CN105527312B - A kind of analysis method for biomass ash melting characteristic - Google Patents
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- 238000000034 method Methods 0.000 claims abstract description 42
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- 238000005259 measurement Methods 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
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- Life Sciences & Earth Sciences (AREA)
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Abstract
The present invention relates to biomass energy gasification fields, in particular it relates to a kind of method for the analysis of biomass ash melting characteristic.The present invention is measured using thermomechanical analyzer, and specific steps include: the preparation of biomass ash sample, the test of biomass ash melting characteristic and the parsing of coal ash meltbility curve；And define respectively: biomass ash sintering stage characteristic temperature Ts, biomass ash melt stage characteristic temperature Tm, the melting characteristic of biomass ash is parsed and evaluated using characteristic temperature；And using characteristic temperature TmAgglomerate loses stream temperature caused by predicting fluidized bed combustion and melting during gasifying because of biomass ash.This method can melting characteristic of the continuous observation ash in entire heating process, test process can also embody ash, and viscosity-temperature characteristic bring changes under the high temperature conditions, therefore, utilize the melting characteristic of thermomechanical analysis test biomass ash, can more objectively and comprehensively reflect ash melting characteristic, and it is reproducible, accuracy is high.
Description
Technical field
The present invention relates to biomass energies to convert field, in particular it relates to a kind of special for biomass ash melting
Property analysis method.
Background technique
Biomass energy absorbs CO in its growth course2Participate in atmosphere in carbon cycle, it can be achieved that greenhouse gases zero
Discharge, it is a kind of environmental-friendly renewable cleaning energy that as fuel, sulphur, nitrogen content in biomass, which are far below coal and heavy oil,
Source.China is about 7.5 hundred million tons as large agricultural country, annual agricultural crop straw annual output, is equivalent to 3.75 hundred million tons of mark coals；Firewood and
The annual exploitable deposit of forestry waste resource is up to 600,000,000 tons or more.But every year because the remaining agricultural crop straw that can not be handled is in field
Direct burning amount is more than 200,000,000 tons, not only wastes stalk resource, while generating a large amount of gray haze.Therefore, biomass is developed and used
The energy can promote rural economic development, alleviate China's energy crisis, mitigate environmental pollution.In biomass utilization technologies, biology
Matter indirect gasification technology is considered as that a kind of great prospect produces hydrogen-rich combustion gas technology, which uses two-stage fluid bed, benefit
Be heat source with solid thermal carriers, under normal pressure reducing atmosphere condition, be not necessarily to making oxygen by air separation, so that it may obtain hydrogen and hydrocarbon content compared with
Therefore high medium calorific value gas is concerned in gasification of biomass field in recent years.Moreover, biomass gasifies in a fluidized bed
Have many advantages, such as that material is uniformly mixed, reaction speed is fast, residence time length, low operation temperature and yield are high in the reactor,
It is especially suitable for the biomass material that moisture content is high, calorific value is low.But content of ashes is higher in stalk biomass fuel, and contains
Have a large amount of alkali metal elements (potassium, sodium), and alkali metal compound has the characteristics that low-melting, brings to biomass transformation process
Problems can especially cause defluidization to even result in serious de-fluidized phenomenon because of clustering phenomena.Therefore, gasification is grasped
The melting characteristic of middle biomass ash can propose to inhibit to find solution because of the technical issues of alkali metal causes to be final.
Melting characteristic for biomass ash and the method for predicting its sintering, the general national standard for using for reference coal ash melting temperatur
(GB/T 30726-2014): initially pyramid method, this method define 4 kinds of characteristic temperatures, i.e., when evaluating coal ash
Deformation temperature DT, softening temperature ST, hemispherical fusion temperature HT and flowing temperature FT, and predicted using initial deformation temperature as sintering temperature
Value, this method are to change record characteristic temperature according to ash sample pattern, and can not continuously record the pattern variation of ash sample, and there are larger
Subjectivity；Moreover, showing that pyramid method is suitable for the higher sample of melting temperature according to the experimental results.In addition, thermomechanical point
Analysis method TMA (thermo-mechanical analyzer) is mainly used for measuring the expansion system of the substances such as plastics, glass in early days
The parameters such as several and phase transition temperature, because passing through the melting characteristic of the measuring method observable substance in entire heating process, once
There is researcher to propose the melting characteristic using thermomechanical analysis measurement coal ash.
But it is not specific to being proposed using thermomechanical analysis measurement coal ash process in existing research
Evaluation index.Moreover, the composition and content with coal ash have significant difference, the composition and its comparision contents of biomass ash
Complexity has the characteristics that the alkali metal contents such as potassium are higher, this causes biomass ash just to will appear melting phenomenon at a lower temperature.
This characteristic of biomass also determines the unworthiness that traditional pyramid method analyzes biomass ash melting characteristic.Therefore, for
Biomass material need to find the analysis method and evaluation index of a kind of suitable measurement biomass ash melting characteristic.
Summary of the invention
To solve the above-mentioned problems, inventor proposes and completes the present invention present invention.
The object of the present invention is to provide a kind of analysis methods for biomass ash melting characteristic.
Analysis method for biomass ash melting characteristic of the invention is measured using thermomechanical analyzer；Its
In, analytical procedure includes: the preparation of biomass ash sample, the measurement of biomass ash melting characteristic, the parsing of melting characteristic curve.
Specifically, the analysis method for biomass ash melting characteristic of the invention, comprising the following steps:
1) biomass ash sample the preparation of biomass ash sample: is made in biomass material burning；
2) measurement of biomass ash melting characteristic: biomass ash sample made from step 1) is carried out using thermomechanical analyzer
Test generates biomass ash melting characteristic curve；
3) parsing of biomass ash melting characteristic curve: pass through analytical procedure 2) obtain melting curve, determine feature temperature
It spends to evaluate the melting characteristic of biomass ash；Contraction rate is reached 0.1% for the first time/DEG C when corresponding temperature as biomass
Ash sintering characteristic temperature Ts；Contraction rate is increased to for the second time 0.1%/DEG C when corresponding temperature as biomass ash melt rank
Section characteristic temperature Tm；As shown in Figure 1；
4) characteristic temperature T is sintered with the biomass ashsEvaluation or prediction biomass ash start the characteristic temperature of sintering；
With the biomass ash melt stage characteristic temperature TmEvaluation is predicted during fluidized bed combustion and gasification by biomass
The characteristic temperature of agglomerate defluidization caused by ash melts.
Analysis method according to the present invention, wherein the step of step 1) burning is as follows: 1-1) by biomass material into
Row is crushed, is ground, and granularity is controlled in 1mm or less；1-2) the burning system ash in combustion furnace；1-3) ash sample obtained is ground
Sieving, granularity control in 0.1mm hereinafter, and using tablet press machine progress tabletting, sheet biomass ash sample is made.It is of the present invention
Combustion furnace can be any kind Small Combustion furnace well known in the art, such as it is preferable to use Muffle furnaces.
Analysis method according to the present invention, wherein grey process is made in the burning are as follows: by combustion furnace with heating rate 4~6
DEG C/min, rise to 250 DEG C from room temperature and kept for 40 minutes or more；It then proceedes to rise to 550 DEG C from 250 DEG C and be kept for 1.5 hours
More than.
Analysis method according to the present invention, wherein the step 2) thermomechanical analyzer is raw to sheet made from step 1)
Substance ash sample carries out testing procedure are as follows: sample is put into test cabinet, is passed through carrier gas；By thermomechanical analyzer with heating rate 2~
It 30 DEG C/min, after rising to 550 DEG C from room temperature, then with 1~6 DEG C/min is continuously heating to terminate.
Analysis method according to the present invention, wherein the carrier gas is air, oxygen, inert gas or reducing atmosphere.Institute
Stating inert gas is nitrogen, helium or argon gas；The reducing atmosphere is vapor, hydrogen or CO.Preferably, carrier gas is argon gas
Or vapor.
Analysis method according to the present invention, it is preferable that the biomass ash sample tested using thermomechanical analyzer
Amount is 30~70mg.
The present invention is suitable for various biomass materials, such as various straws and various forest branches, woody firewood etc.,
Specifically, for example, corn stover, wheat stalk, rice straw, peanut shell and branch etc..
The analysis method of biomass ash melting characteristic of the invention, the purpose is to provide a kind of method to evaluate in biomass
The melting characteristic that biomass ash varies with temperature during burning and gasification.Therefore, to have built small-sized fluidized bed in laboratory anti-
Device is answered, and the small-sized fluidized bed reactor built is utilized to investigate change of the biomass ash in bed during burning and gasification
Change.Experiment investigates biomass by the variation of bed pressure drop in record reaction process using several stalk biomass as raw material
The mistake fluidization characteristic of ash, and the initial temperature for defining bed pressure drop mutation is that agglomerate loses stream temperature, with TaIt indicates.
By comparing biomass ash in mini-reactor agglomerate defluidization characteristic temperature TaIt is melted with the ash obtained using TMA
Melt characteristic temperature TmIt is found that TaWith TmWithin the scope of ± 10 DEG C of difference, therefore, using the T obtained by TMAmTo predict biomass ash
Agglomerate lose stream temperature.Moreover, showing that TMA can accurately measure biomass samples by a large amount of results of laboratory
Initial sintering temperature and fusion temperature, and it is defined as biomass ash sintering stage characteristic temperature Ts(contraction rate reaches for the first time
0.1%/DEG C when corresponding temperature)；Biomass ash melt stage characteristic temperature Tm(contraction rate increases to 0.1% for the second time/DEG C
When corresponding temperature).Moreover, using TMA method can sensitive measurement to sample component change caused by ash softening point variation.
The present invention has the advantages that
1) compared with traditional coal ash meltbility measuring method, thermomechanical analysis of the present invention can be used to observe
Melting characteristic of the ash in entire heating process, and viscosity-temperature characteristic phase of the displacement popped one's head in test also with ash at high temperature
It closes, can preferably reflect the melting characteristic of ash, present preferably repeatability and accuracy；And traditional pyramid method is root
Change record characteristic temperature according to ash sample pattern, and can not continuously record the pattern variation of ash sample, there are larger subjectivities.
2) compared with the coal ash meltbility temperature that pyramid method obtains, a kind of biomass ash melting characteristic of the present invention
Analysis method, the characteristic temperature obtained using thermo-mechanical analysis method can more really be evaluated biomass ash and burn and gasifying
Coal ash meltbility in the process, the characteristic temperature T especially obtained by TMA methodmIt can be used to predict or evaluate and be melted by biomass ash
Melt the temperature for causing agglomerate defluidization phenomenon, this inhibits defluidization phenomenon in reaction process to propose that counte-rplan provide number to be final
According to and theories integration.
Detailed description of the invention
Fig. 1 is the melting curve for the biomass ash that the present invention utilizes thermomechanical analysis to obtain and its signal of characteristic temperature
Figure, wherein TsFor biomass ash sintering stage characteristic temperature, TmFor biomass ash melt stage characteristic temperature.
Fig. 2 is to be utilized respectively pyramid method to measure the characteristic temperature that several canonical biometric matter coal ash meltbilities obtain with TMA method
(schematic diagram of Examples 1 to 4), wherein WS is wheat stalk, and RS is rice straw, and PS is peanut shell, and CS is corn stover,
DT is initial deformation temperature, and ST is softening temperature, and HT hemispherical fusion temperature, FT is flowing temperature.
Fig. 3 is the melting curve of the known Melting Substance obtained using thermomechanical analysis.
Specific embodiment
The present invention is further explained in the light of specific embodiments.
Compared with comparative example measures the melting characteristic of biomass ash with pyramid method using TMA method respectively
The present invention be utilized respectively traditional pyramid method and this application involves TMA method investigated corn stover (CS), wheat
Several characteristic temperatures of stalk (WS), rice straw (RS), peanut shell (PS) coal ash meltbility, are respectively as follows:
In table, △ T1、△T2It respectively indicates are as follows: △ T1=DT-Ts；△T2=ST-Tm.By as a result, it has been found that, obtained using TMA method
The characteristic temperature T arriveds、TmCharacteristic temperature DT (initial deformation temperature), the ST obtained respectively lower than in table by pyramid method (softens temperature
Degree), show that biomass ash lower than sintering phenomenon has just occurred by pyramid method characteristic temperature DT, is being lower than characteristic temperature ST just
Melting phenomenon occurs.Thus it further shows that, obtained characteristic temperature and ash is recorded according to the variation of ash sample pattern by pyramid method
There are large errors for the variation that sample actually occurs.Therefore, the purpose of the present invention is to provide one kind to be suitable for biomass ash melting spy
Property analysis determining method, compared with the national standard (pyramid method) of traditional ash softening point, the biomechanical gray measured by TMA method is melted
The characteristic temperature of characteristic is closer to the actual temperature change observed in experiment.
In order to further verify the reliability that thermomechanical analysis measurement biomass ash melts characteristic, in combination with biomass original
This higher feature of potassium content in material, has selected potassium salt compound (KCl, K of fusing point known to three kinds2CO3、K2SO4) conduct pair
Than being utilized respectively that TMA method obtains respective melting curve (see Fig. 3) and its characteristic temperature is respectively as follows:
As can be seen from the results, the characteristic temperature obtained as TMA method fusing point known to each substance is very close, and the temperature difference range is only
±3℃.Thus result can be shown that, be the fusing point of the substance by the characteristic temperature that TMA method measures pure material.
Embodiment 1 measures the melting characteristic of corn stover ash using thermomechanical analysis (see Fig. 2-CS)
Using corn stover as raw material, crushed, ground 1mm sieve；In Muffle furnace with the heating rate of 5 DEG C/min from
Room temperature rises to 250 DEG C and keeps 1hr, then proceedes to rise to 550 DEG C from 250 DEG C and keeps 2hr, and ash sample is made；Ash sample is ground
Sieving, granularity are less than 0.1mm；It takes 50mg ash sample to carry out tabletting, is put into the test cabinet of thermomechanical analyzer；It is passed through argon gas, with 20
DEG C/heating rate of min rises to 550 DEG C from room temperature, 1000 DEG C/min is then continuously heating to 5 DEG C/min.By to melting
Tracing analysis obtains characteristic temperature: the sintering characteristic temperature T of corn stover ashsIt is 650 DEG C, the melt stage of corn stover ash
Characteristic temperature TmIt is 850 DEG C.And being respectively as follows: DT by the characteristic temperature that pyramid method obtains is 960 DEG C；ST is 1020 DEG C；HT is
1100℃；FT is 1150 DEG C.
Embodiment 2 measures the melting characteristic of rice straw ash using thermomechanical analysis (see Fig. 2-RS)
Using rice straw as raw material, crushed, ground 1mm sieve；With the heating rate of 4 DEG C/min from room temperature in Muffle furnace
It rises to 250 DEG C and is kept for 40 minutes, then proceed to rise to 550 DEG C from 250 DEG C and keep 1.5hr, ash sample is made；Ash sample is ground
Sieving, granularity are less than 0.1mm；It takes 40mg ash sample to carry out tabletting, is put into the test cabinet of thermomechanical analyzer；It is passed through argon gas, with 2
DEG C/heating rate of min rises to 550 DEG C from room temperature, it then proceedes to be warming up to 1050 DEG C/min with 2 DEG C/min.By to melting
Tracing analysis obtains characteristic temperature: the sintering characteristic temperature T of rice straw ashsIt is 651 DEG C, the melt stage characteristic temperature T of rice straw ashm
It is 810 DEG C.And being respectively as follows: DT by the characteristic temperature that pyramid method obtains is 890 DEG C；ST is 970 DEG C；HT is 1010 DEG C；FT is
1040℃。
Embodiment 3 measures the melting characteristic of peanut shell ash using thermomechanical analysis (see Fig. 2-PS)
Using peanut shell as raw material, crushed, ground 1mm sieve；With the heating rate of 6 DEG C/min from room in Muffle furnace
Temperature rise is to 250 DEG C and keeps 2hr, then proceedes to rise to 550 DEG C from 250 DEG C and keeps 3hr, and ash sample is made；Ash sample is ground
Sieve, granularity are less than 0.1mm；It takes 70mg ash sample to carry out tabletting, is put into the test cabinet of thermomechanical analyzer；Be passed through argon gas, with 30 DEG C/
The heating rate of min rises to 550 DEG C from room temperature, is then continuously heating to 1250 DEG C/min with 6 DEG C/min.By to melting curve
Analysis, obtains characteristic temperature: the sintering characteristic temperature T of peanut shell ashsIt is 701 DEG C, the melt stage characteristic temperature T of peanut shell ashm
It is 865 DEG C.And being respectively as follows: DT by the characteristic temperature that pyramid method obtains is 890 DEG C；ST is 960 DEG C；HT is 1020 DEG C；FT is
1050℃。
Embodiment 4 measures the melting characteristic of straw ash using thermomechanical analysis (see Fig. 2-WS)
Using wheat stalk as raw material, crushed, ground 1mm sieve；In Muffle furnace with the heating rate of 5 DEG C/min from
Room temperature rises to 250 DEG C and keeps 1hr, then proceedes to rise to 550 DEG C from 250 DEG C and keeps 2hr, and ash sample is made；Ash sample is ground
Sieving, granularity are less than 0.1mm；It takes 30mg ash sample to carry out tabletting, is put into the test cabinet of thermomechanical analyzer；It is passed through argon gas, with 20
DEG C/heating rate of min rises to 550 DEG C from room temperature, 1150 DEG C/min is then continuously heating to 1 DEG C/min.By to melting
Tracing analysis obtains characteristic temperature: the sintering characteristic temperature T of wheat stalk ashsIt is 720 DEG C, the melt stage of wheat stalk ash
Characteristic temperature TmIt is 1100 DEG C.And being respectively as follows: DT by the characteristic temperature that pyramid method obtains is 1130 DEG C；ST is 1150 DEG C；HT is
1170℃；FT is 1190 DEG C.
Certainly, the present invention can also there are many embodiments, without deviating from the spirit and substance of the present invention, are familiar with
Those skilled in the art can disclosure according to the present invention make various corresponding changes and modification, but these it is corresponding change and
Deformation all should fall within the scope of protection of the appended claims of the present invention.
Claims (8)
1. a kind of analysis method for biomass ash melting characteristic, comprising the following steps:
1) biomass ash sample the preparation of biomass ash sample: is made in biomass material burning；
2) measurement of biomass ash melting characteristic: biomass ash sample made from step 1) is surveyed using thermomechanical analyzer
Examination generates biomass ash melting characteristic curve；
3) parsing of biomass ash melting characteristic curve: pass through analytical procedure 2) obtain melting curve, determine characteristic temperature with
Evaluate the melting characteristic of biomass ash；Contraction rate is reached 0.1% for the first time/DEG C when corresponding temperature as biomass ash burning
Tie characteristic temperature Ts；Contraction rate is increased to for the second time 0.1%/DEG C when corresponding temperature it is special as biomass ash melt stage
Levy temperature Tm；
4) characteristic temperature T is sintered with the biomass ashsEvaluation or prediction biomass ash start the characteristic temperature of sintering；With institute
The biomass ash melt stage characteristic temperature T statedmEvaluation is predicted to be melted during fluidized bed combustion and gasification by biomass ash
The characteristic temperature of agglomerate defluidization caused by melting.
2. analysis method according to claim 1, which is characterized in that the step of step 1) burning is as follows: 1-1) will
Biomass material is crushed, is ground, and granularity is controlled in 1mm or less；1-2) the burning system ash in combustion furnace；It 1-3) will be obtained
Ash sample is ground up, sieved, granularity control in 0.1mm hereinafter, and using tablet press machine progress tabletting, sheet biomass ash sample is made.
3. analysis method according to claim 2, which is characterized in that grey process is made in the burning are as follows: by combustion furnace to rise
Warm 4~6 DEG C/min of rate, rise to 250 DEG C from room temperature and kept for 40 minutes or more；It then proceedes to rise to 550 DEG C from 250 DEG C and protect
It holds 1.5 hours or more.
4. analysis method according to claim 1, which is characterized in that step 2) is described to utilize thermomechanical analyzer to step
1) sheet biomass ash sample made from carries out testing procedure are as follows: sample is put into test cabinet, is passed through carrier gas；By thermomechanical analyzer
With 2~30 DEG C/min of heating rate, after rising to 550 DEG C from room temperature, then with 1~6 DEG C/min it is continuously heating to terminate.
5. analysis method according to claim 4, which is characterized in that the carrier gas is air, oxygen, inert gas or goes back
Originality atmosphere.
6. analysis method according to claim 5, which is characterized in that the inert gas is nitrogen, helium or argon gas；Institute
Stating reducing atmosphere is vapor, hydrogen or CO.
7. analysis method according to claim 6, which is characterized in that the carrier gas is argon gas or vapor.
8. -7 any analysis method according to claim 1, which is characterized in that tested using thermomechanical analyzer
The amount of biomass ash sample is 30~70mg.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610006897.8A CN105527312B (en) | 2016-01-04 | 2016-01-04 | A kind of analysis method for biomass ash melting characteristic |
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| CN107449526B (en) * | 2017-04-20 | 2019-05-03 | 清华大学 | A kind of burner hearth of determining biomass fired boiler is suitable for the method for outlet temperature |
| CN108519301B (en) * | 2018-03-12 | 2020-12-29 | 沈阳环境科学研究院 | Method for evaluating coal and biomass coke reactivity by using thermogravimetric analyzer |
| CN109490189B (en) * | 2018-12-29 | 2024-05-07 | 中国科学技术大学 | Low-temperature experimental device based on dynamic thermo-mechanical analyzer |
| CN113848152B (en) * | 2021-09-02 | 2024-05-14 | 山东东岳高分子材料有限公司 | Method for measuring melt viscosity of fluorine-containing polymer |
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