is a kind of by one or more condensed ring aromatic cores, and composition is connected by bridged bond
Natural macromolecular mixture, be form agron main component, because humic acid have bioactivity, ion exchangeable,
Hydrophily, faintly acid, Absorptive complex wave etc. are widely used in the fields such as agricultural, agricultural chemicals, fertilizer.
Moisture is one of most significant feature of lignite greatly, and the moisture in lignite is highest in all kinds of coals, total moisture one
As can reach 10%-40%, because of its surface hydrophilic group -- the presence of oxygen-containing functional group, make lignite that there are multiple water absorbing properties.
Water-loss reducer is a kind of new functional macromolecule material, has appropriately crosslinked tridimensional network, can absorb it certainly
The water that thousands of times of body quality.Water-loss reducer is mixed with soil, rainwater and irrigation water can not only be firmly pinned, may additionally facilitate soil
The formation of crumb structure, improve the gas permeability of soil, but its cost is higher, salt tolerance it is poor limit its in agricultural extensively should
With.
Tian Yuchuan, Sima Yi Nuerla et al. are at it《The synthesis of acrylic acid-sulfonated humic acid water-absorbing resin》In one text,
Sulfonation is carried out to humic acid using oleum, and height has been synthesized for raw material with acrylic acid (AA) and sulfonated humic acid (SHA)
AA-SHA copolymers [P (AA-SHA)] water-absorbing resin of SHA contents.
The content of the invention
For problems of the prior art, the present invention provides a kind of attapulgite/lignite compounding absorbent-type soil and increased
Oxygen agent and preparation method thereof.
To realize the purpose of the present invention, the invention provides following technical scheme:
A kind of preparation method of attapulgite/lignite compounding absorbent-type soil oxygenation agent, is by the oxidized ammonolysis reaction of lignite
After reason, lignite humic acid is extracted, sulfonation processing then is carried out to lignite humic acid using sodium sulfite as sulfonating agent, afterwards with propylene
Acid, acrylamide and lignite sulfonated humic acid are raw material, and the high suction of lignite sulfonated humic acid base has been synthesized using water solution polymerization process
Water-resin;Concave-convex clay rod and SODIUM PERCARBONATE are pressed into particle, is coated, obtained using above-mentioned high hydroscopic resin afterwards
Soil oxygenation agent.
Concrete technology step is as follows:
(1)The oxidative ammonolysis reaction of lignite:
Lignite be crushed into 60 mesh sieves, impurity is rinsed 2-3 times with running water, deionized water respectively afterwards, be placed on gas afterwards
In solid-liquid phase reaction device, 10% concentrated ammonia liquor and water are added, starts stirring, oxygen is passed through after being warming up to 90-130 DEG C, maintain oxygen
0.2-0.5MPa is pressed in, under 700-900r/min speed conditions, reacts 2-4 hours, is changed after reaction through filtering, drying acquisition nitrogen
Property lignite;
(2)The extraction of lignite humic acid:
Weigh step(1)Lignite sample after processing, the sodium hydroxide solution of mass fraction 1.5% is added in 1/10 ratio,
The magnetic agitation 0.5-2 hours in 40-60 DEG C of water bath with thermostatic control, centrifuged, collected with 3500-4500r/min rotating speed afterwards
Filtrate, is then washed with deionized residue 2-3 times, merges above-mentioned filtrate, and filtrate is precipitated with salt acid for adjusting pH to brownish black analyses
Go out, filtered with Buchner funnel, precipitation is washed with deionized 2-3 times, filter cake is dried in 50-65 DEG C of air blower;
(3)Sulfonation is handled:
By solid-to-liquid ratio 1:15, the sodium hydroxide solution of use quality fraction 1.5% is by step(2)The lignite humic acid dissolving of extraction,
Sodium humate solution is obtained, under the conditions of 45-55 DEG C, according to sulfonating agent solid-to-liquid ratio 1:10 add sulfurous acid into above-mentioned solution
Sodium, 1-2 hours are reacted, obtain lignite sulfonated humic acid sodium solution;
(4)Polymerisation prepares high hydroscopic resin:
Weigh in acrylamide, crosslinking agent N-N methylene-bisacrylamides input reaction bulb, pH is to neutrality for regulation, in ice-water bath
Under the conditions of add a small amount of deionized water stirring and dissolving, add above-mentioned lignite sulfonated humic acid sodium solution, after being uniformly mixed,
Acrylic acid is slowly added under the conditions of 0-5 DEG C, by initiator potassium persulfate with being added to after deionized water dissolving in above-mentioned reaction solution,
It is passed through N2, the magnetic agitation 15-28 minutes at 35-45 DEG C of temperature, 75-85 DEG C is started to warm up afterwards, until generation glue dough
Stop reaction when matter can not stir, lignite sulfonated humic acid base high hydroscopic resin is made;
(5)Crushed after Concave-convex clay rod is mixed with SODIUM PERCARBONATE, grain fineness≤0.15mm after crushing, after crushing
Mixture input pressure machine be pressed into particle, grain graininess is controlled in 1-20mm;
(6)By step(5)Obtained particle preheating, 40-50 DEG C of preheating temperature, is sent into rotary drum coating machine, by paraffin even spread
In the surface of material of motion, then by conveyer belt by the step after crushing(4)High hydroscopic resin particle is dispersed evenly in motion
Surface of material, be allowed to be bonded to surface of material, after cooling, produce soil oxygenation agent product.
Wherein, the mass ratio of acrylic acid, acrylamide and lignite sulfonated humic acid is 2-3:1:1-2.
Wherein, the dosage of described initiator potassium persulfate is the 1-3% of unit gross mass.
Wherein, the dosage of described crosslinking agent N-N methylene-bisacrylamides is the 2-5% of unit gross mass.
Compared with prior art, the present invention has advantages below:
(1)Lignite directly in use, its nitrogen content it is low (<1%), C/N is than high (generally>80), acid big, misapplication on the contrary can
Plant growth is hindered, reduces validity of soil nitrogen etc., therefore the present invention carries out oxidative ammonolysis reaction, extraction to lignite first
Lignite humic acid, the phenylpropyl alcohol alkane cyclic structure of lignite molecule is broken in the presence of oxidant, formed more carboxyls and
Carbonyl, lignite humic acid surface active groups are improved, improve its multiple water absorbing properties.
(2)Using sulfonating agent sodium sulfite to lignite humic acid carry out sulfonation processing, improve its hydrophilicity, afterwards with height
Molecule monomer acrylic acid/acrylamide graft copolymerization, it is prepared for lignite sulfonated humic acid base high hydroscopic resin, product tool of the present invention
Having the advantages that salt resistant character is strong, water absorbent rate is high, rate of water absorption is fast, the addition of humic acid improves the salt resistant character of water-loss reducer,
The active group of other humic acid has stronger complexing power and higher adsorption capacity, thorn to various trace elements in soil
The effect of swashing growth and development of plants, improving soil granular structure and adjust plant nutrient situation.
(3)The present invention is coated using high hydroscopic resin to SODIUM PERCARBONATE, SODIUM PERCARBONATE is slowly decomposed, and is released double
Oxygen water and sodium carbonate, decomposing hydrogen dioxide solution releases oxygen and heat, nonpoisonous and tasteless, moreover it is possible to sterilizes, sterilizes, ensures plant health life
It is long, improve operating efficiency.
Embodiment
A kind of preparation method of attapulgite/lignite compounding absorbent-type soil oxygenation agent, is that the oxidized ammonolysis of lignite is anti-
After should handling, extract lignite humic acid, then using sodium sulfite be sulfonating agent to lignite humic acid progress sulfonation processing, afterwards with
Acrylic acid, acrylamide and lignite sulfonated humic acid are raw material, and lignite sulfonated humic acid base has been synthesized using water solution polymerization process
High hydroscopic resin;Concave-convex clay rod and SODIUM PERCARBONATE are pressed into particle, coated afterwards using above-mentioned high hydroscopic resin,
Obtain soil oxygenation agent.
Concrete technology step is as follows:
(1)The oxidative ammonolysis reaction of lignite:
Lignite be crushed into 60 mesh sieves, impurity is rinsed 3 times with running water, deionized water respectively afterwards, be placed on gas-solid afterwards
In liquid phase reaction device, 10% concentrated ammonia liquor and water are added, starts stirring, oxygen is passed through after being warming up to 110 DEG C, maintain oxygen to be pressed in
0.3MPa, under 800r/min speed conditions, react 3 hours, nitrogen modification lignite is obtained through filtering, drying after reaction;
(2)The extraction of lignite humic acid:
Weigh step(1)Lignite sample after processing, the sodium hydroxide solution of mass fraction 1.5% is added in 1/10 ratio,
Magnetic agitation 1.5 hours in 50 DEG C of waters bath with thermostatic control, centrifuged afterwards with 4000r/min rotating speed, collect filtrate, Ran Houyong
Deionized water washing residue 3 times, merges above-mentioned filtrate, filtrate, to brownish black Precipitation, uses Buchner funnel with salt acid for adjusting pH
Filter, precipitation is washed with deionized 3 times, filter cake is dried in 60 DEG C of air blowers;
(3)Sulfonation is handled:
By solid-to-liquid ratio 1:15, the sodium hydroxide solution of use quality fraction 1.5% is by step(2)The lignite humic acid dissolving of extraction,
Sodium humate solution is obtained, under the conditions of 50 DEG C, according to sulfonating agent solid-to-liquid ratio 1:10 add sodium sulfite into above-mentioned solution, instead
Answer 1.5 hours, obtain lignite sulfonated humic acid sodium solution;
(4)Polymerisation prepares high hydroscopic resin:
Weigh in acrylamide, crosslinking agent N-N methylene-bisacrylamides input reaction bulb, pH is to neutrality for regulation, in ice-water bath
Under the conditions of add a small amount of deionized water stirring and dissolving, add above-mentioned lignite sulfonated humic acid sodium solution, after being uniformly mixed,
Acrylic acid is slowly added under the conditions of 0-5 DEG C, by initiator potassium persulfate with being added to after deionized water dissolving in above-mentioned reaction solution,
It is passed through N2, magnetic agitation 20 minutes, starts to warm up 80 DEG C afterwards at 40 DEG C of temperature, until generation glue granulated substance can not stir
When stop reaction, lignite sulfonated humic acid base high hydroscopic resin is made;
(5)Crushed after Concave-convex clay rod is mixed with SODIUM PERCARBONATE, grain fineness≤0.15mm after crushing, after crushing
Mixture input pressure machine be pressed into particle, grain graininess is controlled in 1-20mm;
(6)By step(5)Obtained particle preheating, 43 DEG C of preheating temperature, is sent into rotary drum coating machine, paraffin is spread evenly across into fortune
Dynamic surface of material, then by conveyer belt by the step after crushing(4)High hydroscopic resin particle is dispersed evenly to the thing in motion
Expect surface, be allowed to be bonded to surface of material, after cooling, produce soil oxygenation agent product.
Wherein, the mass ratio of acrylic acid, acrylamide and lignite sulfonated humic acid is 2-3:1:1-2.
Wherein, the dosage of described initiator potassium persulfate is the 1-3% of unit gross mass.
Wherein, the dosage of described crosslinking agent N-N methylene-bisacrylamides is the 2-5% of unit gross mass.
Claims (5)
1. the preparation method of a kind of attapulgite/lignite compounding absorbent-type soil oxygenation agent, it is characterised in that be through oxygen by lignite
After changing ammonolysis reaction processing, lignite humic acid is extracted, then lignite humic acid is carried out at sulfonation using sodium sulfite as sulfonating agent
Reason, afterwards using acrylic acid, acrylamide and lignite sulfonated humic acid as raw material, lignite sulfonation has been synthesized using water solution polymerization process
Humic acid base high hydroscopic resin;Concave-convex clay rod and SODIUM PERCARBONATE are pressed into particle, afterwards using above-mentioned high hydroscopic resin
Coated, obtain soil oxygenation agent.
2. a kind of preparation method of attapulgite/lignite compounding absorbent-type soil oxygenation agent according to claims 1, its
It is characterised by, concrete technology step is as follows:
(1)The oxidative ammonolysis reaction of lignite:
Lignite be crushed into 60 mesh sieves, impurity is rinsed 2-3 times with running water, deionized water respectively afterwards, be placed on gas afterwards
In solid-liquid phase reaction device, 10% concentrated ammonia liquor and water are added, starts stirring, oxygen is passed through after being warming up to 90-130 DEG C, maintain oxygen
0.2-0.5MPa is pressed in, under 700-900r/min speed conditions, reacts 2-4 hours, is changed after reaction through filtering, drying acquisition nitrogen
Property lignite;
(2)The extraction of lignite humic acid:
Weigh step(1)Lignite sample after processing, the sodium hydroxide solution of mass fraction 1.5% is added in 1/10 ratio,
The magnetic agitation 0.5-2 hours in 40-60 DEG C of water bath with thermostatic control, centrifuged, collected with 3500-4500r/min rotating speed afterwards
Filtrate, is then washed with deionized residue 2-3 times, merges above-mentioned filtrate, and filtrate is precipitated with salt acid for adjusting pH to brownish black analyses
Go out, filtered with Buchner funnel, precipitation is washed with deionized 2-3 times, filter cake is dried in 50-65 DEG C of air blower;
(3)Sulfonation is handled:
By solid-to-liquid ratio 1:15, the sodium hydroxide solution of use quality fraction 1.5% is by step(2)The lignite humic acid dissolving of extraction,
Sodium humate solution is obtained, under the conditions of 45-55 DEG C, according to sulfonating agent solid-to-liquid ratio 1:10 add sulfurous acid into above-mentioned solution
Sodium, 1-2 hours are reacted, obtain lignite sulfonated humic acid sodium solution;
(4)Polymerisation prepares high hydroscopic resin:
Weigh in acrylamide, crosslinking agent N-N methylene-bisacrylamides input reaction bulb, pH is to neutrality for regulation, in ice-water bath
Under the conditions of add a small amount of deionized water stirring and dissolving, add above-mentioned lignite sulfonated humic acid sodium solution, after being uniformly mixed,
Acrylic acid is slowly added under the conditions of 0-5 DEG C, by initiator potassium persulfate with being added to after deionized water dissolving in above-mentioned reaction solution,
It is passed through N2, the magnetic agitation 15-28 minutes at 35-45 DEG C of temperature, 75-85 DEG C is started to warm up afterwards, until generation glue dough
Stop reaction when matter can not stir, lignite sulfonated humic acid base high hydroscopic resin is made;
(5)Crushed after Concave-convex clay rod is mixed with SODIUM PERCARBONATE, grain fineness≤0.15mm after crushing, after crushing
Mixture input pressure machine be pressed into particle, grain graininess is controlled in 1-20mm;
(6)By step(5)Obtained particle preheating, 40-50 DEG C of preheating temperature, is sent into rotary drum coating machine, by paraffin even spread
In the surface of material of motion, then by conveyer belt by the step after crushing(4)High hydroscopic resin particle is dispersed evenly in motion
Surface of material, be allowed to be bonded to surface of material, after cooling, produce soil oxygenation agent product.
3. a kind of preparation method of attapulgite/lignite compounding absorbent-type soil oxygenation agent according to claims 1,2,
Characterized in that, the mass ratio of acrylic acid, acrylamide and lignite sulfonated humic acid is 2-3:1:1-2.
4. a kind of preparation method of attapulgite/lignite compounding absorbent-type soil oxygenation agent according to claims 2, its
It is characterised by, the dosage of described initiator potassium persulfate is the 1-3% of unit gross mass.
5. a kind of preparation method of attapulgite/lignite compounding absorbent-type soil oxygenation agent according to claims 2, its
It is characterised by, the dosage of described crosslinking agent N-N methylene-bisacrylamides is the 2-5% of unit gross mass.
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CN111233573A (en) * | 2020-01-19 | 2020-06-05 | 浙江丰瑜生态科技股份有限公司 | Newly-reclaimed rice field soil improvement humic acid compound fertilizer and preparation method thereof |
CN111233550A (en) * | 2020-01-19 | 2020-06-05 | 浙江丰瑜生态科技股份有限公司 | Humic acid water-soluble fertilizer suitable for hickory planting and preparation method and application thereof |
CN112500865A (en) * | 2020-12-17 | 2021-03-16 | 江苏植丰生物科技有限公司 | Alkaline soil remediation microbial inoculum and preparation method thereof |
CN115322790A (en) * | 2022-08-03 | 2022-11-11 | 国能朗新明环保科技有限公司 | Matrix modifier for coal mine refuse dump and preparation method thereof |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111233573A (en) * | 2020-01-19 | 2020-06-05 | 浙江丰瑜生态科技股份有限公司 | Newly-reclaimed rice field soil improvement humic acid compound fertilizer and preparation method thereof |
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CN111233550B (en) * | 2020-01-19 | 2021-11-23 | 浙江丰瑜生态科技股份有限公司 | Humic acid water-soluble fertilizer suitable for hickory planting and preparation method and application thereof |
CN111233573B (en) * | 2020-01-19 | 2021-11-30 | 浙江丰瑜生态科技股份有限公司 | Newly-reclaimed rice field soil improvement humic acid compound fertilizer and preparation method thereof |
CN112500865A (en) * | 2020-12-17 | 2021-03-16 | 江苏植丰生物科技有限公司 | Alkaline soil remediation microbial inoculum and preparation method thereof |
CN115322790A (en) * | 2022-08-03 | 2022-11-11 | 国能朗新明环保科技有限公司 | Matrix modifier for coal mine refuse dump and preparation method thereof |
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