CN109504487A - A kind of method that plant cellulose and lignin mixture nitre esterification prepare fuel - Google Patents
A kind of method that plant cellulose and lignin mixture nitre esterification prepare fuel Download PDFInfo
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- CN109504487A CN109504487A CN201811213944.1A CN201811213944A CN109504487A CN 109504487 A CN109504487 A CN 109504487A CN 201811213944 A CN201811213944 A CN 201811213944A CN 109504487 A CN109504487 A CN 109504487A
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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
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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
- C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
- C10L2290/08—Drying or removing water
-
- 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
- C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
- C10L2290/28—Cutting, disintegrating, shredding or grinding
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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
- C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
- C10L2290/36—Applying radiation such as microwave, IR, UV
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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
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Solid Fuels And Fuel-Associated Substances (AREA)
Abstract
The present invention provides a kind of methods that plant cellulose and lignin mixture nitre esterification prepare fuel comprising following steps: (1) to plant material pre-processes；(2) step (1) gains filtered through precipitating, be dried to obtain with the mixture of cellulose and wood powder；(3) nitre esterification: adding mixture into progress nitre esterification in nitration mixture, and the temperature of nitre esterification is 25 DEG C~58 DEG C, and the reaction time is 5min~3h；(4) pass through subsequent stable treatment, washing of precipitate, obtain nitrocellulose mixed ester fuel.The present invention is handled plant mixed raw material using nitre esterification techniques, the mole atom number ratio of energy Elements C, H, O, N etc. contained in plant cellulose mixture is set to change, the element recombinated after nitrification is able to achieve oxygen balance, under the conditions of certain pressure, temperature, humidity, granularity, the regular stable no air burning of parallel layers, is converted to heat and gas energy after igniting.
Description
Technical field
The invention belongs to the preparation technical fields of nitrocellulose fuel, and in particular to a kind of plant cellulose and lignin
The method that mixture nitre esterification prepares fuel.
Background technique
Cellulose is easy to plant in nature acquisition, agricultural crop straw, and cellulose abundant is rich in forestry timber；Nitre
Cellulose, also known as nitrocotton or cellulose nitrate are the products of cellulose and nitric acid reaction, are a kind of chemical industry materials containing energy
Material, is widely used in gunpowder, explosive and propellant, paint, celluloid arts.The gunpowder combustion manufactured with this material
There is no smog when burning, therefore also known as smokeless gun propellant, environmental pollution it is small.Currently, nitrocellulose production both domestic and external is mainly with essence
Cotton processed is raw material, is to chemically react cotton by the mixed acid after purification processing again with nitric acid and sulfuric acid, then pass through
It crosses a series of postprocessing working procedures processing and obtains.Since purified cotton produces nitrocellulose higher cost, and output of cotton is limited,
Therefore, find the plant cellulose of alternative purified cotton carried out by the work that fuel is made in nitre esterification and obtain centainly at
Effect, plant material, agricultural crop straw etc. are sugared rich in cellulose abundant, lignin, pectic substance, gumminess and non-cellulose, but
It is that it needs complicated preprocessing process, DNA purity height, boiling alkali cleaning, bleaching are that good cellulose just can be through nitration reaction
Obtain good security, the nitrocellulose that burn rate is fast, specific efficiency is high.And often due to cellulose in plant tissue and lignin
Close weave in is difficult to be completely separated, although being had conducted extensive research to the separation of cellulose, extraction process,
But limited by extracting method, pretreatment process when producing fiber is still complicated various, other portions in addition to cellulose
Divide energy matter not to be utilized, becomes harmful and reluctant substance.
On the other hand, traditional nitre-sulphur mixed acid nitrification system, the splitting action of sulfuric acid cause the viscosity of esterification products to reduce
The even destruction of fibre morphology rinses and consumes a large amount of water and the energy with stable treatment, also generates a large amount of waste water and exhaust gas, right
Environment causes greatly to pollute；Product is to prevent from thermally decomposing, and extends the shelf life and needs to add corresponding raw material and technique and drop
Low energy is not able to satisfy green manufacturing, the extensive function of making fuel for energy field.
Therefore, seek a kind of method that can be directly nitrified to cellulose mixed raw material, it can will be in plant tissue
Cellulose, lignin carry out nitre esterification together to obtain nitre esterification fuel, and good product performance, viscosity stability can be obtained
High, good security fuel, becomes technical problem urgently to be resolved.
Summary of the invention
The object of the invention is in order to solve the above-mentioned technical problem, and provide a kind of plant cellulose mixture nitre esterification combustion
The preparation method of material, method provided by the invention are handled plant mixed raw material using nitre esterification techniques, make plant fiber
The atomic weight ratio of energy Elements C, H, O, N etc. contained in plain mixture changes, and recombinates later element and is able to achieve oxygen
Balance, under certain pressure, temperature, humidity under no air conditions, it is gentle that the stable burning of parallel layers rule is converted to heat
Physical efficiency amount realizes no air burning very well.
To achieve the goals above, the technical solution adopted by the present invention is a kind of plant cellulose mixture nitre esterification fuel
Preparation method, comprising the following steps:
(1) plant material pre-processes: carrying out shearing grinding after plant material is cleaned airing, obtaining granularity is 0.0374mm
Then the plant fiber powder of~0.300mm >=50% carries out washing sub-sieve, dehydration to plant fiber powder, by different material
Size selectively carries out boiling or microwave radiation processing；
(2) it prepares mixture: gains after step (1) pretreatment being filtered through precipitating, are dried to obtain cellulose and wood powder
Mixture, the averag density of the mixture is 320kg/m3-510kg/m3；
(3) nitre esterification: adjust mixture temperature be 3 DEG C~48 DEG C, granularity be 0.0374mm~0.300mm >=
50%, water content adds mixture into nitration mixture progress nitre esterification less than 5%, and the temperature of nitre esterification is 25 DEG C~
58 DEG C, the reaction time is 5min~3h；The nitration mixture is the mixture of nitric acid and sulfuric acid, and as mass fraction, nitric acid is dense for nitration mixture
Degree is 89%-98%, content 23.5%-55.5%, sulfuric acid concentration 89%-98%, content 37.0%-69.0%；Water
Content is divided to be lower than 7.5%；
(4) waste acidity recovery: the nitre sulphur spent acid after nitre esterification is recycled；
(5) stable treatment: stable treatment is carried out to nitre esterification products using autoclaving technology, it is excessive sweet that adjustment is precipitated
Oil；
(6) it washing of precipitate: is diluted with water into step (5) gains, cryoprecipitation filtering, obtains nitrocellulose after washing
Plain mixed ester fuel.
The present invention provides a kind of method that cellulose and lignin mixed plant powder are directly carried out nitre esterification treatment,
The nitrocellulose mixed ester fuel nitrogen content being prepared can be adjusted as needed, adjusting range be 6.5%~
Between 12.5%, make to introduce nitro compounds in the organic compound molecule of energy Elements C, H, O, N etc. contained in plant, forms nitre
Acyl cation and phenyl ring row Electrophilic Aromatic substitution reaction, and the fuel that the hydrogen ion for sloughing molecule obtains；The fuel can pass through
Dry humidity is≤4.9%, granularity 0.0374mm~0.300mm >=50%, pressure≤0.10MPa~1.36MPa, firing temperature
It≤235 DEG C, realizes after igniting without air burning, is converted into heat and gas energy.The good security of fuel, impurity content can
Control, the degree of polymerization and viscosity are more excellent, and the combustion heat value of fuel is constant, can carry out effective energy conversion at tolerance.
Preparation method of the invention carries out shearing after cleaning is dried to plant material, at normal temperature with clear water in equipment for grinding
Middle grinding is rinsed, sub-sieve, and the lignin, starch, impurity of low energy are removed, and screenings matter can be made by the dry fermentation of precipitating
Agricultural fertilizer or direct returning to farmland are handled, and mixture drying comb solution in sieve, on-the-sieve material is recycled back to mill, by green manufacturing
Directly to the mixed raw material in plant based on cellulose and wood powder, the method for carrying out nitre esterification processing is divided into depending on variety classes
Only make once boiling before or after nitrification, the energy element in plant is fully utilized, waste of low pollution is small, treatment process letter
Single, the nitre esterification fuel performance being prepared is good, viscosity stability is high, good security, can largely using agricultural crop straw and
Other planting plants are raw material；Fuel obtained burns in addition to that itself can stablize the low ignition temperature of parallel layers in no air conditions
Outside, the burn rate for concocting other energetic materials, synthesis fuel combination can also be bonded.
Plant is made of cell wall, pit and lumen, axial tracheid, conduit, wood-fibred, wood radiaftive rays etc.；It includes fibre
Element, lignin, pectic substance, gumminess and non-cellulose sugar are tieed up, is in pencil parallel by 7000~10000 glucose molecules
Column, the flammable energy element of the polymer connected through glycosidic linkage are efficiently utilized.Product after the esterification of this method nitre is still
So keep the fibrous structure of pristine fibre element.It is observed under ordinary ray, fiber appearance structure and pristine fibre after nitrification
Element is similar, and observing can find that the two has significant difference under polarized light.Tonal brightness under polarised light is with esterification degree difference
And it changes.As esterification degree is continuously improved, gradually become glassy yellow from steel gray (nitrogen content 11%), or even silver-colored blue
(nitrogen content is more than 11.8%).Nitre esterification, which is carried out, according to the different selectivity of the type of plant does disposable boiling with front or rear.
Further, the wood powder includes the mixture of wood pulp, collacin and xylose.
Further, being carried out in step (2) to the powder that gains medium viscosity is excessive after pretreatment, smoke amount is higher
Destructive distillation carbonization pretreatment, removal starch, lignin and impurity reduce ash content and grinding coefficient.
Further, the nitre esterification is first added in continuous nitrification machine or interval nitrification machine in step (3)
Then mixture stirring is added in nitration mixture into nitration mixture, it is anti-that the continuation of nitration mixture mixture is continuously added to progress nitre esterification simultaneously in proportion
It answers, the mixture carries out comb solution and drying process before reaction is added.
Further, the waste acidity recovery process in step (4) is as follows: by the mixed material after nitre esterification from nitrification
Machine outflow, through cooling material, after inputting centrifugal separator separation, spent acid is flowed out from bell mouth, by giving up after precipitating in sour pond
Acid tube road input Gravity Separation machine is separated, and precipitates filtering using cooling, chemical examination concentration and component ratio are made into mixed again
Acid carries out closed cycle utilization.
Further, the spent acid after step (3) nitration reaction is entered spent acid thermal decomposer, carry out thermally decomposing pre- place
Reason.
Further, step (5) in using heat weak acid and weak caustic solution under high pressure successively carry out acid boil, alkali
It boils and fine purifiation.
Further, the condition of the autoclaving is temperature: 150 DEG C -163 DEG C, pressure: 0.5MPa-0.7MPa.
Further, boiling described in step (1) processing temperature be 98 DEG C~100 DEG C, the microwave treatment it is micro-
Wave radiation amount is 4.9W/g powder.
Further, the nitrocellulose mixed ester fuel is soaked in water in conveying, transport, storage, protect
Card humidity is 19%-28%.
The present invention still further provides the nitrocellulose mixed ester fuel that the above method is prepared, and is to plant
Raw material directly carries out nitre esterification treatment, and contained energy Elements C in plant, the atomic weight ratio of H, O, N is made to change, reset with
The fuel obtained afterwards；The nitrogen content of the fuel is 8.6%~12.5%, which can fire under no air conditions
It burns, is converted into heat and gas energy.
Compared with prior art, the beneficial effects of the present invention are: the present invention provides a kind of pair of plant cellulose and wood
The method that quality mixed raw material carries out direct nitre esterification, can obtain that impurity content is low, good nitrocellulose fuel, make to plant
The atomic weight ratio of energy Elements C, H, O, N etc. contained in object changes, and resets later element and is able to achieve oxygen balance,
Certain pressure, temperature, humidity are converted to heat, gas without burning under air conditions；Its degree of nitration is high, calorific value is high, viscosity is steady
Qualitative high, good security.It carries out cleaning nitrification fuel production using plant tissue raw material the present invention also provides a whole set of
Technique carries out high efficiente callback utilization to the exhaust gas and spent acid generated in nitrifying process, has the characteristics of energy conservation and environmental protection.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments to the present invention
It is specifically described, it is necessary to, it is noted that following embodiment is used only for that the present invention is explained and illustrated, be not used to
Limit the present invention.Some nonessential modifications and adaptations that those skilled in the art are made according to foregoing invention content, still belong to
In protection scope of the present invention.
Embodiment 1
A kind of preparation method of plant nitrocellulose mixed ester fuel, comprising the following steps:
(1) it is dried after washing with water agricultural crop straw and carries out shearing grinding, obtaining granularity is 0.0374mm~0.300mm
Then >=50% crop branch fiber powder carries out washing sub-sieve, dehydration to the fiber powder, then carries out at microwave radiation
Reason, the amount of radiation of microwave are 4.9W/g powder, handle 40min；
(2) powder excessive to step (1) gains medium viscosity, smoke amount is higher carries out destructive distillation carbonization pretreatment, removal
Starch, lignin and impurity reduce ash content and grinding coefficient, then through precipitating filtering, be dried to obtain the mixed of cellulose and wood powder
Material is closed, the averag density of mixture is 320kg/m3；Wood powder includes the mixture of wood pulp, collacin and xylose；
(3) comb solution and drying process are first carried out to mixture, are 320kg/m by averag density3Mixing package be sent to comb
Solution machine, cardboard shape cellulose are sent to cutting machine and are shredded, and convey drying interlocking set by air-flow to after cellulose comb solution,
Cellulose is sent to nitrification operation；Then adjust mixture temperature be 3 DEG C, granularity be 0.4um~50um, water content 4%,
Nitre esterification is carried out in continuous nitrification machine, the temperature of nitre esterification is 25 DEG C~28 DEG C, the reaction time be 5min~
10min, wherein nitration mixture is the mixture of nitric acid and sulfuric acid, and as mass fraction, concentration of nitric acid 89%, content is nitration mixture
23.5%, sulfuric acid concentration 89%, content 69.0%；Moisture content is 7.5%；
In above-mentioned steps, the cellulose that dry humidity is about 4% will be passed through and be transported in production line in magazine formula measuring tank,
Nitration mixture pump is driven into head tank.Cellulose, nitration mixture are measured when entering nitrator.What is come out from storage tank is mixed
Acid, be through over-heat-exchanger, it is therefore an objective to be heated or cooled to it, to reach required temperature, then enter back into nitrator.
Nitric-sulfuric acid is added into nitrator under stiring, is then automatically stopped cellulose feed, does not stop acid adding during this period；
In above-mentioned steps, the nitre generated after nitration reaction, sulphur cigarette are entered into nitre, sulphur cigarette absorption system water is absorbed at dilute
Nitre, sulphur nitration mixture；Spent acid after nitration reaction is entered into spent acid thermal decomposer, carries out thermal decomposition pretreatment；
(4) mixed material after nitre esterification is inputted into centrifugal separator point through cooling material from nitrification machine outflow
From rear, spent acid is flowed out from bell mouth, is separated after precipitating in sour pond by spent acid pipeline input Gravity Separation machine, using cold
But precipitating filtering, chemically examines concentration and component ratio is made into nitration mixture again and carries out closed cycle utilization.By what is generated after nitration reaction
Nitre, sulphur cigarette enter nitre, sulphur cigarette absorption system water is absorbed into dilute nitre, sulphur nitration mixture；
(5) stable treatment is carried out to nitration product using autoclaving technology, step is the weak acid and weak base using heat
Solution by high-temperature and high-pressure conditions successively to nitration product carry out acid boil, soda boiling and fine purifiation, the condition of autoclaving is temperature:
150 DEG C, pressure: 0.5MPa；The acid waste water that the step generates is entered dilution machine to be recycled；
(6) filtering is precipitated after being diluted with water, cool down into step (5) obtained solid object, obtains nitrocellulose after washing
Mixed ester fuel, is soaked in water into fuel, guarantees that humidity is 19%, then conveyed, transported and stored.
Embodiment 2
A kind of preparation method of plant nitrocellulose mixed ester fuel, comprising the following steps:
(1) it is dried after washing with water agricultural crop straw and carries out shearing grinding, obtaining granularity is 0.0374mm~0.300mm
Then >=50% crop branch fiber powder carries out washing sub-sieve, dehydration to the fiber powder, then carries out boiling processing,
Temperature is 98 DEG C, boiling 1h or more；
(2) powder excessive to step (1) gains medium viscosity, smoke amount is higher carries out destructive distillation carbonization pretreatment, removal
Starch, lignin and impurity reduce ash content and grinding coefficient, then through precipitating filtering, be dried to obtain the mixed of cellulose and wood powder
Material is closed, the averag density of mixture is 430kg/m3；Wood powder includes the mixture of wood pulp, collacin and xylose；
(3) comb solution and drying process are first carried out to mixture, are 430kg/m by averag density3Mixing package be sent to comb
Solution machine, cardboard shape cellulose are sent to cutting machine and are shredded, and convey drying interlocking set by air-flow to after cellulose comb solution,
Cellulose is sent to nitrification operation；Then adjust mixture temperature be 30 DEG C~35 DEG C, granularity be 0.0374mm~0.300mm >=
50%, water content carries out nitre esterification less than 5% in interval nitrification machine, and the temperature of nitre esterification is 30 DEG C~35 DEG C,
Reaction time is 1h, and wherein nitration mixture is the mixture of nitric acid and sulfuric acid, and as mass fraction, concentration of nitric acid 98% contains nitration mixture
Amount is 25.5%, sulfuric acid concentration 98%, content 67.0%；Moisture content is 7.5%；
In above-mentioned steps, the cellulose that dry humidity is about 5% will be passed through and be transported in production line in magazine formula measuring tank,
Nitration mixture pump is driven into head tank.Cellulose, nitration mixture are measured when entering nitrator.What is come out from storage tank is mixed
Acid, be through over-heat-exchanger, it is therefore an objective to be heated or cooled to it, to reach required temperature, then enter back into nitrator.
Nitric-sulfuric acid is added into nitrator under stiring, is then automatically stopped cellulose feed, does not stop acid adding during this period；
In above-mentioned steps, the nitre generated after nitration reaction, sulphur cigarette are entered into nitre, sulphur cigarette absorption system water is absorbed at dilute
Nitre, sulphur nitration mixture；Spent acid after nitration reaction is inputted into spent acid thermal decomposer, carries out thermal decomposition pretreatment；
(4) mixed material after nitre esterification is inputted into centrifugal separator point through cooling material from nitrification machine outflow
From rear, spent acid is flowed out from bell mouth, is separated after precipitating in sour pond by spent acid pipeline input Gravity Separation machine, using cold
But precipitating filtering, chemically examines concentration and component ratio is made into nitration mixture again and carries out closed cycle utilization.By what is generated after nitration reaction
Nitre, sulphur cigarette enter nitre, sulphur cigarette absorption system water is absorbed into dilute nitre, sulphur nitration mixture；
(5) stable treatment is carried out to nitration product using autoclaving technology, step is the weak acid and weak base using heat
Solution by high-temperature and high-pressure conditions successively to nitration product carry out acid boil, soda boiling and fine purifiation, the condition of autoclaving is temperature:
156 DEG C, pressure: 0.6MPa；The acid waste water that the step generates is entered dilution machine to be recycled；
(6) filtering is precipitated after being diluted with water, cool down into step (5) obtained solid object, obtains nitrocellulose after washing
Mixed ester fuel, is soaked in water into fuel, guarantees that humidity is 28%, then conveyed, transported and stored.
Embodiment 3
A kind of preparation method of plant nitrocellulose mixed ester fuel, comprising the following steps:
(1) it is dried after washing with water raw material bamboo and carries out shearing grinding, obtain the bamboo that granularity is 100 μm~150 μm
Then fiber powder carries out washing sub-sieve, dehydration to the fiber powder, then carries out boiling processing, temperature is 100 DEG C, boiling 1h
More than；
(2) powder excessive to step (1) gains medium viscosity, smoke amount is higher carries out destructive distillation carbonization pretreatment, removal
Starch, lignin and impurity reduce ash content and grinding coefficient, then through precipitating filtering, be dried to obtain the mixed of cellulose and wood powder
Material is closed, the averag density of mixture is 510kg/m3；Wood powder includes the mixture of wood pulp, collacin and xylose；
(3) comb solution and drying process are first carried out to mixture, are 510kg/m by averag density3Mixing package be sent to comb
Solution machine, cardboard shape cellulose are sent to cutting machine and are shredded, and convey drying interlocking set by air-flow to after cellulose comb solution,
Cellulose is sent to nitrification operation；Then the temperature for adjusting mixture is 48 DEG C, and granularity is 100 μm~150 μm, water content 3%,
Nitre esterification is carried out in continuous nitrification machine, the temperature of nitre esterification is 56 DEG C~58 DEG C, reaction time 3h, wherein mixing
Acid be nitric acid and sulfuric acid mixture, nitration mixture as mass fraction, concentration of nitric acid 96%, content 24.5%, sulfuric acid concentration
It is 98%, content 68.0%；Moisture content is 7.5%；
In above-mentioned steps, the cellulose that dry humidity is about 3% will be passed through and be transported in production line in magazine formula measuring tank,
Nitration mixture pump is driven into head tank.Cellulose, nitration mixture are measured when entering nitrator.What is come out from storage tank is mixed
Acid, be through over-heat-exchanger, it is therefore an objective to be heated or cooled to it, to reach required temperature, then enter back into nitrator.
Nitric-sulfuric acid is added into nitrator under stiring, is then automatically stopped cellulose feed；
In above-mentioned steps, the nitre generated after nitration reaction, sulphur cigarette are entered into nitre, sulphur cigarette absorption system water is absorbed at dilute
Nitre, sulphur nitration mixture；Spent acid after nitration reaction is entered into spent acid thermal decomposer, carries out thermal decomposition pretreatment；
(4) mixed material after nitre esterification is inputted into centrifugal separator point through cooling material from nitrification machine outflow
From rear, spent acid is flowed out from bell mouth, is separated after precipitating in sour pond by spent acid pipeline input Gravity Separation machine, using cold
But precipitating filtering, chemically examines concentration and component ratio is made into nitration mixture again and carries out closed cycle utilization, by what is generated after nitration reaction
Nitre, sulphur cigarette enter nitre, sulphur cigarette absorption system water is absorbed into dilute nitre, sulphur nitration mixture；
(5) stable treatment is carried out to nitration product using autoclaving technology, step is the weak acid and weak base using heat
Solution by high-temperature and high-pressure conditions successively to nitration product carry out acid boil, soda boiling and fine purifiation, the condition of autoclaving is temperature:
163 DEG C, pressure: 0.7MPa；The acid waste water that the step generates is entered dilution machine to be recycled；
(6) filtering is precipitated after being diluted with water, cool down into step (5) obtained solid object, obtains nitrocellulose after washing
Mixed ester fuel, is soaked in water into fuel, guarantees that humidity is 22%, then conveyed, transported and stored.
Embodiment 4
A kind of preparation method of plant nitrocellulose mixed ester fuel, comprising the following steps:
(1) dried after washing with water raw material bamboo and carry out shearing grinding, obtain granularity be 0.0374mm~0.300mm >=
Then 50% bamboo fiber powder carries out washing sub-sieve, dehydration to the fiber powder, then carries out microwave radiation processing, microwave
Amount of radiation is 4.9W/g powder, handles 30min or more；
(2) powder excessive to step (1) gains medium viscosity, smoke amount is higher carries out destructive distillation carbonization pretreatment, removal
Starch, lignin and impurity reduce ash content and grinding coefficient, then through precipitating filtering, be dried to obtain the mixed of cellulose and wood powder
Material is closed, the averag density of mixture is 470kg/m3；It include the mixture of wood pulp, collacin and xylose in wood powder；
(3) comb solution and drying process are first carried out to mixture, are 470kg/m by averag density3Mixing package be sent to comb
Solution machine conveys drying interlocking set by air-flow to after cellulose comb solution, cellulose is sent to nitrification operation；Then mixing is adjusted
The temperature of material is 5 DEG C, and granularity is 0.0374mm~0.300mm >=50%, and water content 4% carries out nitre in continuous nitrification machine
Esterification, the temperature of nitre esterification are 40 DEG C, reaction time 40min, and wherein nitration mixture is the mixture of nitric acid and sulfuric acid,
Nitration mixture as mass fraction, concentration of nitric acid 95%, content 25.5%, sulfuric acid concentration 95%, content 69.0%；Moisture
Content is 5.5%；
In above-mentioned steps, the cellulose that dry humidity is about 4% will be passed through and be transported in production line in magazine formula measuring tank,
Nitration mixture pump is driven into head tank.Cellulose, nitration mixture are measured when entering nitrator.What is come out from storage tank is mixed
Acid, be through over-heat-exchanger, it is therefore an objective to and it is heated or cooled, to reach required temperature, then enters back into nitrator,
Nitric-sulfuric acid is added into nitrator under stiring, is then automatically stopped cellulose feed, does not stop acid adding during this period；
In above-mentioned steps, the nitre generated after nitration reaction, sulphur cigarette are entered into nitre, sulphur cigarette absorption system water is absorbed at dilute
Nitre, sulphur nitration mixture；Spent acid after nitration reaction is entered into spent acid thermal decomposer, carries out thermal decomposition pretreatment；
(4) mixed material after nitre esterification is inputted into centrifugal separator point through cooling material from nitrification machine outflow
From rear, spent acid is flowed out from bell mouth, is separated after precipitating in sour pond by spent acid pipeline input Gravity Separation machine, using cold
But precipitating filtering, chemically examines concentration and component ratio is made into nitration mixture again and carries out closed cycle utilization, by what is generated after nitration reaction
Nitre, sulphur cigarette enter nitre, sulphur cigarette absorption system water is absorbed into dilute nitre, sulphur nitration mixture；
(5) stable treatment is carried out to nitration product using autoclaving technology, step is the weak acid and weak base using heat
Solution by high-temperature and high-pressure conditions successively to nitration product carry out acid boil, soda boiling and fine purifiation, the condition of autoclaving is temperature:
155 DEG C, pressure: 0.7MPa；The acid waste water that the step generates is entered dilution machine to be recycled；
(6) filtering is precipitated after being diluted with water, cool down into step (5) obtained solid object, obtains nitrocellulose after washing
Mixed ester fuel, is soaked in water into fuel, guarantees that humidity is 24%, then conveyed, transported and stored.
Embodiment 5
A kind of preparation method of plant nitrocellulose mixed ester fuel, comprising the following steps:
(1) dried after washing with water raw material agricultural crop straw and carry out shearing grinding, obtain granularity be 0.0374mm~
Then the bamboo fiber powder of 0.300mm >=50% carries out washing sub-sieve, dehydration to the fiber powder, then carries out microwave radiation
Processing, microwave radiation amount are 4.9W/g powder, handle 20min；
(2) powder excessive to step (1) gains medium viscosity, smoke amount is higher carries out destructive distillation carbonization pretreatment, removal
Starch, lignin and impurity reduce ash content and grinding coefficient, then through precipitating filtering, be dried to obtain the mixed of cellulose and wood powder
Material is closed, the averag density of mixture is 350kg/m3；It include the mixture of wood pulp, collacin and xylose in wood powder；
(3) comb solution and drying process are first carried out to mixture, are 350kg/m by averag density3Mixing package be sent to comb
Solution machine conveys drying interlocking set by air-flow to after cellulose comb solution, cellulose is sent to nitrification operation；Then mixing is adjusted
The temperature of material is 35 DEG C, and granularity is 20um~40um, and water content 4% carries out nitre esterification, nitre ester in interval nitrification machine
The temperature for changing reaction is 32 DEG C, reaction time 2.5h, and wherein nitration mixture is the mixture of nitric acid and sulfuric acid, and nitration mixture presses mass fraction
Meter, concentration of nitric acid 92%, content 24.5%, sulfuric acid concentration 95%, content 69.0%；Moisture content is 6.5%；
In above-mentioned steps, the cellulose that dry humidity is about 4% will be passed through and be transported in production line in magazine formula measuring tank,
Nitration mixture pump is driven into head tank.Cellulose, nitration mixture are measured when entering nitrator, what is come out from storage tank is mixed
Acid, be through over-heat-exchanger, it is therefore an objective to and it is heated or cooled, to reach required temperature, then enters back into nitrator,
Nitric-sulfuric acid is added into nitrator under stiring, is then automatically stopped cellulose feed, does not stop acid adding during this period；
In above-mentioned steps, the nitre generated after nitration reaction, sulphur cigarette are entered into nitre, sulphur cigarette absorption system water is absorbed at dilute
Nitre, sulphur nitration mixture；Spent acid after nitration reaction is entered into spent acid thermal decomposer, carries out thermal decomposition pretreatment；
(4) mixed material after nitre esterification is inputted into centrifugal separator point through cooling material from nitrification machine outflow
From rear, spent acid is flowed out from bell mouth, is separated after precipitating in sour pond by spent acid pipeline input Gravity Separation machine, using cold
But precipitating filtering, chemically examines concentration and component ratio is made into nitration mixture again and carries out closed cycle utilization, by what is generated after nitration reaction
Nitre, sulphur cigarette enter nitre, sulphur cigarette absorption system water is absorbed into dilute nitre, sulphur nitration mixture；
(5) stable treatment is carried out to nitration product using autoclaving technology, step is the weak acid and weak base using heat
Solution by high-temperature and high-pressure conditions successively to nitration product carry out acid boil, soda boiling and fine purifiation, the condition of autoclaving is temperature:
160 DEG C, pressure: 0.5MPa；The acid waste water that the step generates is entered dilution machine to be recycled；
(6) filtering is precipitated after being diluted with water, cool down into step (5) obtained solid object, obtains nitrocellulose after washing
Mixed ester fuel, is soaked in water into fuel, guarantees that humidity is 26%, then conveyed, transported and stored.
Experimental example
Performance measurement is carried out to the nitrocellulose mixed ester fuel that above-described embodiment 1-5 is prepared, acquired results are such as
Shown in table 1:
The primary quality measure of 1 mixed ester fuel of table
As it can be seen from table 1 the degree of nitration for the nitrocellulose fuel being prepared in 1-5 of the embodiment of the present invention is high, peace
It is qualitative it is good, impurity content is low, viscosity stability is good.
Fuel is prepared according to the method for embodiment, by being adjusted to plant energy element, nitrogen content, which is prepared, is
8.6%~12.5% fuel combination, to generation heat, the hot coefficient of flash burn and the specific volume system of different nitrocellulose mixed ester fuel
Number measured value is as shown in table 2 below:
Generation heat, the hot coefficient of flash burn and the specific volume coefficient of the different nitre esterification composite fibre fuel of table 2
Note: β in tableiFor flash burn heat, UiFor specific volume
From table 2 it can be seen that the nitrocellulose fuel of different nitrogen contents has been prepared in the embodiment of the present invention, make to plant
The atomic weight ratio of energy Elements C, H, O, N etc. contained in object changes, and resets later element and is able to achieve oxygen balance,
Certain pressure, temperature, humidity burn under no air conditions and are converted to thermal energy, gas；Its primary combustion product composition such as table
3:
3 primary combustion product of table forms measured value (mol/100g)
Claims (10)
1. a kind of method that plant cellulose and lignin mixture nitre esterification prepare fuel, which is characterized in that including following step
It is rapid:
(1) plant material pre-process: by plant material cleaning dry after carry out shearing grinding, obtain granularity be 0.0374mm~
Then the plant fiber powder of 0.300mm >=50% carries out washing sub-sieve, dehydration to plant fiber powder, big by different material
Small selectivity carries out boiling or microwave radiation processing；
(2) prepare mixture: by gains after step (1) pretreatment through precipitating filtering, be dried to obtain the mixed of cellulose and wood powder
Material is closed, the averag density of the mixture is 320kg/m3-510kg/m3；
(3) nitre esterification: the temperature for adjusting mixture is 3 DEG C~48 DEG C, and granularity is 0.0374mm~0.300mm >=50%,
Water content adds mixture into progress nitre esterification in nitration mixture less than 5%, and the temperature of nitre esterification is 25 DEG C~58 DEG C,
Reaction time is 5min~3h；The nitration mixture is the mixture of nitric acid and sulfuric acid, and as mass fraction, concentration of nitric acid is nitration mixture
89%-98%, content 23.5%-55.5%, sulfuric acid concentration 89%-98%, content 37.0%-69.0%；Moisture contains
Amount is not higher than 7.5%；
(4) waste acidity recovery: the nitre sulphur spent acid after nitre esterification is recycled；
(5) stable treatment: stable treatment is carried out to nitre esterification products using autoclaving technology, adjustment excess of glycerol is precipitated；
(6) it washing of precipitate: is diluted with water into step (5) gains, cryoprecipitation filtering, it is mixed that nitrocellulose is obtained after washing
Close ester fuel.
2. the method that plant cellulose according to claim 1 and lignin mixture nitre esterification prepare fuel, feature
It is, the wood powder includes the mixture of wood pulp, collacin and xylose.
3. the method that plant cellulose according to claim 1 and lignin mixture nitre esterification prepare fuel, feature
It is, in step (2), destructive distillation carbonization pretreatment is carried out to the powder that gains medium viscosity is excessive after pretreatment, smoke amount is higher,
Remove starch, lignin and impurity.
4. the method that plant cellulose according to claim 1 and lignin mixture nitre esterification prepare fuel, feature
It is, in step (3), the nitre esterification is that nitration mixture is first added in continuous nitrification machine or interval nitrification machine, then to mixed
Mixture stirring is added in acid and carries out nitre esterification, the mixture carries out comb solution and drying process before reaction is added.
5. the method that plant cellulose according to claim 1 and lignin mixture nitre esterification prepare fuel, feature
It is, the waste acidity recovery process in step (4) is as follows: by the mixed material after nitre esterification from nitrification machine outflow, through cooling
Material, input centrifugal separator separation after, spent acid from bell mouth flow out, in sour pond precipitate after by spent acid pipeline input gravity
Seperator is separated, and using cooling precipitating filtering, chemically examines concentration and component ratio is made into nitration mixture again and carries out closed cycle
It utilizes.
6. the method that plant cellulose according to claim 1 and lignin mixture nitre esterification prepare fuel, feature
Be, successively carried out under high pressure using the weak acid and weak caustic solution of heat in step (5) acid boil, soda boiling and fine purifiation.
7. the method that plant cellulose according to claim 6 and lignin mixture nitre esterification prepare fuel, feature
It is, the condition of the autoclaving is temperature: 150 DEG C -163 DEG C, pressure: 0.5MPa-0.7MPa.
8. the method that plant cellulose according to claim 1 and lignin mixture nitre esterification prepare fuel, feature
It is, the temperature of the processing of boiling described in step (1) is 98 DEG C~100 DEG C, and the microwave radiation amount of the microwave treatment is 4.9W/
G powder.
9. the method that plant cellulose according to claim 1 and lignin mixture nitre esterification prepare fuel, feature
It is, the nitrocellulose mixed ester fuel is soaked in water in conveying, transport, storage, and guarantee humidity is 19%-
28%.
10. the nitrocellulose mixed ester fuel that any one of -9 the methods are prepared, feature exist according to claim 1
In being directly to carry out nitre esterification treatment to plant material, make to introduce in the organic compound molecule of contained energy element in plant
Nitro compounds form nitryl cation and phenyl ring row Electrophilic Aromatic substitution reaction, slough the fuel that the hydrogen ion of molecule obtains；It is described
The nitrogen content of fuel is 6.5%~12.5%, which is≤4.9% by dry humidity, granularity 0.0374mm~0.300mm
>=50%, pressure≤0.10MPa~1.36MPa, firing temperature≤235 DEG C are realized and burn under no air conditions, are converted into heat
Amount and gas energy.
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