CN111040820B - Processing technology for improving flame-retardant biomass particles by utilizing micro-nano steam explosion slag - Google Patents
Processing technology for improving flame-retardant biomass particles by utilizing micro-nano steam explosion slag Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L5/00—Solid fuels
- C10L5/40—Solid fuels essentially based on materials of non-mineral origin
- C10L5/44—Solid fuels essentially based on materials of non-mineral origin on vegetable substances
- C10L5/445—Agricultural waste, e.g. corn crops, grass clippings, nut shells or oil pressing residues
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L2230/00—Function and purpose of a components of a fuel or the composition as a whole
- C10L2230/22—Function and purpose of a components of a fuel or the composition as a whole for improving fuel economy or fuel efficiency
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel
Abstract
The invention discloses a biomass particle for improving flame resistance by utilizing micro-nano steam explosion slag and a processing technology thereof, belonging to the technical field of biomass energy. Mixing sodium alginate with water, standing for swelling, heating, stirring and dissolving, adding sodium periodate, heating for reaction to obtain modified sodium alginate liquid, adjusting pH of the modified steam exploded slag, oleic acid, lipase, xylitol and the modified sodium alginate liquid, heating, stirring for reaction, adding calcium nitrate solution, stirring and mixing, granulating, performing freeze-thaw cycle to obtain a blank, stirring and mixing zinc polyacrylate resin, xylene and n-butyl alcohol, adding the blank, and performing vacuum drying to obtain the biomass particles for improving flame resistance by utilizing micro-nano steam exploded slag. The novel flame-retardant biomass particles provided by the invention have excellent mildew-proof and anti-slagging performances.
Description
Technical Field
The invention discloses a biomass particle for improving flame resistance by utilizing micro-nano steam explosion slag and a processing technology thereof, belonging to the technical field of biomass energy.
Background
The biomass particle fuel is a typical biomass solid forming fuel, has the advantages of high efficiency, cleanness, easy ignition and CO2Zero emission and the like, can replace fossil fuels such as coal and the like and is applied to civil fields such as cooking, heating and the like and industrial fields such as boiler combustion, power generation and the like. The yield of biomass resources in China is rich, wherein the annual yield of crop straws is about 6 hundred million t, and the method has great development potential. However, the biomass pellet fuel produced by taking biomass such as straw as raw material has high ash content and alkali metal content, so that the problems of slag bonding, alkali metal and chlorine corrosion, serious fly ash in equipment and the like are easy to occur during use, and higher requirements are put forward for combustion technology and equipment.
Physical quality of biomass fuels has been studied by sequinuan and the like; characteristics of ignition, burnout and the like of the biomass granular fuel are researched by adopting TG-DTG thermal analysis technology in the manner of wise and king green apple and the like; the Maliaoling and the like research factors influencing the combustion speed of the straw briquette, and the marxianlan and the like research influencing factors influencing the ignition performance of the briquette. Gilbec, JuanF.Gonz-lez respectively research the formation and characteristics of slagging in a household stove of different wood and straw type (including energy crops and the like) molding fuels, BomanC and LindaSJohansson respectively research the combustion characteristics of the wood fuels and the molding fuels, MariaOlsson researches the discharge amount of pollutants when cork particles are combusted, J.Dias researches the combustion characteristics and the discharge amount of pollutants in the household stove of 4 different particle fuels, and Georg Baerhaler determines that main elements influencing the ash formation in the biomass fuels are Al, Ca, Fe, K, Mg and the like.
Disclosure of Invention
The invention aims to provide a biomass particle for improving flame resistance by utilizing micro-nano steam explosion slag and a processing technology thereof, so as to solve the problems in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
a flame-retardant biomass particle is improved by utilizing micro-nano steam explosion slag, and comprises the following raw materials in parts by weight: 10-20 parts of zinc polyacrylate resin, 40-60 parts of dimethylbenzene, 40-60 parts of n-butyl alcohol and 20-30 parts of blank.
The blank comprises the following raw materials in parts by weight: 20-30 parts of steam explosion residues, 2-3 parts of oleic acid, 0.1-0.2 part of lipase, 2-3 parts of xylitol and 30-40 parts of sodium alginate solution.
The modified steam explosion slag can also be modified steam explosion slag; the modified steam explosion slag comprises the following raw materials in parts by weight: 20-30 parts of mixed steam explosion residues, 1-2 parts of biogas slurry, 0.1-0.2 part of cane sugar, 30-50 parts of water and 10-20 parts of calcium chloride solution; the mixed steam explosion slag comprises the following raw materials in parts by weight: 20-30 parts of corn straw, 10-20 parts of wheat straw and 10-20 parts of cotton straw.
The sodium alginate solution can also be modified sodium alginate solution; the modified sodium alginate liquid comprises the following raw materials in parts by weight: 2-3 parts of sodium alginate, 100-120 parts of water and 0.01-0.02 part of sodium periodate.
The biomass particles for improving the flame resistance by utilizing the micro-nano steam explosion slag comprise the following raw materials in parts by weight: 20 parts of zinc polyacrylate resin, 60 parts of dimethylbenzene, 60 parts of n-butyl alcohol and 30 parts of blank.
A processing technology for improving flame-retardant biomass particles by utilizing micro-nano steam explosion slag comprises the following specific preparation methods:
(1) steam explosion;
(2) fermenting the product obtained in the step (1);
(3) fumigating the substance obtained in the step (2);
(4) preparing modified sodium alginate solution;
(5) mixing and granulating;
(6) treating the product obtained in the step (5);
(7) and (6) detecting.
The preparation method for improving the flame-retardant biomass particles by utilizing the micro-nano steam explosion slag comprises the following steps:
(1) mixing corn straw, wheat straw and cotton straw, and performing steam explosion to obtain mixed steam explosion residues;
(2) the method comprises the following steps of fermenting and mixing mixed steam explosion slag, biogas slurry, cane sugar and water, adding a calcium chloride solution, adjusting the pH value with a sodium hydroxide solution, filtering, freezing, ball-milling, sieving and drying to obtain pretreated steam explosion slag, wherein in the process, calcium ions in a system are precipitated by the sodium hydroxide solution and are dispersed in the mixed steam explosion slag, then, freezing is carried out to form ice crystals inside the mixed steam explosion slag, and the ice crystals are crushed into micro-nano steam explosion slag under the action of a ball mill, wherein the micro-nano steam explosion slag has a large specific surface area, so that the system is more fully contacted with oxygen, the product can be fully combusted, and the anti-slagging performance of the product is improved;
(3) fumigating and pretreating steam explosion slag by hydrofluoric acid steam, washing and drying to obtain modified steam explosion slag, wherein the pretreated steam explosion slag is frozen in the step (2) to increase the spacing between cells inside steam explosion slag particles, so that the hydrofluoric acid steam can be favorably and fully permeated into the steam explosion slag, silicon dioxide in steam explosion slag particle fibers can be fully reacted, the siliceous material in the steam explosion slag can be favorably removed, and the slag bonding resistance of the product can be further improved by removing a large amount of siliceous material;
(4) mixing sodium alginate with water, standing for swelling, heating, stirring for dissolving, adding sodium periodate, heating for reacting to obtain modified sodium alginate solution, and oxidizing hydroxy on a sodium alginate molecular chain into aldehyde group by sodium periodate oxidation treatment;
(5) placing modified steam exploded slag and modified sodium alginate liquid into a reaction kettle, adding sodium hydroxide solution to adjust pH, heating, stirring, reacting, cooling, adding glacial acetic acid to adjust pH, adding oleic acid, lipase, xylitol and calcium nitrate solution, stirring, mixing, granulating, performing freeze-thaw cycle, filtering and drying to obtain a blank, wherein in the process, firstly, aldehyde groups on molecular chains of the modified sodium alginate and hydroxyl aldol on the surfaces of steam exploded slag particle fibers are subjected to condensation reaction by adding the modified sodium alginate liquid under an alkaline heating condition to improve the bonding performance between the modified alginic acid and the steam exploded slag particle fibers, then calcium ions can crosslink the modified sodium alginate in a system by adding the calcium nitrate solution to enable the surfaces of the modified steam exploded slag to tightly wrap a modified sodium alginate film, and then the strength of the modified sodium alginate film is further improved by performing freeze-thaw cycle, the formed modified sodium alginate film can play a good role in blocking, so that the mildew resistance of the system is improved; secondly, oleic acid, xylitol, lipase and lipase are added to catalyze the esterification of oleic acid and xylitol to generate xylitol oleate, even a small amount of water exists in the system in the long-term use process, the xylitol oleate is hydrolyzed and consumed by the xylitol oleate, the hydrolysate of the xylitol oleate is difficult to be absorbed and utilized by microorganisms, and the microorganisms cannot survive without absorbing nutrient components, so that the product can be effectively prevented from mildewing for a long time; thirdly, water in the system is frozen through freeze thawing circulation, the frozen volume of the water is increased, gaps in the system are favorably widened, the gaps among the systems are further improved through the freeze thawing circulation, the contact area of the product and oxygen is further increased, the product can be further and fully combusted, and the anti-slagging performance of the product is further improved;
(6) stirring and mixing zinc polyacrylate resin, xylene and n-butyl alcohol, adding the blank, stirring and mixing, filtering, and drying in vacuum to obtain the biomass particles for improving the flame resistance by utilizing the micro-nano steam explosion slag;
(7) and (5) carrying out performance detection on the obtained product.
The specific preparation process of the flame-retardant biomass particles by utilizing the micro-nano steam explosion slag comprises the following steps:
(1) according to the weight parts, sequentially taking 20-30 parts of corn straw, 10-20 parts of wheat straw and 10-20 parts of cotton straw, placing the corn straw, the wheat straw and the cotton straw in a steam explosion tank, keeping the pressure for 60-90 s under the conditions that the steam explosion pressure is 2.8-3.5 MPa and the temperature is 160-180 ℃, and opening a discharge valve to instantaneously release pressure to obtain mixed steam explosion residues;
(2) taking 20-30 parts of mixed steam explosion slag, 1-2 parts of biogas slurry, 0.1-0.2 part of cane sugar, 30-50 parts of water and 10-20 parts of calcium chloride solution in sequence, putting the mixed steam explosion slag, the biogas slurry, the cane sugar and the water into a fermentation kettle, fermenting and mixing for 3-5 days at the temperature of 30-35 ℃ and the rotating speed of 100-200 r/min, adding the calcium chloride solution with the mass fraction of 10-20% into the fermentation kettle, adding the sodium hydroxide solution with the mass fraction of 20-30% into the fermentation kettle to adjust the pH to 12.5-12.8, filtering to obtain filter residue, putting the filter residue into liquid nitrogen to freeze to obtain frozen filter residue, putting the frozen filter residue into a ball mill, sieving by a 300-mesh sieve to obtain ball grinding materials, putting the ball grinding materials into an oven, and putting the ball grinding materials at the temperature of 105-110 ℃, drying to obtain pretreated steam explosion slag;
(3) placing the pretreated steam explosion residues in a fluidized bed reactor, introducing hydrofluoric acid steam into the fluidized bed reactor at a rate of 60-90 mL/min for treatment for 30min to obtain fumigation filter residues, washing the fumigation filter residues with ammonia water with a mass fraction of 20-30% until a washing solution is neutral, placing the washed fumigation filter residues in an oven, and drying at a temperature of 105-110 ℃ until the weight of the fumigation filter residues is constant to obtain modified steam explosion residues;
(4) sequentially taking 2-3 parts of sodium alginate, 100-120 parts of water and 0.01-0.02 part of sodium periodate according to parts by weight, placing the sodium alginate and the water in a beaker, stirring for 10-20 min by using a glass rod, standing and swelling for 3-5 h, then placing the beaker in a digital display speed measurement constant-temperature magnetic stirrer, heating, stirring and dissolving for 40-60 min at the temperature of 90-95 ℃ and the rotating speed of 500-600 r/min, then adding the sodium periodate into the beaker, and heating and reacting for 40-60 min at the temperature of 90-95 ℃ and the rotating speed of 500-600 r/min to obtain a modified sodium alginate solution;
(5) taking 20-30 parts of modified steam explosion slag, 2-3 parts of oleic acid, 0.1-0.2 part of lipase, 2-3 parts of xylitol and 30-40 parts of modified sodium alginate liquid in sequence by weight, putting the modified steam explosion slag and the modified sodium alginate liquid into a reaction kettle, adding a sodium hydroxide solution with the mass fraction of 20-30% into the reaction kettle to adjust the pH value to 8.6-8.9, heating and stirring the mixture for 40-60 min at the temperature of 140-160 ℃ and the rotating speed of 300-500 r/min, cooling the mixture to room temperature, adding glacial acetic acid into the reaction kettle to adjust the pH value to 7.1-7.3, adding an oleic acid, the lipase, the xylitol and a calcium nitrate solution into the reaction kettle, stirring and mixing the mixture for 40-60 min at the rotating speed of 600-800 r/min to obtain a mixed slurry, putting the mixed slurry into a granulator for granulation to obtain granules, putting the granules into a refrigerator, freezing for 5-8 hours at the temperature of-1 to-10 ℃ to obtain frozen granules, then placing the frozen granules at room temperature to be completely melted, performing freeze-thaw cycling for 5-8 times, filtering to obtain No. 1 filter cake, then placing the No. 1 filter cake in an oven, and drying to constant weight at the temperature of 105-110 ℃ to obtain a blank;
(6) taking 10-20 parts of zinc polyacrylate resin, 40-60 parts of dimethylbenzene, 40-60 parts of n-butanol and 20-30 parts of blank in sequence according to parts by weight, placing the zinc polyacrylate resin, the dimethylbenzene and the n-butanol into a single-neck flask, stirring and mixing for 40-60 min under the condition of the rotating speed of 500-600 r/min, then adding the blank into the single-neck flask, mixing for 40-60 min under the condition of the rotating speed of 500-600 r/min, filtering to obtain No. 2 filter cake, then placing the No. 2 filter cake into a drying box, vacuumizing, placing the filter cake in a pressure range of 0-10 KPa, and vacuum drying for 40-60 min under the condition of the temperature of 105-110 ℃ to obtain the flame-resistant biomass particles lifted by utilizing the micro-nano steam explosion slag;
(7) and (5) carrying out performance detection on the obtained product.
Compared with the prior art, the invention has the beneficial effects that:
in the preparation process, firstly, calcium ions in a system are precipitated by using a sodium hydroxide solution and dispersed in mixed steam explosion slag, then, ice crystals are formed inside the mixed steam explosion slag through freezing, and the mixed steam explosion slag is crushed into micro-nano steam explosion slag under the action of a ball mill, wherein the micro-nano steam explosion slag has a large specific surface area, so that the system is more fully contacted with oxygen, the product can be fully combusted, and the anti-slagging performance of the product is improved;
secondly, the pretreated steam explosion slag is frozen in the step (2) to increase the distance between cells inside steam explosion slag particles, so that hydrofluoric acid vapor can fully permeate into the steam explosion slag, silicon dioxide in steam explosion slag particle fibers can fully react, siliceous materials in the steam explosion slag can be removed, and the anti-slagging performance of the product can be further improved due to the removal of a large amount of siliceous materials;
thirdly, adding a modified sodium alginate liquid, and performing condensation reaction between aldehyde groups on a molecular chain of the modified sodium alginate and hydroxyl aldol on the surface of the steam exploded slag particle fiber under an alkaline heating condition to improve the bonding performance between the modified alginic acid and the steam exploded slag particle fiber;
thirdly, oleic acid, xylitol, lipase and lipase are added to catalyze the esterification of oleic acid and xylitol to generate xylitol oleate, even a small amount of water exists in the system in the long-term use process, the xylitol oleate is hydrolyzed and consumed by the xylitol oleate, the hydrolysate of the xylitol oleate is difficult to be absorbed and utilized by microorganisms, and the microorganisms cannot survive without absorbing nutrient components, so that the product can be effectively prevented from mildewing for a long time;
finally, through freeze thawing cycle, the moisture in the system freezes, and the frozen volume of water increases, is favorable to widening the space in the system, through freeze thawing cycle for the space between the system obtains further promotion, and the product further increases with oxygen area of contact, makes the further abundant burning of product, thereby makes the anti slagging scorification performance of product obtain further promotion.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to more clearly illustrate the method provided by the present invention, the following examples are used to describe the method in detail, and the method for testing each index of the biomass particles using micro-nano scale steam explosion slag to improve the flame resistance is as follows:
1. mildew resistance: performing performance detection according to GB/T21866;
2. anti-slagging performance: performing performance test with reference to GB/T219;
example 1
(1) According to the weight parts, sequentially taking 30 parts of corn straw, 20 parts of wheat straw and 20 parts of cotton straw, placing the corn straw, the wheat straw and the cotton straw in a steam explosion tank, keeping the pressure for 90s under the conditions that the steam explosion pressure is 3.5MPa and the temperature is 180 ℃, and opening a discharge valve to instantaneously release pressure to obtain mixed steam explosion residues;
(2) according to the weight parts, sequentially taking 30 parts of mixed steam explosion slag, 2 parts of biogas slurry, 0.2 part of cane sugar, 50 parts of water and 20 parts of calcium chloride solution, placing the mixed steam explosion slag, the biogas slurry and the cane sugar in a fermentation kettle, fermenting and mixing for 5 days at the temperature of 35 ℃ and the rotating speed of 200r/min, then adding 20% by mass of the calcium chloride solution into the fermentation kettle, adding 30% by mass of sodium hydroxide solution into the fermentation kettle at the rotating speed of 600r/min to adjust the pH to 12.8, filtering to obtain filter residue, then placing the filter residue in liquid nitrogen for freezing to obtain frozen filter residue, then placing the frozen filter residue in a ball mill for ball milling, sieving by a 300-mesh sieve to obtain ball grinding materials, then placing the ball grinding materials in an oven, and drying at the temperature of 110 ℃ to obtain pretreated steam explosion slag;
(3) placing the pretreated steam explosion residues in a fluidized bed reactor, introducing hydrofluoric acid steam into the fluidized bed reactor at a rate of 90mL/min for treatment for 30min to obtain fumigation filter residues, washing the fumigation filter residues with ammonia water with a mass fraction of 30% until washing liquid is neutral, placing the washed fumigation filter residues in an oven, and drying at a temperature of 110 ℃ until the weight of the fumigation filter residues is constant to obtain modified steam explosion residues;
(4) taking 3 parts of sodium alginate, 120 parts of water and 0.02 part of sodium periodate in sequence according to parts by weight, placing the sodium alginate and the water in a beaker, stirring for 20min by using a glass rod, standing and swelling for 5h, then placing the beaker in a digital display speed measurement constant temperature magnetic stirrer, heating, stirring and dissolving for 60min at the temperature of 95 ℃ and the rotating speed of 600r/min, then adding the sodium periodate into the beaker, and heating and reacting for 60min at the temperature of 95 ℃ and the rotating speed of 600r/min to obtain a modified sodium alginate solution;
(5) taking 30 parts of modified steam explosion slag, 3 parts of oleic acid, 0.2 part of lipase, 3 parts of xylitol and 40 parts of modified sodium alginate liquid in sequence, putting the modified steam explosion slag and the modified sodium alginate liquid into a reaction kettle, adding a sodium hydroxide solution with the mass fraction of 30% into the reaction kettle to adjust the pH value to 8.9, heating and stirring the mixture for reaction for 60 minutes at the temperature of 160 ℃ and the rotating speed of 500r/min, cooling the mixture to room temperature, adding glacial acetic acid into the reaction kettle to adjust the pH value to be 7.3, adding a oleic acid solution, a lipase, xylitol and a calcium nitrate solution into the reaction kettle, stirring and mixing the mixture for 60 minutes at the rotating speed of 800r/min to obtain mixed slurry, then placing the mixed slurry into a granulator for granulation to obtain granules, then placing the granules into a refrigerator, freezing the granules for 8 hours at the temperature of-10 ℃, obtaining frozen granules, then placing the frozen granules at room temperature to be completely melted, performing freeze-thaw cycle for 8 times, filtering to obtain No. 1 filter cake, then placing the No. 1 filter cake in an oven, and drying at the temperature of 110 ℃ to constant weight to obtain blanks;
(6) taking 20 parts of zinc polyacrylate resin, 60 parts of dimethylbenzene, 60 parts of n-butyl alcohol and 30 parts of blank in sequence according to parts by weight, placing the zinc polyacrylate resin, the dimethylbenzene and the n-butyl alcohol into a single-neck flask, stirring and mixing for 60min under the condition that the rotating speed is 600r/min, then adding the blank into the single-neck flask, mixing for 60min under the condition that the rotating speed is 600r/min, filtering to obtain No. 2 filter cake, then placing the No. 2 filter cake into a drying box, vacuumizing and placing at-10 KPa, and vacuum drying for 60min under the condition that the temperature is 110 ℃, thus obtaining the biomass particles for improving the flame resistance by utilizing the micro-nano steam explosion slag;
(7) and (5) carrying out performance detection on the obtained product.
Example 2
(1) According to the weight parts, sequentially taking 30 parts of corn straw, 20 parts of wheat straw and 20 parts of cotton straw, placing the corn straw, the wheat straw and the cotton straw in a steam explosion tank, keeping the pressure for 90s under the conditions that the steam explosion pressure is 3.5MPa and the temperature is 180 ℃, and opening a discharge valve to instantaneously release pressure to obtain mixed steam explosion residues;
(2) taking 30 parts of mixed steam explosion slag, 2 parts of biogas slurry, 0.2 part of cane sugar and 50 parts of water in sequence according to parts by weight, placing the mixed steam explosion slag, the biogas slurry, the cane sugar and the water in a fermentation kettle, fermenting and mixing for 5 days at the temperature of 35 ℃ and the rotating speed of 200r/min, adding a sodium hydroxide solution with the mass fraction of 30% into the fermentation kettle to adjust the pH to 12.8, filtering to obtain filter residue, placing the filter residue in liquid nitrogen to freeze to obtain frozen filter residue, placing the frozen filter residue in a ball mill to perform ball milling, sieving by a 300-mesh sieve to obtain ball grinding materials, placing the ball grinding materials in an oven, and drying at the temperature of 110 ℃ to obtain pretreated steam explosion slag;
(3) placing the pretreated steam explosion residues in a fluidized bed reactor, introducing hydrofluoric acid steam into the fluidized bed reactor at a rate of 90mL/min for treatment for 30min to obtain fumigation filter residues, washing the fumigation filter residues with ammonia water with a mass fraction of 30% until washing liquid is neutral, placing the washed fumigation filter residues in an oven, and drying at a temperature of 110 ℃ until the weight of the fumigation filter residues is constant to obtain modified steam explosion residues;
(4) taking 3 parts of sodium alginate, 120 parts of water and 0.02 part of sodium periodate in sequence according to parts by weight, placing the sodium alginate and the water in a beaker, stirring for 20min by using a glass rod, standing and swelling for 5h, then placing the beaker in a digital display speed measurement constant temperature magnetic stirrer, heating, stirring and dissolving for 60min at the temperature of 95 ℃ and the rotating speed of 600r/min, then adding the sodium periodate into the beaker, and heating and reacting for 60min at the temperature of 95 ℃ and the rotating speed of 600r/min to obtain a modified sodium alginate solution;
(5) taking 30 parts of modified steam explosion slag, 3 parts of oleic acid, 0.2 part of lipase, 3 parts of xylitol and 40 parts of modified sodium alginate liquid in sequence, putting the modified steam explosion slag and the modified sodium alginate liquid into a reaction kettle, adding a sodium hydroxide solution with the mass fraction of 30% into the reaction kettle to adjust the pH value to 8.9, heating and stirring the mixture for reaction for 60 minutes at the temperature of 160 ℃ and the rotating speed of 500r/min, cooling the mixture to room temperature, adding glacial acetic acid into the reaction kettle to adjust the pH value to be 7.3, adding a oleic acid solution, a lipase, xylitol and a calcium nitrate solution into the reaction kettle, stirring and mixing the mixture for 60 minutes at the rotating speed of 800r/min to obtain mixed slurry, then placing the mixed slurry into a granulator for granulation to obtain granules, then placing the granules into a refrigerator, freezing the granules for 8 hours at the temperature of-10 ℃, obtaining frozen granules, then placing the frozen granules at room temperature to be completely melted, performing freeze-thaw cycle for 8 times, filtering to obtain No. 1 filter cake, then placing the No. 1 filter cake in an oven, and drying at the temperature of 110 ℃ to constant weight to obtain blanks;
(6) taking 20 parts of zinc polyacrylate resin, 60 parts of dimethylbenzene, 60 parts of n-butyl alcohol and 30 parts of blank in sequence according to parts by weight, placing the zinc polyacrylate resin, the dimethylbenzene and the n-butyl alcohol into a single-neck flask, stirring and mixing for 60min under the condition that the rotating speed is 600r/min, then adding the blank into the single-neck flask, mixing for 60min under the condition that the rotating speed is 600r/min, filtering to obtain No. 2 filter cake, then placing the No. 2 filter cake into a drying box, vacuumizing and placing at-10 KPa, and vacuum drying for 60min under the condition that the temperature is 110 ℃, thus obtaining the biomass particles for improving the flame resistance by utilizing the micro-nano steam explosion slag;
(7) and (5) carrying out performance detection on the obtained product.
Example 3
(1) According to the weight parts, sequentially taking 30 parts of corn straw, 20 parts of wheat straw and 20 parts of cotton straw, placing the corn straw, the wheat straw and the cotton straw in a steam explosion tank, keeping the pressure for 90s under the conditions that the steam explosion pressure is 3.5MPa and the temperature is 180 ℃, and opening a discharge valve to instantaneously release pressure to obtain mixed steam explosion residues;
(2) taking 30 parts of mixed steam explosion slag, 2 parts of biogas slurry, 0.2 part of cane sugar, 50 parts of water and 20 parts of calcium chloride solution in sequence, placing the mixed steam explosion slag, the biogas slurry and the cane sugar in a fermentation kettle, fermenting and mixing for 5 days at the temperature of 35 ℃ and the rotating speed of 200r/min, then adding the calcium chloride solution with the mass fraction of 20% into the fermentation kettle, adding the sodium hydroxide solution with the mass fraction of 30% into the fermentation kettle at the rotating speed of 600r/min to adjust the pH to 12.8, filtering to obtain filter residue, then placing the filter residue in a drying oven, and drying at the temperature of 110 ℃ to obtain pretreated steam explosion slag;
(3) placing the pretreated steam explosion residues in a fluidized bed reactor, introducing hydrofluoric acid steam into the fluidized bed reactor at a rate of 90mL/min for treatment for 30min to obtain fumigation filter residues, washing the fumigation filter residues with ammonia water with a mass fraction of 30% until washing liquid is neutral, placing the washed fumigation filter residues in an oven, and drying at a temperature of 110 ℃ until the weight of the fumigation filter residues is constant to obtain modified steam explosion residues;
(4) taking 3 parts of sodium alginate, 120 parts of water and 0.02 part of sodium periodate in sequence according to parts by weight, placing the sodium alginate and the water in a beaker, stirring for 20min by using a glass rod, standing and swelling for 5h, then placing the beaker in a digital display speed measurement constant temperature magnetic stirrer, heating, stirring and dissolving for 60min at the temperature of 95 ℃ and the rotating speed of 600r/min, then adding the sodium periodate into the beaker, and heating and reacting for 60min at the temperature of 95 ℃ and the rotating speed of 600r/min to obtain a modified sodium alginate solution;
(5) taking 30 parts of modified steam explosion slag, 3 parts of oleic acid, 0.2 part of lipase, 3 parts of xylitol and 40 parts of modified sodium alginate liquid in sequence, putting the modified steam explosion slag and the modified sodium alginate liquid into a reaction kettle, adding a sodium hydroxide solution with the mass fraction of 30% into the reaction kettle to adjust the pH value to 8.9, heating and stirring the mixture for reaction for 60 minutes at the temperature of 160 ℃ and the rotating speed of 500r/min, cooling the mixture to room temperature, adding glacial acetic acid into the reaction kettle to adjust the pH value to be 7.3, adding a oleic acid solution, a lipase, xylitol and a calcium nitrate solution into the reaction kettle, stirring and mixing the mixture for 60 minutes at the rotating speed of 800r/min to obtain mixed slurry, then placing the mixed slurry into a granulator for granulation to obtain granules, then placing the granules into a refrigerator, freezing the granules for 8 hours at the temperature of-10 ℃, obtaining frozen granules, then placing the frozen granules at room temperature to be completely melted, performing freeze-thaw cycle for 8 times, filtering to obtain No. 1 filter cake, then placing the No. 1 filter cake in an oven, and drying at the temperature of 110 ℃ to constant weight to obtain blanks;
(6) taking 20 parts of zinc polyacrylate resin, 60 parts of dimethylbenzene, 60 parts of n-butyl alcohol and 30 parts of blank in sequence according to parts by weight, placing the zinc polyacrylate resin, the dimethylbenzene and the n-butyl alcohol into a single-neck flask, stirring and mixing for 60min under the condition that the rotating speed is 600r/min, then adding the blank into the single-neck flask, mixing for 60min under the condition that the rotating speed is 600r/min, filtering to obtain No. 2 filter cake, then placing the No. 2 filter cake into a drying box, vacuumizing and placing at-10 KPa, and vacuum drying for 60min under the condition that the temperature is 110 ℃, thus obtaining the biomass particles for improving the flame resistance by utilizing the micro-nano steam explosion slag;
(7) and (5) carrying out performance detection on the obtained product.
Example 4
(1) According to the weight parts, sequentially taking 30 parts of corn straw, 20 parts of wheat straw and 20 parts of cotton straw, placing the corn straw, the wheat straw and the cotton straw in a steam explosion tank, keeping the pressure for 90s under the conditions that the steam explosion pressure is 3.5MPa and the temperature is 180 ℃, and opening a discharge valve to instantaneously release pressure to obtain mixed steam explosion residues;
(2) according to the weight parts, sequentially taking 30 parts of mixed steam explosion slag, 2 parts of biogas slurry, 0.2 part of cane sugar, 50 parts of water and 20 parts of calcium chloride solution, placing the mixed steam explosion slag, the biogas slurry and the cane sugar in a fermentation kettle, fermenting and mixing for 5 days at the temperature of 35 ℃ and the rotating speed of 200r/min, then adding 20% by mass of the calcium chloride solution into the fermentation kettle, adding 30% by mass of sodium hydroxide solution into the fermentation kettle at the rotating speed of 600r/min to adjust the pH to 12.8, filtering to obtain filter residue, then placing the filter residue in liquid nitrogen for freezing to obtain frozen filter residue, then placing the frozen filter residue in a ball mill for ball milling, sieving by a 300-mesh sieve to obtain ball grinding materials, then placing the ball grinding materials in an oven, and drying at the temperature of 110 ℃ to obtain pretreated steam explosion slag;
(3) taking 3 parts of sodium alginate, 120 parts of water and 0.02 part of sodium periodate in sequence according to parts by weight, placing the sodium alginate and the water in a beaker, stirring for 20min by using a glass rod, standing and swelling for 5h, then placing the beaker in a digital display speed measurement constant temperature magnetic stirrer, heating, stirring and dissolving for 60min at the temperature of 95 ℃ and the rotating speed of 600r/min, then adding the sodium periodate into the beaker, and heating and reacting for 60min at the temperature of 95 ℃ and the rotating speed of 600r/min to obtain a modified sodium alginate solution;
(4) according to the weight parts, sequentially taking 30 parts of pretreated steam explosion slag, 3 parts of oleic acid, 0.2 part of lipase, 3 parts of xylitol and 40 parts of modified sodium alginate liquid, putting the pretreated steam explosion slag and the modified sodium alginate liquid into a reaction kettle, adding a sodium hydroxide solution with the mass fraction of 30% into the reaction kettle to adjust the pH value to 8.9, heating and stirring the mixture for reaction for 60 minutes at the temperature of 160 ℃ and the rotating speed of 500r/min, cooling the mixture to room temperature, adding glacial acetic acid into the reaction kettle to adjust the pH value to be only 7.3, adding the oleic acid, the lipase, the xylitol and a calcium nitrate solution into the reaction kettle, stirring and mixing the mixture for 60 minutes at the rotating speed of 800r/min to obtain mixed slurry, then putting the mixed slurry into a granulator for granulation to obtain granules, then putting the granules into a refrigerator, freezing the granules for 8 hours at the temperature of-10 ℃, obtaining frozen granules, then placing the frozen granules at room temperature to be completely melted, performing freeze-thaw cycle for 8 times, filtering to obtain No. 1 filter cake, then placing the No. 1 filter cake in an oven, and drying at the temperature of 110 ℃ to constant weight to obtain blanks;
(6) taking 20 parts of zinc polyacrylate resin, 60 parts of dimethylbenzene, 60 parts of n-butyl alcohol and 30 parts of blank in sequence according to parts by weight, placing the zinc polyacrylate resin, the dimethylbenzene and the n-butyl alcohol into a single-neck flask, stirring and mixing for 60min under the condition that the rotating speed is 600r/min, then adding the blank into the single-neck flask, mixing for 60min under the condition that the rotating speed is 600r/min, filtering to obtain No. 2 filter cake, then placing the No. 2 filter cake into a drying box, vacuumizing and placing at-10 KPa, and vacuum drying for 60min under the condition that the temperature is 110 ℃, thus obtaining the biomass particles for improving the flame resistance by utilizing the micro-nano steam explosion slag;
(6) and (5) carrying out performance detection on the obtained product.
Example 5
(1) According to the weight parts, sequentially taking 30 parts of corn straw, 20 parts of wheat straw and 20 parts of cotton straw, placing the corn straw, the wheat straw and the cotton straw in a steam explosion tank, keeping the pressure for 90s under the conditions that the steam explosion pressure is 3.5MPa and the temperature is 180 ℃, and opening a discharge valve to instantaneously release pressure to obtain mixed steam explosion residues;
(2) according to the weight parts, sequentially taking 30 parts of mixed steam explosion slag, 2 parts of biogas slurry, 0.2 part of cane sugar, 50 parts of water and 20 parts of calcium chloride solution, placing the mixed steam explosion slag, the biogas slurry and the cane sugar in a fermentation kettle, fermenting and mixing for 5 days at the temperature of 35 ℃ and the rotating speed of 200r/min, then adding 20% by mass of the calcium chloride solution into the fermentation kettle, adding 30% by mass of sodium hydroxide solution into the fermentation kettle at the rotating speed of 600r/min to adjust the pH to 12.8, filtering to obtain filter residue, then placing the filter residue in liquid nitrogen for freezing to obtain frozen filter residue, then placing the frozen filter residue in a ball mill for ball milling, sieving by a 300-mesh sieve to obtain ball grinding materials, then placing the ball grinding materials in an oven, and drying at the temperature of 110 ℃ to obtain pretreated steam explosion slag;
(3) placing the pretreated steam explosion residues in a fluidized bed reactor, introducing hydrofluoric acid steam into the fluidized bed reactor at a rate of 90mL/min for treatment for 30min to obtain fumigation filter residues, washing the fumigation filter residues with ammonia water with a mass fraction of 30% until washing liquid is neutral, placing the washed fumigation filter residues in an oven, and drying at a temperature of 110 ℃ until the weight of the fumigation filter residues is constant to obtain modified steam explosion residues;
(4) taking 3 parts of sodium alginate, 120 parts of water and 0.02 part of sodium periodate in sequence according to parts by weight, placing the sodium alginate and the water in a beaker, stirring for 20min by using a glass rod, standing and swelling for 5h, then placing the beaker in a digital display speed measurement constant temperature magnetic stirrer, heating, stirring and dissolving for 60min at the temperature of 95 ℃ and the rotating speed of 600r/min, then adding the sodium periodate into the beaker, and heating and reacting for 60min at the temperature of 95 ℃ and the rotating speed of 600r/min to obtain a modified sodium alginate solution;
(5) according to the weight parts, sequentially taking 30 parts of modified steam explosion slag and 40 parts of modified sodium alginate liquid, placing the modified steam explosion slag and the modified sodium alginate liquid in a reaction kettle, adding a sodium hydroxide solution with the mass fraction of 30% into the reaction kettle to adjust the pH value to 8.9, heating and stirring for reaction for 60min at the temperature of 160 ℃ and the rotating speed of 500r/min, cooling to room temperature, adding glacial acetic acid into the reaction kettle to adjust the pH value to be only 7.3, then adding a calcium nitrate solution into the reaction kettle, stirring and mixing for 60min at the rotating speed of 800r/min to obtain mixed slurry, then placing the mixed slurry in a granulator for granulation to obtain granules, then placing the granules in a refrigerator, freezing for 8h at the temperature of-10 ℃ to obtain frozen granules, then placing the frozen granules at room temperature for complete melting, performing freeze thawing for 8 times, filtering to obtain No. 1 filter cake, placing No. 1 filter cake in an oven, and drying at 110 deg.C to constant weight to obtain blank;
(6) taking 20 parts of zinc polyacrylate resin, 60 parts of dimethylbenzene, 60 parts of n-butyl alcohol and 30 parts of blank in sequence according to parts by weight, placing the zinc polyacrylate resin, the dimethylbenzene and the n-butyl alcohol into a single-neck flask, stirring and mixing for 60min under the condition that the rotating speed is 600r/min, then adding the blank into the single-neck flask, mixing for 60min under the condition that the rotating speed is 600r/min, filtering to obtain No. 2 filter cake, then placing the No. 2 filter cake into a drying box, vacuumizing and placing at-10 KPa, and vacuum drying for 60min under the condition that the temperature is 110 ℃, thus obtaining the biomass particles for improving the flame resistance by utilizing the micro-nano steam explosion slag;
(7) and (5) carrying out performance detection on the obtained product.
Example 6
(1) According to the weight parts, sequentially taking 30 parts of corn straw, 20 parts of wheat straw and 20 parts of cotton straw, placing the corn straw, the wheat straw and the cotton straw in a steam explosion tank, keeping the pressure for 90s under the conditions that the steam explosion pressure is 3.5MPa and the temperature is 180 ℃, and opening a discharge valve to instantaneously release pressure to obtain mixed steam explosion residues;
(2) according to the weight parts, sequentially taking 30 parts of mixed steam explosion slag, 2 parts of biogas slurry, 0.2 part of cane sugar, 50 parts of water and 20 parts of calcium chloride solution, placing the mixed steam explosion slag, the biogas slurry and the cane sugar in a fermentation kettle, fermenting and mixing for 5 days at the temperature of 35 ℃ and the rotating speed of 200r/min, then adding 20% by mass of the calcium chloride solution into the fermentation kettle, adding 30% by mass of sodium hydroxide solution into the fermentation kettle at the rotating speed of 600r/min to adjust the pH to 12.8, filtering to obtain filter residue, then placing the filter residue in liquid nitrogen for freezing to obtain frozen filter residue, then placing the frozen filter residue in a ball mill for ball milling, sieving by a 300-mesh sieve to obtain ball grinding materials, then placing the ball grinding materials in an oven, and drying at the temperature of 110 ℃ to obtain pretreated steam explosion slag;
(3) placing the pretreated steam explosion residues in a fluidized bed reactor, introducing hydrofluoric acid steam into the fluidized bed reactor at a rate of 90mL/min for treatment for 30min to obtain fumigation filter residues, washing the fumigation filter residues with ammonia water with a mass fraction of 30% until washing liquid is neutral, placing the washed fumigation filter residues in an oven, and drying at a temperature of 110 ℃ until the weight of the fumigation filter residues is constant to obtain modified steam explosion residues;
(4) taking 30 parts of modified steam explosion slag, 3 parts of oleic acid, 0.2 part of lipase, 3 parts of xylitol and 40 parts of sodium alginate liquid in sequence, placing the modified steam explosion slag and the sodium alginate liquid in a reaction kettle, adding a sodium hydroxide solution with the mass fraction of 30% into the reaction kettle to adjust the pH value to 8.9, heating and stirring the mixture for reaction for 60min at the temperature of 160 ℃ and the rotating speed of 500r/min, cooling the mixture to room temperature, adding glacial acetic acid into the reaction kettle to adjust the pH value to be only 7.3, then adding a oleic acid solution, a lipase, xylitol and a calcium nitrate solution into the reaction kettle, stirring and mixing the mixture for 60min at the rotating speed of 800r/min to obtain mixed slurry, then placing the mixed slurry in a granulator for granulation to obtain granules, then placing the granules in a refrigerator, freezing the granules for 8h at the temperature of-10 ℃ to obtain frozen granules, then placing the frozen granules at room temperature to be completely melted, performing freeze-thaw cycle for 8 times, filtering to obtain No. 1 filter cake, placing the No. 1 filter cake in an oven, and drying at the temperature of 110 ℃ to constant weight to obtain a blank;
(5) taking 20 parts of zinc polyacrylate resin, 60 parts of dimethylbenzene, 60 parts of n-butyl alcohol and 30 parts of blank in sequence according to parts by weight, placing the zinc polyacrylate resin, the dimethylbenzene and the n-butyl alcohol into a single-neck flask, stirring and mixing for 60min under the condition that the rotating speed is 600r/min, then adding the blank into the single-neck flask, mixing for 60min under the condition that the rotating speed is 600r/min, filtering to obtain No. 2 filter cake, then placing the No. 2 filter cake into a drying box, vacuumizing and placing at-10 KPa, and vacuum drying for 60min under the condition that the temperature is 110 ℃, thus obtaining the biomass particles for improving the flame resistance by utilizing the micro-nano steam explosion slag;
(6) and (5) carrying out performance detection on the obtained product.
Example 7
(1) According to the weight parts, sequentially taking 30 parts of corn straw, 20 parts of wheat straw and 20 parts of cotton straw, placing the corn straw, the wheat straw and the cotton straw in a steam explosion tank, keeping the pressure for 90s under the conditions that the steam explosion pressure is 3.5MPa and the temperature is 180 ℃, and opening a discharge valve to instantaneously release pressure to obtain mixed steam explosion residues;
(2) according to the weight parts, sequentially taking 30 parts of mixed steam explosion slag, 2 parts of biogas slurry, 0.2 part of cane sugar, 50 parts of water and 20 parts of calcium chloride solution, placing the mixed steam explosion slag, the biogas slurry and the cane sugar in a fermentation kettle, fermenting and mixing for 5 days at the temperature of 35 ℃ and the rotating speed of 200r/min, then adding 20% by mass of the calcium chloride solution into the fermentation kettle, adding 30% by mass of sodium hydroxide solution into the fermentation kettle at the rotating speed of 600r/min to adjust the pH to 12.8, filtering to obtain filter residue, then placing the filter residue in liquid nitrogen for freezing to obtain frozen filter residue, then placing the frozen filter residue in a ball mill for ball milling, sieving by a 300-mesh sieve to obtain ball grinding materials, then placing the ball grinding materials in an oven, and drying at the temperature of 110 ℃ to obtain pretreated steam explosion slag;
(3) placing the pretreated steam explosion residues in a fluidized bed reactor, introducing hydrofluoric acid steam into the fluidized bed reactor at a rate of 90mL/min for treatment for 30min to obtain fumigation filter residues, washing the fumigation filter residues with ammonia water with a mass fraction of 30% until washing liquid is neutral, placing the washed fumigation filter residues in an oven, and drying at a temperature of 110 ℃ until the weight of the fumigation filter residues is constant to obtain modified steam explosion residues;
(4) taking 3 parts of sodium alginate, 120 parts of water and 0.02 part of sodium periodate in sequence according to parts by weight, placing the sodium alginate and the water in a beaker, stirring for 20min by using a glass rod, standing and swelling for 5h, then placing the beaker in a digital display speed measurement constant temperature magnetic stirrer, heating, stirring and dissolving for 60min at the temperature of 95 ℃ and the rotating speed of 600r/min, then adding the sodium periodate into the beaker, and heating and reacting for 60min at the temperature of 95 ℃ and the rotating speed of 600r/min to obtain a modified sodium alginate solution;
(5) taking 30 parts of modified steam explosion slag, 3 parts of oleic acid, 0.2 part of lipase, 3 parts of xylitol and 40 parts of modified sodium alginate liquid in sequence, putting the modified steam explosion slag and the modified sodium alginate liquid into a reaction kettle, adding a sodium hydroxide solution with the mass fraction of 30% into the reaction kettle to adjust the pH value to 8.9, heating and stirring the mixture for reaction for 60 minutes at the temperature of 160 ℃ and the rotating speed of 500r/min, cooling the mixture to room temperature, adding glacial acetic acid into the reaction kettle to adjust the pH value to be 7.3, adding a oleic acid solution, a lipase, xylitol and a calcium nitrate solution into the reaction kettle, stirring and mixing the mixture for 60 minutes at the rotating speed of 800r/min to obtain mixed slurry, then placing the mixed slurry into a granulator for granulation to obtain granules, then placing the granules into a refrigerator, freezing the granules for 8 hours at the temperature of-10 ℃, obtaining frozen granules, then placing the frozen granules at room temperature to be completely melted, filtering after 8 times of freeze-thaw cycle to obtain No. 1 filter cake, then placing the No. 1 filter cake in an oven, and drying to constant weight at the temperature of 110 ℃ to obtain the biomass granules for improving the flame resistance by utilizing the micro-nano steam explosion slag;
(6) and (5) carrying out performance detection on the obtained product.
(1) According to the weight parts, sequentially taking 30 parts of corn straw, 20 parts of wheat straw and 20 parts of cotton straw, placing the corn straw, the wheat straw and the cotton straw in a steam explosion tank, keeping the pressure for 90s under the conditions that the steam explosion pressure is 3.5MPa and the temperature is 180 ℃, and opening a discharge valve to instantaneously release pressure to obtain mixed steam explosion residues;
(2) according to the weight parts, sequentially taking 30 parts of mixed steam explosion slag, 2 parts of biogas slurry, 0.2 part of cane sugar, 50 parts of water and 20 parts of calcium chloride solution, placing the mixed steam explosion slag, the biogas slurry and the cane sugar in a fermentation kettle, fermenting and mixing for 5 days at the temperature of 35 ℃ and the rotating speed of 200r/min, then adding 20% by mass of the calcium chloride solution into the fermentation kettle, adding 30% by mass of sodium hydroxide solution into the fermentation kettle at the rotating speed of 600r/min to adjust the pH to 12.8, filtering to obtain filter residue, then placing the filter residue in liquid nitrogen for freezing to obtain frozen filter residue, then placing the frozen filter residue in a ball mill for ball milling, sieving by a 300-mesh sieve to obtain ball grinding materials, then placing the ball grinding materials in an oven, and drying at the temperature of 110 ℃ to obtain pretreated steam explosion slag;
(3) placing the pretreated steam explosion residues in a fluidized bed reactor, introducing hydrofluoric acid steam into the fluidized bed reactor at a rate of 90mL/min for treatment for 30min to obtain fumigation filter residues, washing the fumigation filter residues with ammonia water with a mass fraction of 30% until washing liquid is neutral, placing the washed fumigation filter residues in an oven, and drying at a temperature of 110 ℃ until the weight of the fumigation filter residues is constant to obtain modified steam explosion residues;
(4) taking 3 parts of sodium alginate, 120 parts of water and 0.02 part of sodium periodate in sequence according to parts by weight, placing the sodium alginate and the water in a beaker, stirring for 20min by using a glass rod, standing and swelling for 5h, then placing the beaker in a digital display speed measurement constant temperature magnetic stirrer, heating, stirring and dissolving for 60min at the temperature of 95 ℃ and the rotating speed of 600r/min, then adding the sodium periodate into the beaker, and heating and reacting for 60min at the temperature of 95 ℃ and the rotating speed of 600r/min to obtain a modified sodium alginate solution;
(5) taking 30 parts of modified steam explosion slag, 3 parts of oleic acid, 0.2 part of lipase, 3 parts of xylitol and 40 parts of modified sodium alginate liquid in sequence, putting the modified steam explosion slag and the modified sodium alginate liquid into a reaction kettle, adding a sodium hydroxide solution with the mass fraction of 30% into the reaction kettle to adjust the pH value to 8.9, heating and stirring the mixture for reaction for 60 minutes at the temperature of 160 ℃ and the rotating speed of 500r/min, cooling the mixture to room temperature, adding glacial acetic acid into the reaction kettle to adjust the pH value to be 7.3, adding a oleic acid solution, a lipase, xylitol and a calcium nitrate solution into the reaction kettle, stirring and mixing the mixture for 60 minutes at the rotating speed of 800r/min to obtain mixed slurry, then placing the mixed slurry into a granulator for granulation to obtain granules, then placing the granules into a refrigerator, freezing the granules for 8 hours at the temperature of-10 ℃, obtaining frozen granules, then placing the frozen granules at room temperature to be completely melted, performing freeze-thaw cycle for 8 times, filtering to obtain No. 1 filter cake, then placing the No. 1 filter cake in an oven, and drying at the temperature of 110 ℃ to constant weight to obtain blanks;
(6) taking 20 parts of zinc polyacrylate resin, 60 parts of dimethylbenzene, 60 parts of n-butyl alcohol and 30 parts of blank in sequence according to parts by weight, placing the zinc polyacrylate resin, the dimethylbenzene and the n-butyl alcohol into a single-neck flask, stirring and mixing for 60min under the condition that the rotating speed is 600r/min, then adding the blank into the single-neck flask, mixing for 60min under the condition that the rotating speed is 600r/min, filtering to obtain No. 2 filter cake, then placing the No. 2 filter cake into a drying box, vacuumizing and placing at-10 KPa, and vacuum drying for 60min under the condition that the temperature is 110 ℃, thus obtaining the biomass particles for improving the flame resistance by utilizing the micro-nano steam explosion slag;
(7) and (5) carrying out performance detection on the obtained product.
Example 8
(1) According to the weight parts, sequentially taking 30 parts of corn straw, 20 parts of wheat straw and 20 parts of cotton straw, placing the corn straw, the wheat straw and the cotton straw in a steam explosion tank, keeping the pressure for 90s under the conditions that the steam explosion pressure is 3.5MPa and the temperature is 180 ℃, and opening a discharge valve to instantaneously release pressure to obtain mixed steam explosion residues;
(2) according to the weight parts, sequentially taking 30 parts of mixed steam explosion slag, 2 parts of biogas slurry, 0.2 part of cane sugar, 50 parts of water and 20 parts of calcium chloride solution, placing the mixed steam explosion slag, the biogas slurry and the cane sugar in a fermentation kettle, fermenting and mixing for 5 days at the temperature of 35 ℃ and the rotating speed of 200r/min, then adding 20% by mass of the calcium chloride solution into the fermentation kettle, adding 30% by mass of sodium hydroxide solution into the fermentation kettle at the rotating speed of 600r/min to adjust the pH to 12.8, filtering to obtain filter residue, then placing the filter residue in liquid nitrogen for freezing to obtain frozen filter residue, then placing the frozen filter residue in a ball mill for ball milling, sieving by a 300-mesh sieve to obtain ball grinding materials, then placing the ball grinding materials in an oven, and drying at the temperature of 110 ℃ to obtain pretreated steam explosion slag;
(3) placing the pretreated steam explosion residues in a fluidized bed reactor, introducing hydrofluoric acid steam into the fluidized bed reactor at a rate of 90mL/min for treatment for 30min to obtain fumigation filter residues, washing the fumigation filter residues with ammonia water with a mass fraction of 30% until washing liquid is neutral, placing the washed fumigation filter residues in an oven, and drying at a temperature of 110 ℃ until the weight of the fumigation filter residues is constant to obtain modified steam explosion residues;
(4) taking 3 parts of sodium alginate, 120 parts of water and 0.02 part of sodium periodate in sequence according to parts by weight, placing the sodium alginate and the water in a beaker, stirring for 20min by using a glass rod, standing and swelling for 5h, then placing the beaker in a digital display speed measurement constant temperature magnetic stirrer, heating, stirring and dissolving for 60min at the temperature of 95 ℃ and the rotating speed of 600r/min, then adding the sodium periodate into the beaker, and heating and reacting for 60min at the temperature of 95 ℃ and the rotating speed of 600r/min to obtain a modified sodium alginate solution;
(5) taking 30 parts of modified steam explosion slag, 3 parts of oleic acid, 0.2 part of lipase, 3 parts of xylitol and 40 parts of modified sodium alginate liquid in sequence, placing the modified steam explosion slag and the modified sodium alginate liquid in a reaction kettle, adding a sodium hydroxide solution with the mass fraction of 30% into the reaction kettle to adjust the pH value to 8.9, heating and stirring the mixture for reaction for 60 minutes at the temperature of 160 ℃ and the rotating speed of 500r/min, cooling the mixture to room temperature, adding glacial acetic acid into the reaction kettle to adjust the pH value to be 7.3, adding an oleic acid solution, a lipase, xylitol and a calcium nitrate solution into the reaction kettle, stirring and mixing the mixture for 60 minutes at the rotating speed of 800r/min, filtering the mixture to obtain No. 1 filter cake, placing the No. 1 filter cake in an oven, and drying the mixture to constant weight at the temperature of 110 ℃ to obtain a blank;
(6) taking 20 parts of zinc polyacrylate resin, 60 parts of dimethylbenzene, 60 parts of n-butyl alcohol and 30 parts of blank in sequence according to parts by weight, placing the zinc polyacrylate resin, the dimethylbenzene and the n-butyl alcohol into a single-neck flask, stirring and mixing for 60min under the condition that the rotating speed is 600r/min, then adding the blank into the single-neck flask, mixing for 60min under the condition that the rotating speed is 600r/min, filtering to obtain No. 2 filter cake, then placing the No. 2 filter cake into a drying box, vacuumizing and placing at-10 KPa, and vacuum drying for 60min under the condition that the temperature is 110 ℃, thus obtaining the biomass particles for improving the flame resistance by utilizing the micro-nano steam explosion slag;
(7) and (5) carrying out performance detection on the obtained product.
Comparative example
(1) According to the weight parts, sequentially taking 30 parts of corn straw, 20 parts of wheat straw and 20 parts of cotton straw, placing the corn straw, the wheat straw and the cotton straw in a steam explosion tank, keeping the pressure for 90s under the conditions that the steam explosion pressure is 3.5MPa and the temperature is 180 ℃, and opening a discharge valve to instantaneously release pressure to obtain mixed steam explosion residues;
(2) taking 30 parts of mixed steam explosion slag, 2 parts of biogas slurry, 0.2 part of cane sugar and 50 parts of water in sequence according to parts by weight, placing the mixed steam explosion slag, the biogas slurry, the cane sugar and the water in a fermentation kettle, fermenting and mixing for 5 days at the temperature of 35 ℃ and the rotating speed of 200r/min, adding a sodium hydroxide solution with the mass fraction of 30% into the fermentation kettle to adjust the pH to 12.8, filtering to obtain filter residue, placing the filter residue in liquid nitrogen to freeze to obtain frozen filter residue, placing the frozen filter residue in a ball mill to perform ball milling, sieving by a 300-mesh sieve to obtain ball grinding materials, placing the ball grinding materials in an oven, and drying at the temperature of 110 ℃ to obtain pretreated steam explosion slag;
(5) according to the weight portion, sequentially taking 30 portions of pre-treated steam explosion slag and 40 portions of sodium alginate liquid, placing the pre-treated steam explosion slag and the sodium alginate liquid in a reaction kettle, adding a sodium hydroxide solution with the mass fraction of 30% into the reaction kettle to adjust the pH value to 8.9, heating and stirring for reaction for 60min at the temperature of 160 ℃ and the rotating speed of 500r/min, cooling to room temperature, adding glacial acetic acid into the reaction kettle to adjust the pH value to be only 7.3, adding a calcium nitrate solution into the reaction kettle, stirring and mixing for 60min at the rotating speed of 800r/min to obtain mixed slurry, placing the mixed slurry in a granulator for granulation to obtain granules, placing the granules in a refrigerator, freezing for 8h at the temperature of-10 ℃ to obtain frozen granules, placing the frozen granules at room temperature until the granules are completely melted, and performing freeze-thaw cycle for 8 times, filtering to obtain No. 1 filter cake, then placing No. 1 filter cake in an oven, and drying to constant weight at the temperature of 110 ℃ to obtain biomass particles for improving flame resistance by utilizing micro-nano steam explosion slag;
(6) and (5) carrying out performance detection on the obtained product.
Performance test table:
table 1:
as can be seen from table 1: through comparison of the comparison documents 1, 2 and 3 with the comparison examples, calcium ions in the system are precipitated by using a sodium hydroxide solution and dispersed in the mixed steam explosion slag, and then the steam explosion slag can reach a nanometer level through freezing and crushing, so that the specific surface area of the steam explosion slag is increased, the system is more fully contacted with oxygen, the product can be fully combusted, and the anti-slagging performance of the product is improved; as can be seen by comparing examples 1 and 4 with the comparative example, the pretreated steam explosion slag is frozen in the step (2) to increase the distance between cells inside steam explosion slag particles, so that hydrofluoric acid vapor can be favorably and fully permeated into the steam explosion slag, silicon dioxide in steam explosion slag particle fibers can be fully reacted, silicon in the steam explosion slag can be favorably removed, a large amount of silicon can be removed, so that the anti-slagging performance of the product is further improved, by comparing examples 1 and 5 with the comparative example, oleic acid, xylitol, lipase and lipase are added to catalyze the esterification of oleic acid and xylitol to generate the xylitol oleate, in the long-term use process, even if a small amount of moisture exists in the system, the xylitol oleate is hydrolyzed and consumed by the xylitol oleate, the hydrolysate of the xylitol oleate is difficult to be absorbed and utilized by microorganisms, and the microorganisms cannot survive after absorbing nutrients, the product can be effectively prevented from mildewing for a long time; example 1, example 6, example 8 and comparative example, by adding modified sodium alginate solution, under alkaline heating conditions, aldehyde groups on the molecular chain of the modified sodium alginate react with hydroxyl aldol on the surface of the steam exploded slag particle fiber to improve the binding performance between the modified alginic acid and the steam exploded slag particle fiber, then by adding calcium nitrate solution, calcium ions can crosslink the modified sodium alginate in the system to enable the surface of the modified steam exploded slag to tightly wrap the modified sodium alginate membrane, then by freeze-thaw cycle, the strength of the modified sodium alginate membrane is further improved, the formed modified sodium alginate membrane can play a good barrier role, so that the mildew resistance of the system is improved, after freeze-thaw cycle, water in the system freezes, the water freezing volume is increased, the gap in the system is favorably widened, and by freeze-thaw cycle, the gaps among the systems are further improved, the contact area of the product and oxygen is further increased, the product can be further and fully combusted, and the anti-slagging performance of the product is further improved.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein, and any reference thereto is therefore intended to be embraced therein.
Claims (1)
1. A processing technology for improving flame-retardant biomass particles by utilizing micro-nano steam explosion slag is characterized by comprising the following steps of: the specific preparation process of the flame-retardant biomass particles by utilizing the micro-nano steam explosion slag comprises the following steps: (1) placing corn straws, wheat straws and cotton straws in a steam explosion tank, keeping the pressure for 60-90 s under the conditions of steam explosion pressure of 2.8-3.5 MPa and temperature of 160-180 ℃, and opening a discharge valve to instantly release pressure to obtain mixed steam explosion residues; (2) placing the mixed steam explosion slag, biogas slurry, cane sugar and water in a fermentation kettle, fermenting and mixing for 3-5 days at the temperature of 30-35 ℃ and at the rotating speed of 100-200 r/min, adding a calcium chloride solution with the mass fraction of 10-20% into the fermentation kettle, adding a sodium hydroxide solution with the mass fraction of 20-30% into the fermentation kettle at the rotating speed of 400-600 r/min to adjust the pH to 12.5-12.8, filtering to obtain filter residue, freezing the filter residue in liquid nitrogen to obtain frozen filter residue, placing the frozen filter residue in a ball mill for ball milling, sieving with a 300-mesh sieve to obtain ball grinding materials, placing the ball grinding materials in an oven, and drying at the temperature of 105-110 ℃ to obtain pretreated steam explosion slag; (3) placing the pretreated steam explosion residues in a fluidized bed reactor, introducing hydrofluoric acid steam into the fluidized bed reactor at a rate of 60-90 mL/min for treatment for 30min to obtain fumigation filter residues, washing the fumigation filter residues with ammonia water with a mass fraction of 20-30% until a washing solution is neutral, placing the washed fumigation filter residues in an oven, and drying at a temperature of 105-110 ℃ until the weight of the fumigation filter residues is constant to obtain modified steam explosion residues; (4) placing sodium alginate and water in a beaker, stirring for 10-20 min by using a glass rod, standing and swelling for 3-5 h, then placing the beaker in a digital display speed measurement constant-temperature magnetic stirrer, heating, stirring and dissolving for 40-60 min at the temperature of 90-95 ℃ and the rotating speed of 500-600 r/min, then adding sodium periodate into the beaker, and heating and reacting for 40-60 min at the temperature of 90-95 ℃ and the rotating speed of 500-600 r/min to obtain a modified sodium alginate solution; (5) placing modified steam explosion slag and modified sodium alginate liquid into a reaction kettle, adding 20-30 mass percent sodium hydroxide solution into the reaction kettle to adjust the pH value to 8.6-8.9, heating and stirring the mixture for reaction for 40-60 min at the temperature of 140-160 ℃ and the rotating speed of 300-500 r/min, cooling the mixture to room temperature, adding glacial acetic acid into the reaction kettle to adjust the pH value to 7.1-7.3, adding oleic acid, lipase, xylitol and calcium nitrate solution into the reaction kettle, stirring and mixing the mixture for 40-60 min at the rotating speed of 600-800 r/min to obtain mixed slurry, placing the mixed slurry into a granulator for granulation to obtain granules, placing the granules into a refrigerator, freezing the granules for 5-8 h at the temperature of-1-10 ℃ to obtain frozen granules, placing the frozen granules at room temperature to be completely melted, performing freeze thawing circulation for 5-8 times, filtering to obtain No. 1 filter cake, placing the No. 1 filter cake in an oven, and drying at 105-110 ℃ to constant weight to obtain a blank; (6) putting zinc polyacrylate resin, xylene and n-butyl alcohol into a single-neck flask, stirring and mixing for 40-60 min at the rotation speed of 500-600 r/min, adding a blank into the single-neck flask, mixing for 40-60 min at the rotation speed of 500-600 r/min, filtering to obtain No. 2 filter cake, putting the No. 2 filter cake into a drying box, vacuumizing to 0-minus 10KPa, and vacuum drying for 40-60 min at the temperature of 105-110 ℃ to obtain the flame-resistant biomass particles lifted by the micro-nano steam explosion slag; the zinc polyacrylate resin, the dimethylbenzene, the n-butyl alcohol and the blank are prepared from the following components in parts by weight: 10-20 parts of zinc polyacrylate resin, 40-60 parts of dimethylbenzene, 40-60 parts of n-butanol and 20-30 parts of blank; (7) and (5) carrying out performance detection on the obtained product.
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| CN111040820A (en) | 2020-04-21 |
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