CN106281530A - A kind of method of alkali oxygen low-temperature oxidation Shengli Brown - Google Patents

A kind of method of alkali oxygen low-temperature oxidation Shengli Brown Download PDF

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CN106281530A
CN106281530A CN201610633780.2A CN201610633780A CN106281530A CN 106281530 A CN106281530 A CN 106281530A CN 201610633780 A CN201610633780 A CN 201610633780A CN 106281530 A CN106281530 A CN 106281530A
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coal
temperature
alkali oxygen
oxidation
brown
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CN106281530B (en
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何润霞
刘全生
王斌
王丹丹
智科端
宋银敏
陈家明
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Inner Mongolia University of Technology
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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
    • C10L5/02—Solid fuels such as briquettes consisting mainly of carbonaceous materials of mineral or non-mineral origin
    • C10L5/04—Raw material of mineral origin to be used; Pretreatment thereof
    • 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
    • C10L10/00—Use of additives to fuels or fires for particular purposes
    • 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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  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
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Abstract

A kind of method that the invention discloses alkali oxygen low-temperature oxidation Shengli Brown, is prepared by following steps: by coal grinding, 105 DEG C of dry 4h, obtains coal dust；Respectively coal dust and NaOH solution are added in autoclave, seal autoclave, logical oxygen to 0.6MPa, by room temperature to 150 300 DEG C under the rotating speed of 300r/min, constant temperature 1h during final temperature, after be cooled to room temperature, obtain sample；By sample sucking filtration, filtering residue distilled water wash, to pH=8, after at 105 DEG C of dry 4h, obtain different temperatures alkali oxygen low-temperature oxidation Shengli Brown.The invention enables Shengli Brown combustibility generation significant change, its spontaneous combustion tendency of Shengli Brown after using the method to process significantly reduces, especially become apparent from 150 200 DEG C of alkali oxygen oxidation coal sample effects, substantially increase the safety in coal saving and transportation, there is significant economic and social benefit.

Description

A kind of method of alkali oxygen low-temperature oxidation Shengli Brown
Technical field
The invention belongs to technical field of coal chemical industry, a kind of method being specifically related to alkali oxygen low-temperature oxidation Shengli Brown.
Background technology
Coal is as the main energy sources of China, and its high-efficiency cleaning utilizes and is possible not only to alleviate the pollution to environment, more important Be that it becomes a kind of resource and important industrial chemicals.The Inner Mongol is that the Large-scale Coal of China produces one of province, and yield is only Inferior to Shanxi, coal reserves occupies whole nation second.
Brown coal are the coals that in the coal resources of the Inner Mongol, reserves are maximum, and wherein Shengli Coalfield is Xilinguole Beit area Maximum brown coal coalfield, the reserves of brown coal are 24,200,000,000 tons.Brown coal spontaneous combustion is because brown coal and can adsorb at normal temperatures in air Oxygen, and occur oxidation reaction to produce heat, if the heat produced can not distribute and continue to gather the temperature making brown coal very well Rise, just cause the spontaneous combustion of brown coal when reaching the ignition point of brown coal.Brown coal relatively bituminous coal and anthracite ignition point are lower, it is easier to There is spontaneous combustion.Particularly Shengli Brown due to the contour self-ignition index of its high-moisture, high volatile and rich oxygen content cause its Produce, store, utilize, the aspect such as transport is all extremely restricted, and therefore its precondition being fully utilized is to make it can Long-time storage and long distance transportation, application is very restricted.Therefore, the problem of Shengli Brown spontaneous combustion is solved for improving The utilization rate of brown coal has very important significance.
Summary of the invention
A kind of method that it is an object of the invention to provide alkali oxygen low-temperature oxidation Shengli Brown, after using the method to process Its spontaneous combustion tendency of Shengli Brown significantly reduces.
The present invention is achieved through the following technical solutions.
A kind of method of alkali oxygen low-temperature oxidation Shengli Brown, is prepared by following steps:
1) by coal grinding to 80-100 mesh, 105 DEG C of dry 4h, obtain coal dust；
2) respectively the NaOH solution of coal dust and 0.5mol/L is added in autoclave, seal autoclave, logical oxygen Gas to 0.6MPa, by room temperature to 150-300 DEG C under the rotating speed of 300r/min, constant temperature 1h during final temperature, after be cooled to room temperature, Obtain sample；
3) by sample sucking filtration, filtering residue distilled water wash, until pH=8, then at 105 DEG C of dry 4h, obtain different temperatures Alkali oxygen low-temperature oxidation Shengli Brown.
Described coal is the Shengli Brown in Xilinguole Beit area.
The mass ratio of described coal dust and NaOH solution is 1: 4-6.
The described heating-up time is 1h.
The method that the invention have the benefit that alkali oxygen low-temperature oxidation Shengli Brown of the present invention so that Shengli Brown burns Performance generation significant change, its spontaneous combustion tendency of Shengli Brown after using the method to process significantly reduces, especially with 150-200 DEG C Alkali oxygen oxidation coal sample effect becomes apparent from, and substantially increases the safety in coal saving and transportation, has significant economy And social benefit.
Accompanying drawing explanation
Fig. 1 is the infrared spectrogram that embodiment 1-4 and comparative example 1-2 prepare product；
Fig. 2 is XRD figure spectrum and the Gauss matched curve figure thereof that embodiment 1-4 and comparative example 1-2 prepare product；
Fig. 3 is Raman collection of illustrative plates and the Gauss matched curve figure thereof that embodiment 1-4 and comparative example 1-2 prepare product；
Fig. 4 is the CO that embodiment 1-4 and comparative example 1-2 prepare product burning2Growing amount and efficiency of carbon con version figure；
Fig. 5 is the TG/DTG combustion pattern of the product that embodiment 1-4 and comparative example 1-2 prepare.
In figure: SL-150 is embodiment 1；SL-200 is embodiment 2；SL-250 is embodiment 3；SL-300 is embodiment 4； SL-Raw is comparative example 1；SL-RT is comparative example 2.
Detailed description of the invention
With embodiment, technical scheme is described in more detail below in conjunction with the accompanying drawings.
Embodiment 1
A kind of method of alkali oxygen low-temperature oxidation Shengli Brown, is prepared by following steps:
1) by coal grinding to 80-100 mesh, 105 DEG C of dry 4h, obtain coal dust；
2) adding in autoclave by the NaOH solution of coal dust and 0.5mol/L, seal autoclave, logical oxygen is extremely 0.6MPa, by room temperature to 150 DEG C under the rotating speed of 300r/min, constant temperature 1h during final temperature, after be cooled to room temperature, obtain sample；
3) by sample sucking filtration, filtering residue distilled water wash, until pH=8, then at 105 DEG C of dry 4h, obtain 150 DEG C of alkali oxygen Low-temperature oxidation Shengli Brown, is designated as SL-150.
Described coal is the Shengli Brown in Xilinguole Beit area.
The mass ratio of described coal dust and NaOH solution is 1: 4.
The described heating-up time is 1h.
Embodiment 2
A kind of method of alkali oxygen low-temperature oxidation Shengli Brown, is prepared by following steps:
1) by coal grinding to 80-100 mesh, 105 DEG C of dry 4h, obtain coal dust；
2) adding in autoclave by the NaOH solution of coal dust and 0.5mol/L, seal autoclave, logical oxygen is extremely 0.6MPa, by room temperature to 200 DEG C under the rotating speed of 300r/min, constant temperature 1h during final temperature, after be cooled to room temperature, obtain sample；
3) by sample sucking filtration, filtering residue distilled water wash, until pH=8, then at 105 DEG C of dry 4h, obtain 200 DEG C of alkali oxygen Low-temperature oxidation Shengli Brown, is designated as SL-200.
Described coal is the Shengli Brown in Xilinguole Beit area.
The mass ratio of described coal dust and NaOH solution is 1: 5.
The described heating-up time is 1h.
Embodiment 3
A kind of method of alkali oxygen low-temperature oxidation Shengli Brown, is prepared by following steps:
1) by coal grinding to 80-100 mesh, 105 DEG C of dry 4h, obtain coal dust；
2) adding in autoclave by the NaOH solution of coal dust and 0.5mol/L, seal autoclave, logical oxygen is extremely 0.6MPa, by room temperature to 250 DEG C under the rotating speed of 300r/min, constant temperature 1h during final temperature, after be cooled to room temperature, obtain sample；
3) by sample sucking filtration, filtering residue distilled water wash, until pH=8, then at 105 DEG C of dry 4h, obtain 250 DEG C of alkali oxygen Low-temperature oxidation Shengli Brown, is designated as SL-250.
Described coal is the Shengli Brown in Xilinguole Beit area.
The mass ratio of described coal dust and NaOH solution is 1: 5.
The described heating-up time is 1h.
Embodiment 4
A kind of method of alkali oxygen low-temperature oxidation Shengli Brown, is prepared by following steps:
1) by coal grinding to 80-100 mesh, 105 DEG C of dry 4h, obtain coal dust；
2) adding in autoclave by the NaOH solution of coal dust and 0.5mol/L, seal autoclave, logical oxygen is extremely 0.6MPa, by room temperature to 300 DEG C under the rotating speed of 300r/min, constant temperature 1h during final temperature, after be cooled to room temperature, obtain sample；
3) by sample sucking filtration, filtering residue distilled water wash, until pH=8, then at 105 DEG C of dry 4h, obtain 300 DEG C of alkali oxygen Low-temperature oxidation Shengli Brown, is designated as SL-300.
Described coal is the Shengli Brown in Xilinguole Beit area.
The mass ratio of described coal dust and NaOH solution is 1: 6.
The described heating-up time is 1h.
Comparative example 1
The Shengli Brown in Xilinguole Beit area is ground to 80-100 mesh, 105 DEG C of dry 4h, obtains coal dust, be designated as SL-Raw。
Comparative example 2
The method of a kind of room temperature alkali oxygen oxidation Shengli Brown, is prepared by following steps:
1) Shengli Brown in Xilinguole Beit area is ground to 80-100 mesh, 105 DEG C of dry 4h, obtains coal dust；
2) by the NaOH solution mix homogeneously of coal dust and 0.5mol/L, stir under the rotating speed of air atmosphere 300r/min 3h, stands 2h, obtains sample；
The mass ratio of described coal dust and NaOH solution is 1: 5；
3) by sample sucking filtration, filtering residue distilled water wash, until pH=8, then at 105 DEG C of dry 4h, obtain room temperature alkali oxygen Oxidation Shengli Brown, is designated as SL-RT.
Industrial Analysis
Table 1 is the Industrial Analysis result that embodiment 1-4 and comparative example 1-2 prepare product.
The Industrial Analysis result of the product that table 1 embodiment 1-4 and comparative example 1-2 prepare
As shown in Table 1, compared with comparative example 1, embodiment 1-4 and the moisture of comparative example 2, content of ashes all increase.Contrast The volatile matter content of example 2 slightly raises, and the volatile matter content of embodiment 1-4 reduces on the contrary；And process with alkali oxygen low-temperature oxidation The raising of temperature reduces amplitude and increases.
Fig. 1 is the infrared spectrogram that embodiment 1-4 and comparative example 1-2 prepare product.As shown in Figure 1, room temperature alkali oxygen oxidation Front and back functional group's change of coal sample (comparative example 1 and comparative example 2) is little, and different temperatures alkali oxygen low-temperature oxidation is to coal sample functional group Kind and content have significantly impact.Wave number is at 3600-3000cm-1Between be the absworption peak district of hydroxyl, raw coal (comparative example 1) there is a wider absworption peak in this interval, after the oxidation of room temperature alkali oxygen (comparative example 2), this peak has almost no change, and 150-200 DEG C of alkali oxygen low-temperature oxidation coal sample (embodiment 1 and embodiment 2) is more similar at the peak in this interval, with comparative example 1 phase Ratio, peak type narrows and intensity increases, when alkali oxygen low oxidation temperature is increased to 250-300 DEG C (embodiment 3 and embodiment 4), The coal sample absorption peak strength in this interval is bigger.Above-mentioned phenomenon shows, the oxidation of room temperature alkali oxygen is little on hydroxyl impact in brown coal, but After alkali oxygen low oxidation temperature raises, the hydroxy radical content of coal sample substantially increases.Wave number is at 3000-2800cm-1Between be aliphatic The absorption vibrating area of C-H, 2923cm-1、2857cm-1Correspond respectively to-CH in cycloalkane or aliphatic hydrocarbon3With-CH2Asymmetric and Symmetrical stretching vibration.Comparative example 1 is the most sharp-pointed at this absworption peak at two, after different temperatures alkali oxygen oxidation processes, and 2925cm-1、 2848cm-1The absworption peak at place all weakens, and in the range of room temperature-200 DEG C, with the rising of alkali oxygen oxidation temperature, almost disappears, When treatment temperature is increased to 250-300 DEG C, the absworption peak at this occurs again, illustrates that alkali oxygen low-temperature oxidation processes the fat made in coal Fat hydrocarbon side chain reduces, and 150-200 DEG C is reduced at most.Wave number is at 1700cm-1Neighbouring peak is that the stretching vibration of carbonyl (C=O) is inhaled Receive peak, it is considered that in coal, absworption peak is caused by-COOH at this, comparative example 1 and comparative example 2 coal sample in this place all it can be seen that Faint absworption peak, and exist with acromion form, different temperatures alkali oxygen low-temperature oxidation coal sample is then hardly visible at this Absworption peak, illustrates in comparative example 1 and comparative example 2 with the presence of a small amount of carboxyl, and after higher temperature alkali oxygen low-temperature oxidation, In coal, carboxyl drastically reduces, and therefore the absworption peak at this disappears.Wave number 1600cm-1And 1580cm-1The peak at place is phenyl ring skeleton C=C stretching vibration absworption peak, after different temperatures alkali oxygen low-temperature oxidation, this absworption peak at two does not changes much, and brown coal are described Main body framework structure be not destroyed.1100cm-1、1030cm-1Absworption peak belong to the flexible of Si-O-Si in mineral Vibration, after the oxidation of room temperature alkali oxygen, this peak has no significant change, but the two peak in 150-200 DEG C of alkali oxygen low-temperature oxidation coal sample Weaken, and the two peak occurs again in 250-300 DEG C of alkali oxygen low-temperature oxidation coal sample, illustrate that room temperature alkali oxygen aoxidizes mineral In SiO2Impact is little, and in 150-200 DEG C of alkali oxygen low temperature oxidization process, part SiO2Generation is reacted with NaOH Na2SiO3, so 1100cm-1And 1030cm-1The peak at place weakens, and when alkali oxygen low-temperature oxidation is warmed up to 250-300 DEG C, sodium silicate There is Na2SiO3+2H2O==H2SiO3+ 2NaOH hydrolysis, and the H generated2SiO3It is heated and is decomposed into SiO2(JCPDS 82-1574) and H2O, so 2 θ=24.23 ° occur in that again SiO in 250-300 DEG C of alkali oxygen low-temperature oxidation coal sample2(JCPDS Absworption peak 82-1574).
Fig. 2 is X ray diffracting spectrum and the Gauss matched curve figure thereof that embodiment 1-4 and comparative example 1-2 prepare product. From Fig. 2 (a), each product all has a wider diffraction maximum in the range of 10-35 °, and this peak is to be folded by γ and 002 two peaks Adding and form, wherein γ peak is positioned between 10-20 °, and 002 peak is positioned between 20-35 °.002 peak is usually by fragrance crystallite in coal sample Structure is piled up and is formed.Above-mentioned coal sample is carried out swarming matching (using one of them sample as representative, such as Fig. 2 (b)), and according to Interlamellar spacing (the d of the microcrystalline silicon solar cells of Blagg and Scherrer Equation for Calculating coal sample, i.e. aromatic structure002), fragrance synusia heap Long-pending height (Lc) and fragrance synusia diameter (La), further according to formulaCalculate the coalification journey of coal sample Degree, the i.e. percent of condensation fragrance layer ring, microcrystalline silicon solar cells result of calculation is shown in Table 2.
Table 2 embodiment 1-4 and comparative example 1-2 prepare the microcrystalline silicon solar cells of product
Note: d002: aromatic structure interlamellar spacing；Lc: fragrance synusia piling height；La: the size of fragrance synusia；P: coalification journey Degree
002 peak of native graphite is positioned at 26.6 °, and as can be seen from Table 2,002 peak of six kinds of coal samples is respectively less than 26.6 °, Except 002 θ=22.74 °, peak 2 of raw coal all between 24-25 °, illustrate these from 26.6 ° of relatively far ultraviolets, the angle of diffraction of remaining coal sample Coal sample is respectively provided with the structure of class graphite.The degree of graphitization of raw coal is relatively low, and after alkali oxygen aoxidizes, the degree of graphitization of coal sample is bright Aobvious increase, and along with the rising of alkali oxygen low oxidation temperature, the angular higher angle of diffraction offsets, when alkali oxygen low oxidation temperature When increasing to 250-300 DEG C, the angle of diffraction reduces, but aoxidizes coal sample higher than raw coal with room temperature alkali oxygen.The aromatic structure interlamellar spacing of raw coal d002=0.3745nm, after alkali oxygen low-temperature oxidation processes, the interlamellar spacing of coal sample is respectively less than raw coal, but its fragrance synusia piling height Lc, size La of fragrance synusia and degree of coalification P all increase, and illustrate that alkali oxygen low-temperature oxidation causes coal aromatisation structure to have after processing Sequence strengthens, and when alkali oxygen low-temperature oxidation treatment temperature is 150-200 DEG C, degree of coalification is maximum.
Fig. 3 is Raman spectrum and the Gauss matched curve (matched curve that embodiment 1-4 and comparative example 1-2 prepare product Using one of them figure as representing).In figure, two obvious raman frequency vibration areas are respectively belonging to D peak (1340- 1380cm-1) and G peak (1580-1600cm-1), the defect peak that D peak and G peak represent in coal respectively (is commonly referred to be in plane Defect and heteroatomic vibration cause) and coal in bigger aromatic ring structure.As seen from the figure, the intensity at D peak and G peak is with alkali oxygen The raising of oxidation temperature and increase, 150-200 DEG C reaches maximum, and 250-300 DEG C is weakened on the contrary.The plan of Raman spectrum parameter Close result and be listed in table 3.I thereinD/IGIt is widely used in as an important parameter studying crystal and graphite-like structure, generation The surface defect degree (disordered carbon of marginal portion) of table coal, this ratio is the least, then the degree of graphitization of sample is the highest, defect journey Spend the least.From table 3, after different temperatures alkali oxygen low-temperature oxidation processes, ID/IGAll reduce, especially with treatment temperature as 150-200 DEG C time, reduce at most, the coal sample defective bit quantity minimizing processed be described, under lattice defect structure proportion in this temperature range Fall.When treatment temperature increases to 250-300 DEG C, the defect level of coal sample increases on the contrary, consistent with XRD characterization result.S peak master That to be represented is-Sp in coal3-the CH of hydridization3Group and Car-Cal aromatic ring side chain, Is/IGThe biggest, contained aromatic proton fat in coal sample The ratio of fat side chain is the highest, and after the process of alkali oxygen low-temperature oxidation, in coal, aromatic proton aliphatic side chains reduces, 150-200 DEG C of alkali oxygen cryogenic oxygen Change aromatic proton aliphatic side chains in coal sample minimum.IGL/IGThe biggest, the content of carbonyl is the highest, as seen from the table, at alkali oxygen low-temperature oxidation After reason, the content of carbonyl all declines, and illustrates that-COOH the partial exfoliation being connected with phenyl ring or fat in coal enters in solution.GRPeak, VLPeak and VRMain representative 3-5 phenyl ring in peak forms polymerization aromatic ring and the sp of be connected with aromatic ring methyl and methylene2-sp3Structure, ID/I(DR+VR+VL)The biggest, the methyl, the methylene content that show to be joined directly together with phenyl ring are the lowest, the change explanation alkali of data from table Oxygen low-temperature oxidation processes the sp causing being connected with aromatic ring2-sp3Valence bond structure there occurs change.
Table 3 embodiment 1-4 and comparative example 1-2 prepare the Raman fitting parameter of product
Fig. 4 is the CO that embodiment 1-4 and comparative example 1-2 prepare product burning2Growing amount and efficiency of carbon con version figure.Permissible by figure Know, when the coal sample of comparative example 1 is burnt in air atmosphere, only have larger amount of CO at about 340 DEG C2Generate.Room temperature alkali oxygen oxygen Change coal sample and two CO then occur2Generate peak, lay respectively at 200 DEG C and 640 DEG C, and the intensity at later peak is much larger than first Peak, illustrates CO2Main in about 640 DEG C generations, when alkali oxygen low oxidation temperature is increased to 150-200 DEG C, CO2Go out peak temperature Putting off until 760-770 DEG C, relatively comparative example 1 improves 320-330 DEG C, relatively comparative example 2CO2Mainly generate temperature and improve 120- 130 DEG C, and only one of which peak.When alkali oxygen low oxidation temperature is increased to 250-300 DEG C, CO2Go out peak temperature to reduce on the contrary, and Occur in that three CO2Generate peak.Above experimental result illustrates, alkali oxygen low-temperature oxidation makes brown coal burning generate CO2Temperature improve , in the range of room temperature to 200 DEG C, along with the rising of alkali oxygen low oxidation temperature, generate CO2Temperature improve, but when temperature After degree reaches 250 DEG C, generate CO2Temperature reduce on the contrary, by a CO2Generate peak and become three CO2Generate peak.
Fig. 5 is the TG/DTG combustion pattern that embodiment 1-4 and comparative example 1-2 prepare product.Can from TG curve Going out, each coal sample is mainly weightless (initiation temperature), and after 300 DEG C, the weight loss rate of comparative example 1 coal dust is very fast, and through alkali oxygen oxygen The equal weakened at different degrees of weight loss rate before coal sample after change 500 DEG C, room temperature alkali oxygen oxidation coal sample weight loss rate is less than contrast Example 1 coal sample, processes coal sample more than other temperature alkali oxygen low-temperature oxidation, and 150-200 DEG C of alkali oxygen low-temperature oxidation processes coal sample at 760- Weight loss rate before 790 DEG C is the slowest, and burning weight loss main peak moves to high-temperature region, there is obvious combustion lag phenomenon, says Bright 150-200 DEG C of alkali oxygen low-temperature oxidation processes and makes the chemical oxidation performance of coal sample substantially reduce, and ignition temperature is greatly improved, spontaneous combustion Tendency reduces.
In order to the spontaneous combustion tendency of each coal sample is intuitively described, the ignition temperature of coal sample need to be determined, use TG-DTG method to calculate The ignition temperature obtaining raw coal is 310.40 DEG C, brings up to 405.96 DEG C after room temperature alkali oxygen oxidation processes, and 150-200 DEG C of alkali oxygen is low After temperature oxidation processes, ignition temperature increases substantially, and is increased to 740-760 DEG C by the 310.40 of raw coal DEG C, continues to improve alkali oxygen Low-temperature oxidation treatment temperature to 250-300 DEG C, ignition temperature (410-440 DEG C) declines on the contrary, higher than comparative example 1 coal sample and room temperature Alkali oxygen oxidation coal sample, but process coal sample much smaller than 150-200 DEG C of alkali oxygen low-temperature oxidation.
The above, the only present invention preferably detailed description of the invention, protection scope of the present invention is not limited to this, any ripe Know those skilled in the art in the technical scope of present disclosure, the letter of the technical scheme that can become apparent to Altered or equivalence are replaced and are each fallen within protection scope of the present invention.

Claims (4)

1. the method for an alkali oxygen low-temperature oxidation Shengli Brown, it is characterised in that prepared by following steps:
1) by coal grinding to 80-100 mesh, 105 DEG C of dry 4h, obtain coal dust；
2) adding in autoclave by the NaOH solution of coal dust and 0.5mol/L respectively, seal autoclave, logical oxygen is extremely 0.6MPa, by room temperature to 150-300 DEG C under the rotating speed of 300r/min, constant temperature 1h during final temperature, after be cooled to room temperature, obtain sample Product；
3) by sample sucking filtration, filtering residue distilled water wash, until pH=8, then at 105 DEG C of dry 4h, obtain different temperatures alkali oxygen Low-temperature oxidation Shengli Brown.
Method the most according to claim 1, it is characterised in that described coal is that the triumph in Xilinguole Beit area is brown Coal.
Method the most according to claim 1, it is characterised in that the mass ratio of described coal dust and NaOH solution is 1: 4-6.
Method the most according to claim 1, it is characterised in that the described heating-up time is 1h.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107632107A (en) * 2017-08-14 2018-01-26 华中科技大学 A kind of Burning Behavior For Pulverized Coal quick determination method
CN108587714A (en) * 2018-02-11 2018-09-28 内蒙古工业大学 A kind of sodium base lignite and preparation method thereof
CN114292631A (en) * 2021-12-01 2022-04-08 安徽理工大学 Preparation method of environment-friendly coal-based self-heating material capable of rapidly heating in high amplitude
CN114410329A (en) * 2022-02-10 2022-04-29 山西沁新能源集团股份有限公司 High carbon coke with hybrid carbon and method for producing the same

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62192492A (en) * 1986-02-19 1987-08-24 Terunaito:Kk Dispersant for solid fuel-water slurry
CN103319324A (en) * 2012-03-20 2013-09-25 北京化工大学 Method for preparing benzene carboxylic acids by alkali-oxygen oxidation of brown coals

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62192492A (en) * 1986-02-19 1987-08-24 Terunaito:Kk Dispersant for solid fuel-water slurry
CN103319324A (en) * 2012-03-20 2013-09-25 北京化工大学 Method for preparing benzene carboxylic acids by alkali-oxygen oxidation of brown coals

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