CN103566899B - A kind of integrated conduct method of agricultural stalk - Google Patents
A kind of integrated conduct method of agricultural stalk Download PDFInfo
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Abstract
The invention discloses a kind of integrated conduct method of agricultural stalk, by agricultural stalk by obtaining liquid product and solid product after pre-treatment, pretreatment, carbonization treatment, wherein liquid product obtained coal water slurry dispersing agent product after condensation, sulfonating reaction, solid product obtains solid absorbent product through modified.The present invention effectively can avoid the waste water pollution problem that in prior art, Treating straw produces, and is used as coal water slurry dispersing agent, achieves good technique effect after the liquid product being rich in lignin being carried out condensation, sulfonating reaction; Meanwhile, the solid absorbent product that method of the present invention obtains, because course of reaction accurately controls, selects optimum technological parameter, has good adsorption effect, effectively can purify the anion in waste water, cationic pollutant.
Description
Technical field
The present invention relates to a kind of processing method of stalk, particularly relate to a kind of integrated conduct method of agricultural stalk, to prepare solid absorbent product and coal water slurry dispersing agent product.
Background technology
Since 2006, the whole nation from the leadership to the masses strengthens energy-saving and emission-reduction work, and State Council has issued the decision strengthening energy conservation, has formulated a series of policies and measures promoting energy-saving and emission-reduction, each department, all departments have made work arrangements in succession, and energy-saving and emission-reduction work achieves positive progress.But the whole nation did not realize the target of the energy-saving and cost-reducing and pollution emission reduction determined the beginning of the year in 2006, increase the difficulty of 4 years energy-conservation emission reduction works after Eleventh Five-Year Plan.More severe is, the first quarter in 2007, industry particularly highly energy-consuming, high pollution industry increase too fast, account for the electric power of national industrial energy consumption and sulfur dioxide (SO2) emissions nearly 70%, iron and steel, coloured, the large industry growth by 20.6% of building materials, PETROLEUM PROCESSING, chemical industry etc. six, accelerate 6.6 percentage points on year-on-year basis.Meanwhile, still there is the problems such as understanding is not in place, responsibility is indefinite, measure does not match, policy imperfection, input are not implemented, coordination is incapable in various work.
Country's " 12 planning " clearly proposes the target of energy-saving and emission-reduction, and namely by 2015, per GDP CO2 emission reduces by 17%; Per Unit GDP Energy Consumption declines 16%; Non-fossil energy accounts for primary energy consumption ratio and brings up again high 3.1 percentage points, from 8.3% to 11.4%; Total emissions of major pollutants reduces by the target of 8 to 10%.In addition, 12 " also specify that major pollutants control total class in planning, on Eleventh Five-Year Plan COD, these two classification bases of carbon dioxide, add the pollutant catabolic gene index of ammonia nitrogen and nitrogen oxide two classifications.The binding indicator that " 12 " planning proposes the definitely resolution that reduces discharging of national energy-saving.The major pollutants that State Council determines 5 aspects reduce discharging key project: one is attach most importance to urban wastewater treatment facility and supporting pipeline network construction, existing utility upgrading, specific resistance to filtration Facilities Construction, promotes denitrogenation dephosphorizing ability.Two is attach most importance to industries such as pulping and paper-making, printing and dyeing, food processing, agricultural byproducts processings, continues to strengthen water pollutions deep treatment and process and technology innovation.Three is advance desulphurization denitration engineering construction.Four is carry out agricultural sources prevention and cure of pollution.Five is control motor vehicle emission.
Agricultural stalk is the general name of ripe crops cauline leaf (fringe) part, is often referred to wheat, paddy rice, corn, potato class, oil plant, cotton, the remainder of sugarcane after results seed.The photosynthetic product of crops has over half being present in stalk.According to United Nations Environment Programme (UNEP) statistics, annual the produced stalk of the various crops planted in the world reaches 1,700,000,000 tons.
Stalk, as the common agricultural wastes in China rural area, has the advantages that distribution is wide, stock number is large.According to its chemical composition, stalk primarily of cellulose, hemicellulose and lignin composition, in addition containing a small amount of can by the ash content of the neutral fluxes such as water, ethanol, benzene or diluted acid, aqueous slkali extracting, can organic matter etc. be extracted.
Stalk is not only crops significant by-products, is also the important resources of production of industrial and agricultural production simultaneously.But at present, traditional burning, the also aspect such as field, feed are still mainly rested on to the process of stalk.Wherein, crop straw burning is in recent years all the more for people pay attention to.According to statistics, the annual stalk output in the whole world about 2,900,000,000 tons, wherein about has 66% direct returning to farmland or is burnt as domestic energy.Crop straw burning not only can produce CO, SO
2deng toxic and harmful, also can produce a large amount of pellets, bring harm to human health.In fact, crop straw burning not only brings environmental pollution, is also a kind of serious wasting of resources.The potential value of abundant excavation stalk, stalk is used as the raw material of industry, is the main development direction of straw utilization in recent years, and also this is the importance of the energy-saving and emission-reduction task implementing country 12 planning.
In prior art, CN102614853A is that a kind of adsorbent prepared by raw material with carbonaceous material, first carbonaceous material is immersed in metal chloride solutions, to be impregnated fully after carry out drying, then dried mixture is put into tube furnace and carries out carbonization-activation pore-creating and prepare compound adsorbent; Compound adsorbent after carbonization-activation is mixed with metal dust glass putty and aluminium powder, adds binding agent and stir, between the fin being then filled into metal fin pipe, dry; Metal fin pipe with adsorbent and metal dust is put into tube furnace sinter, by metal dust, adsorbent and metal fin pipe are sintered together.
CN102815699A discloses a kind of preparation method of Novel snow pine branch carbonaceous material, for adopting hydrothermal carbonization legal system for described cdear branch carbonaceous material, comprises the steps: that collecting cdear tree drops at the branch on ground, peeling; Branch after peeling is cut into segment, puts into the water being dissolved with appropriate citric acid and carry out hydrothermal carbonization reaction, the temperature of wherein hydrothermal carbonization reaction is 180 ~ 220 DEG C, and the reaction time is 28 ~ 32 hours; The reacted solution containing carbide is cooled rear also elimination solution naturally, carbide is washed final vacuum drying; Dried carbide is carried out grind rear acquisition described cdear branch carbonaceous material.
Meanwhile, also disclosed in prior art after stalk was carried out process and be used as environment conscious material, such as petroleum adsorbent, heavy metal absorbent etc.But, there is a large amount of lignin in the waste liquid of the method generation of the Treating straw existed in prior art, cause being difficult to administer, form secondary pollution, the technological deficiencies such as the adsorbent effect prepared is bad, do not have a kind of method of integrated treatment stalk in prior art.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of integrated conduct method of agricultural stalk, to overcome the problem of the generation waste liquor contamination existed in prior art, but turn waste into wealth, prepare coal water slurry dispersing agent and efficient solid absorbent product.
An integrated conduct method for agricultural stalk, is characterized in that, comprises the steps:
(1) pretreatment: agricultural stalk is carried out drying process, grind further with mixer after the agricultural stalk of drying is cut into segment, then 100 order sub-sieves are crossed, get the lower stalk of sub-sieve sieve and use washed with de-ionized water 2-3 times, use vavuum pump suction filtration afterwards until filtrate becomes clarification, the stalk powder obtained obtains pretreated stalk powder in drying baker after 55 DEG C of drying 24-48h;
(2) pre-treatment: pretreated stalk powder step (1) obtained uses the sodium hydroxide solution swollen process of 0.01-0.09mol/L, the swollen time is 48-64 hour, after swollen terminates, regulate pH to 6.6-7.4, after centrifugal filtration, use washed with de-ionized water 2-3 times, be then placed in drying baker in 65 DEG C of drying 24-48h; Obtain the stalk powder after pre-treatment;
(3) carbonization treatment: stalk powder, deionized water and the expoxy propane taken after the pre-treatment that step (2) obtains adds in reactor, sealing, pass into nitrogen 20-60min reactor internal residual gas is discharged, after again air inlet and valve of giving vent to anger being tightened, open magnetic stirring apparatus to stir, and logical cooling water protection magnetic stirring apparatus, by electronic oven, reactor is heated to 220-250 DEG C; After reaching reaction temperature, stop heating, first naturally cool to 180 DEG C, after pass into condensed water, until reactor is cooled to normal temperature; Then open reactor, product is obtained liquid product and solid product after suction filtration; Solid product, at 110-120 DEG C of drying 26-36h, obtains the solid material after carbonization treatment; The quality usage ratio of stalk powder, deionized water and expoxy propane wherein after the pre-treatment that obtains of step (2) is 5-20:500-1500:3-5;
(4) modification: 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride is dissolved in isopropanol-water mixed solution, form mixed solution A, then the solid material that step (3) obtains is joined in above-mentioned mixed solution A, wherein, 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride, the mass ratio of isopropyl alcohol and water is 5-10:16-23:200-230, the mass ratio of the solid material that 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and step (3) obtain is 1-3:5-10, gained mixture is at 30-65 DEG C, reaction 12-20h, after reaction terminates, the pH of reaction system is adjusted to 6.5-7, then filter obtained solution, the solid product after filtration uses washed with de-ionized water 2-3 times, then at 110-120 DEG C of dry 26-48h, obtains the solid product of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride modification,
Monoxone is dissolved in alcohol-water mixed solution, form mixed solution B, wherein, the mass ratio of monoxone, ethanol and water is 4-9:20-100:20-98, the solid product of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride modification is joined in mixed solution B, wherein, the solid product of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride modification and chloroacetic mass ratio are 5-10:6-12; Stirring reaction 13-24h at 40-80 DEG C; After reaction terminates, the pH of above-mentioned system is adjusted to 6.6-7.5; Then filter obtained solution, the solid product after filtration uses washed with de-ionized water 5-9 times, then at 110-115 DEG C of drying 30-72h, obtains solid absorbent product;
(5) coal water slurry dispersing agent is prepared: the pH of liquid product step (3) obtained is adjusted to 12-12.8, warming while stirring to 75 DEG C, drip formaldehyde and carry out condensation reaction 1-2h, then temperature is risen to 90 DEG C, add sodium sulfite and carry out sulfonating reaction 2-3h, be cooled to normal temperature discharging after reaction terminates, obtain coal water slurry dispersing agent product.
Further, described agricultural stalk is wheat stalk, rice straw, maize straw, cotton stalk or sugarcane stalk.
The integrated conduct method of a kind of agricultural stalk disclosed by the invention, effectively can avoid the waste water pollution problem that in prior art, Treating straw produces, the present invention is used as coal water slurry dispersing agent after the liquid product being rich in lignin being carried out condensation, sulfonating reaction, achieves good technique effect; Meanwhile, the solid absorbent product that method of the present invention obtains, because course of reaction accurately controls, selects optimum technological parameter, has good adsorption effect, effectively can purify the anion in waste water, cationic pollutant.
Accompanying drawing explanation
Fig. 1 is schematic flow sheet of the present invention.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further elaborated.
Embodiment 1
An integrated conduct method for agricultural stalk, is characterized in that, comprises the steps:
(1) pretreatment: wheat stalk is carried out drying process, grind further with mixer after the wheat stalk of drying is cut into segment, then 100 order sub-sieves are crossed, get the lower stalk of sub-sieve sieve and use washed with de-ionized water 2 times, use vavuum pump suction filtration afterwards until filtrate becomes clarification, the stalk powder obtained obtains pretreated stalk powder in drying baker after 55 DEG C of dry 48h;
(2) pre-treatment: pretreated stalk powder step (1) obtained uses the sodium hydroxide solution swollen process of 0.01mol/L, the swollen time is 48 hours, after swollen terminates, regulate pH to 6.6, after centrifugal filtration, use washed with de-ionized water 2 times, be then placed in drying baker in 65 DEG C of dry 24h; Obtain the stalk powder after pre-treatment;
(3) carbonization treatment: stalk powder, deionized water and the expoxy propane taken after the pre-treatment that step (2) obtains adds in reactor, sealing, pass into nitrogen 20min reactor internal residual gas is discharged, after again air inlet and valve of giving vent to anger being tightened, open magnetic stirring apparatus to stir, and logical cooling water protection magnetic stirring apparatus, by electronic oven, reactor is heated to 220 DEG C; After reaching reaction temperature, stop heating, first naturally cool to 180 DEG C, after pass into condensed water, until reactor is cooled to normal temperature; Then open reactor, product is obtained liquid product and solid product after suction filtration; Solid product, at 110 DEG C of dry 26h, obtains the solid material after carbonization treatment; The quality usage ratio of stalk powder, deionized water and expoxy propane wherein after the pre-treatment that obtains of step (2) is 5:1500:5;
(4) modification: 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride is dissolved in isopropanol-water mixed solution, form mixed solution A, then the solid material that step (3) obtains is joined in above-mentioned mixed solution A, wherein, the mass ratio of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride, isopropyl alcohol and water is 5:23:230, the mass ratio of the solid material that 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and step (3) obtain is 1:10, gained mixture is at 30 DEG C, reaction 12h, is adjusted to 6.5 by the pH of reaction system after reaction terminates; Then filter obtained solution, the solid product after filtration uses washed with de-ionized water 2 times, then at 110 DEG C of dry 26h, obtains the solid product of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride modification;
Monoxone is dissolved in alcohol-water mixed solution, form mixed solution B, wherein, the mass ratio of monoxone, ethanol and water is 4:100:98, the solid product of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride modification is joined in mixed solution B, wherein, the solid product of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride modification and chloroacetic mass ratio are 5:12; Stirring reaction 13h at 40 DEG C; After reaction terminates, the pH of above-mentioned system is adjusted to 6.6; Then filter obtained solution, the solid product after filtration uses washed with de-ionized water 5 times, then at 110 DEG C of dry 30h, obtains solid absorbent product;
(5) coal water slurry dispersing agent is prepared: the pH of liquid product step (3) obtained is adjusted to 12, warming while stirring to 75 DEG C, drip formaldehyde and carry out condensation reaction 1h, then temperature is risen to 90 DEG C, add sodium sulfite and carry out sulfonating reaction 2h, be cooled to normal temperature discharging after reaction terminates, obtain coal water slurry dispersing agent product.
Embodiment 2
An integrated conduct method for maize straw, is characterized in that, comprises the steps:
(1) pretreatment: maize straw is carried out drying process, grind further with mixer after the maize straw of drying is cut into segment, then 100 order sub-sieves are crossed, get the lower stalk of sub-sieve sieve and use washed with de-ionized water 3 times, use vavuum pump suction filtration afterwards until filtrate becomes clarification, the stalk powder obtained obtains pretreated stalk powder in drying baker after 55 DEG C of dry 48h;
(2) pre-treatment: pretreated stalk powder step (1) obtained uses the sodium hydroxide solution swollen process of 0.09mol/L, the swollen time is 64 hours, after swollen terminates, regulate pH to 7.4, after centrifugal filtration, use washed with de-ionized water 3 times, be then placed in drying baker in 65 DEG C of dry 48h; Obtain the stalk powder after pre-treatment;
(3) carbonization treatment: stalk powder, deionized water and the expoxy propane taken after the pre-treatment that step (2) obtains adds in reactor, sealing, pass into nitrogen 60min reactor internal residual gas is discharged, after again air inlet and valve of giving vent to anger being tightened, open magnetic stirring apparatus to stir, and logical cooling water protection magnetic stirring apparatus, by electronic oven, reactor is heated to 250 DEG C; After reaching reaction temperature, stop heating, first naturally cool to 180 DEG C, after pass into condensed water, until reactor is cooled to normal temperature; Then open reactor, product is obtained liquid product and solid product after suction filtration; Solid product, at 120 DEG C of dry 36h, obtains the solid material after carbonization treatment; The quality usage ratio of stalk powder, deionized water and expoxy propane wherein after the pre-treatment that obtains of step (2) is 20:500:3;
(4) modification: 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride is dissolved in isopropanol-water mixed solution, form mixed solution A, then the solid material that step (3) obtains is joined in above-mentioned mixed solution A, wherein, the mass ratio of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride, isopropyl alcohol and water is 10:16:200, the mass ratio of the solid material that 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and step (3) obtain is 3:5, gained mixture is at 65 DEG C, reaction 20h, is adjusted to 7 by the pH of reaction system after reaction terminates; Then filter obtained solution, the solid product after filtration uses washed with de-ionized water 3 times, then at 120 DEG C of dry 48h, obtains the solid product of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride modification;
Monoxone is dissolved in alcohol-water mixed solution, form mixed solution B, wherein, the mass ratio of monoxone, ethanol and water is 9:20:20, the solid product of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride modification is joined in mixed solution B, wherein, the solid product of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride modification and chloroacetic mass ratio are 10:6; Stirring reaction 24h at 80 DEG C; After reaction terminates, the pH of above-mentioned system is adjusted to 7.5; Then filter obtained solution, the solid product after filtration uses washed with de-ionized water 9 times, then at 115 DEG C of dry 72h, obtains solid absorbent product;
(5) coal water slurry dispersing agent is prepared: the pH of liquid product step (3) obtained is adjusted to 12.8, warming while stirring to 75 DEG C, drip formaldehyde and carry out condensation reaction 2h, then temperature is risen to 90 DEG C, add sodium sulfite and carry out sulfonating reaction 3h, be cooled to normal temperature discharging after reaction terminates, obtain coal water slurry dispersing agent product.
Embodiment 3
An integrated conduct method for sugarcane stalk, is characterized in that, comprises the steps:
(1) pretreatment: sugarcane stalk is carried out drying process, grind further with mixer after the sugarcane stalk of drying is cut into segment, then 100 order sub-sieves are crossed, get the lower stalk of sub-sieve sieve and use washed with de-ionized water 3 times, use vavuum pump suction filtration afterwards until filtrate becomes clarification, the stalk powder obtained obtains pretreated stalk powder in drying baker after 55 DEG C of dry 48h;
(2) pre-treatment: pretreated stalk powder step (1) obtained uses the sodium hydroxide solution swollen process of 0.08mol/L, the swollen time is 50 hours, after swollen terminates, regulate pH to 7, after centrifugal filtration, use washed with de-ionized water 3 times, be then placed in drying baker in 65 DEG C of dry 40h; Obtain the stalk powder after pre-treatment;
(3) carbonization treatment: stalk powder, deionized water and the expoxy propane taken after the pre-treatment that step (2) obtains adds in reactor, sealing, pass into nitrogen 40min reactor internal residual gas is discharged, after again air inlet and valve of giving vent to anger being tightened, open magnetic stirring apparatus to stir, and logical cooling water protection magnetic stirring apparatus, by electronic oven, reactor is heated to 240 DEG C; After reaching reaction temperature, stop heating, first naturally cool to 180 DEG C, after pass into condensed water, until reactor is cooled to normal temperature; Then open reactor, product is obtained liquid product and solid product after suction filtration; Solid product, at 114 DEG C of dry 30h, obtains the solid material after carbonization treatment; The quality usage ratio of stalk powder, deionized water and expoxy propane wherein after the pre-treatment that obtains of step (2) is 15:600:4;
(4) modification: 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride is dissolved in isopropanol-water mixed solution, form mixed solution A, then the solid material that step (3) obtains is joined in above-mentioned mixed solution A, wherein, the mass ratio of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride, isopropyl alcohol and water is 8:20:210, the mass ratio of the solid material that 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and step (3) obtain is 2:6, gained mixture is at 50 DEG C, reaction 16h, is adjusted to 6.8 by the pH of reaction system after reaction terminates; Then filter obtained solution, the solid product after filtration uses washed with de-ionized water 3 times, then at 115 DEG C of dry 30h, obtains the solid product of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride modification;
Monoxone is dissolved in alcohol-water mixed solution, form mixed solution B, wherein, the mass ratio of monoxone, ethanol and water is 8:50:60, the solid product of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride modification is joined in mixed solution B, wherein, the solid product of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride modification and chloroacetic mass ratio are 7:10; Stirring reaction 20h at 70 DEG C; After reaction terminates, the pH of above-mentioned system is adjusted to 7; Then filter obtained solution, the solid product after filtration uses washed with de-ionized water 8 times, then at 112 DEG C of drying 30-72h, obtains solid absorbent product;
(5) coal water slurry dispersing agent is prepared: the pH of liquid product step (3) obtained is adjusted to 12.6, warming while stirring to 75 DEG C, drip formaldehyde and carry out condensation reaction 2h, then temperature is risen to 90 DEG C, add sodium sulfite and carry out sulfonating reaction 1.6h, be cooled to normal temperature discharging after reaction terminates, obtain coal water slurry dispersing agent product.
The solid absorbent product obtained by embodiment 1-3 carries out absorption test to the copper ion in waste water, and the result after absorption test is as shown in table 1.Table 1 is the absorption test result of embodiment 1-3 to Cu in waste water ion.
As shown in Table 1, the solid absorbent product for preparing of embodiment of the present invention 1-3 all has good adsorption effect to Cu in waste water ion.
Although above-described embodiment is to invention has been detailed description; but it is only the present invention's part embodiment; instead of whole embodiment, people can also obtain other embodiments according to the present embodiment under without creative prerequisite, and these embodiments all belong to protection scope of the present invention.
Claims (2)
1. an integrated conduct method for agricultural stalk, is characterized in that, comprises the steps:
(1) pretreatment: agricultural stalk is carried out drying process, grind further with mixer after the agricultural stalk of drying is cut into segment, then 100 order sub-sieves are crossed, get the lower stalk of sub-sieve sieve and use washed with de-ionized water 2-3 time, use vavuum pump suction filtration afterwards until filtrate becomes clarification, the stalk powder obtained obtains pretreated stalk powder in drying baker after 55 DEG C of dry 24-48h;
(2) pre-treatment: pretreated stalk powder step (1) obtained uses the sodium hydroxide solution swollen process of 0.01-0.09mol/L, the swollen time is 48-64 hour, after swollen terminates, regulate pH to 6.6-7.4, after centrifugal filtration, use washed with de-ionized water 2-3 time, be then placed in drying baker in 65 DEG C of dry 24-48h; Obtain the stalk powder after pre-treatment;
(3) carbonization treatment: stalk powder, deionized water and the expoxy propane taken after the pre-treatment that step (2) obtains adds in reactor, sealing, pass into nitrogen 20-60min reactor internal residual gas is discharged, after again air inlet and valve of giving vent to anger being tightened, open magnetic stirring apparatus to stir, and logical cooling water protection magnetic stirring apparatus, by electronic oven, reactor is heated to 220-250 DEG C; After reaching reaction temperature, stop heating, first naturally cool to 180 DEG C, after pass into condensed water, until reactor is cooled to normal temperature; Then open reactor, product is obtained liquid product and solid product after suction filtration; Solid product, at 110-120 DEG C of dry 26-36h, obtains the solid material after carbonization treatment; The quality usage ratio of stalk powder, deionized water and expoxy propane wherein after the pre-treatment that obtains of step (2) is 5-20: 500-1500: 3-5;
(4) modification: 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride is dissolved in isopropanol-water mixed solution, form mixed solution A, then the solid material that step (3) obtains is joined in above-mentioned mixed solution A, wherein, 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride, the mass ratio of isopropyl alcohol and water is 5-10: 16-23: 200-230, the mass ratio of the solid material that 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and step (3) obtain is 1-3: 5-10, gained mixture is at 30-65 DEG C, reaction 12-20h, after reaction terminates, the pH of reaction system is adjusted to 6.5-7, then filter obtained solution, the solid product after filtration uses washed with de-ionized water 2-3 time, then at 110-120 DEG C of dry 26-48h, obtains the solid product of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride modification,
Monoxone is dissolved in alcohol-water mixed solution, form mixed solution B, wherein, the mass ratio of monoxone, ethanol and water is 4-9: 20-100: 20-98, the solid product of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride modification is joined in mixed solution B, wherein, the solid product of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride modification and chloroacetic mass ratio are 5-10: 6-12; Stirring reaction 13-24h at 40-80 DEG C; After reaction terminates, the pH of above-mentioned system is adjusted to 6.6-7.5; Then filter obtained solution, the solid product after filtration uses washed with de-ionized water 5-9 time, then at 110-115 DEG C of dry 30-72h, obtains solid absorbent product;
(5) coal water slurry dispersing agent is prepared: the pH of liquid product step (3) obtained is adjusted to 12-12.8, warming while stirring to 75 DEG C, drip formaldehyde and carry out condensation reaction 1-2h, then temperature is risen to 90 DEG C, add sodium sulfite and carry out sulfonating reaction 2-3h, be cooled to normal temperature discharging after reaction terminates, obtain coal water slurry dispersing agent product.
2. method according to claim 1, described agricultural stalk is wheat stalk, rice straw, maize straw, cotton stalk or sugarcane stalk.
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| US20110056125A1 (en) * | 2008-04-17 | 2011-03-10 | Csl Carbon Solutions Ltd. | Process for converting biomass to coal-like material using hydrothermal carbonisation |
| US8414664B2 (en) * | 2009-03-02 | 2013-04-09 | HydoChar LLC | Algal coal and process for preparing same |
| CN102626608A (en) * | 2012-04-16 | 2012-08-08 | 南京大学 | Straw modified into amphiprotic adsorbent and preparation method thereof |
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| CN105148849B (en) | 2017-11-07 |
| CN105148849A (en) | 2015-12-16 |
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