CN110218573A - A kind of no catalyst coal base heavy component method for upgrading - Google Patents
A kind of no catalyst coal base heavy component method for upgrading Download PDFInfo
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- CN110218573A CN110218573A CN201910524583.0A CN201910524583A CN110218573A CN 110218573 A CN110218573 A CN 110218573A CN 201910524583 A CN201910524583 A CN 201910524583A CN 110218573 A CN110218573 A CN 110218573A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B55/00—Coking mineral oils, bitumen, tar, and the like or mixtures thereof with solid carbonaceous material
Abstract
The invention belongs to low-temperature pyrolysis of coal tar technical fields, to solve in the heavy-oil modified techniques such as current catalytic hydrogenation, catalytic cracking, term restriction is higher than 400 DEG C, it is a larger energy consumption, the centrostigma for reducing economy, the difficulty that develops skill to entire technique, heavy component hydro-upgrading condition is harsh, catalyst inactivation is the problem that catalytic hydrogenation needs to face, and provides a kind of no catalyst coal base heavy component method for upgrading.350 DEG C of coalite tar or more fractions in heavy component use, biomass dry 12 hours 40-60 mesh pine sawdusts using 100 DEG C；Hydrogen supply dissolvent is to analyze pure naphthane to carry out the heavy component upgrading of coal base.After the addition of biomass pine sawdust, the n-hexane soluble matter yield of the heavy component of reaction raw material rises to 75.46% by 66.63%, and the addition of biomass pine sawdust promotes the lighting process of heavy component, product component Relatively centralized.Reaction temperature can be reduced to 320 DEG C, have stronger promote meaning to practical application.
Description
Technical field
The invention belongs to low-temperature pyrolysis of coal tar technical fields, and in particular to a kind of no catalyst coal base heavy component upgrading
Method.
Background technique
Coal resources in China relative abundance, wherein the reserves of low-order coal account for about 55%.Coal point based on pyrolysis of coal
Grade transformation technology is the important channel realizing low-order coal clean and effective and utilizing.However, tar obtained by the pyrolysis installation run at present
Yield is lower and its heavy components content is higher, and higher heavy component not only makes tar quality variation be difficult to utilize, and
And occluding device is easily condensed, influence the stable operation of pyrolysis system.For pyrolytic process of coal, realize that tar is light in research
There are mainly two types of the effective ways of matter, first is that introduce hydrogen-rich materials and coal copyrolysis, by pyrolysis of coal intermediate product hydrogen supply
The generation for influencing volatile matter obtains more tar light oils；Second is that the substance with catalytic pyrolysis ability is introduced, catalytic pyrolysis coal heat
The volatile matter generated is solved, tar quality is improved by regulation secondary response.Biomass hydrogen-rich and pyrogenous origin biomass semicoke
Has the function of catalytic pyrolysis pyrolysis of coal volatile matter.
But the heavy component of pyrolysis of coal generation accounting in entire thermal decomposition product is larger, accounts for about entire tar component and produces
50% or so of rate.With the increasingly increase to light-end products demand, the processing of heavy component and the importance utilized are more obtained
To embody.Main upgrading means include carrying out Group component separation to raw material first, such as by further distilling cutting at present,
It obtains multiple compared with narrow fraction, then processes upgrading respectively by fraction；Or extracted step by step using different solvents, obtain multiracial group
Point, such as the methods of toluene extracting etc..Although with different Group component separations method can by the more targeted upgrading of raw material,
But undoubtedly such feedstock processing mode makes processing process for upgrading more complicated and long flow path.Finding one kind can be directly by heavy
The method of component upgrading is current one of difficult point.
Heavy oil process for upgrading is all made of catalyst to catalyzing hydrogenating mostly at present, adds in the temperature window that can add hydrogen and cracking
Enter catalyst to improve light materialization of heavy oil degree, catalyst used at present is mainly Fe, Ni, Mo etc. transition metal-catalyzed
Agent, but the addition of catalyst will increase the cost of heavy-oil hydrogenation process, reduce its economy.Meanwhile because heavy component sheet
Negative effect is itself played for catalyst containing hetero atoms such as sulphur, nitrogen in body element, therefore, catalyst inactivation is also catalysis
Hydrogenation process needs one of the problem faced.
Biomass belongs to renewable resource, and the Land use systems of bioenergy are studied extensively all the time.Biomass sheet
Body carbon ratio with higher and hydrogen-carbon ratio, it is considered to be natural phenols aggregation, while possessing more alkali metal content
Deng.Independent biomass liquefying is furtherd investigate by many researchers, to pass through hydrogenation liquid using the attribute of its carbonaceous resource
Change be made oil product, but its oxygen content it is larger be believed to influence oil quality；There is researcher using phenols in its chemical composition then
Aggregation is expected that by hot-working conversion process and the chemicals such as single phenol is made, and realizes biomass high added value recycling benefit with this
With；For it rich in alkali metal components such as K, Na, part researcher, which is expected that by, to be added in other fossil energies, to fill
Point using itself and fossil energy synergistic effect, include that coal gasifies altogether with biomass, coal and biomass co grinding method, coal with it is biological
Matter copyrolysis and biomass semicoke catalytic pyrolysis semicoke etc..The resource utilization process that fossil energy adds biomass is one
Realize the process that the two has complementary advantages, most collaboration facilitation is confirmed by researcher among these.So similarly, in weight
In matter component hydroconversion process, the addition of biomass sawdust can also generate facilitation.
In the heavy-oil modified technique such as the catalytic hydrogenation, the catalytic cracking that are widely studied at present, condition is higher than 400 DEG C more,
Higher reaction temperature is then a larger energy consumption, the centrostigma for reducing economy, the difficulty that develops skill for entire technique.
Summary of the invention
The present invention in order to solve in the heavy-oil modified technique such as the catalytic hydrogenation being widely studied at present, catalytic cracking, compared with
High reaction temperature causes the harshness of reaction condition to be a larger energy consumption, reduction economy, raising for entire technique
The centrostigma of technical difficulty, heavy component hydro-upgrading condition is harsh, and catalyst inactivation is also that catalytic hydrogenation needs face
Problem the problems such as, provide a kind of no catalyst coal base heavy component method for upgrading.
The present invention is realized by following technical solution: a kind of no catalyst coal base heavy component method for upgrading, heavy component
350 DEG C of coalite tar or more the fractions in, biomass dry 12 hours 40-60 mesh pine sawdusts using 100 DEG C；Hydrogen supply is molten
Agent is to analyze pure naphthane to carry out the heavy component upgrading of coal base.
Specific method for upgrading are as follows: (1) heavy component and biomass are mixed according to the ratio of 2:1, raw material 1 is made；(2) will
Hydrogen supply dissolvent is added in raw material 1, is mixed after stirring to slurry, reaction raw materials 2 is made；(3) addition of reaction raw materials 2 high pressure is anti-
It answers in kettle, it is closed and after tightening nut, hydrogen is injected into kettle, pressure is 6MPa under room temperature in reaction kettle；(4) reaction kettle is controlled
Temperature rises to 320 DEG C or 360 DEG C by room temperature with 5 DEG C/min speed, maintains 60 minutes at 320 DEG C or 360 DEG C, entire anti-
Process is answered to be stirred with the revolving speed of 300r/min；(5) after reaction, autoclave Temperature fall is cooled to room temperature,
Solid, liquid, gas product is collected respectively for analyzing.
Hydrogen supply dissolvent is added under 320 DEG C and the following conditions in the present invention after mixing using mink cell focus with a small amount of biomass
Method obtains preferable lighting effect, since the addition of biomass can reduce reaction temperature.The incorporation of biomass can be to production
The lighting degree of product has an impact, and the incorporation of hydrogen supply dissolvent then will affect light oil ratio, therefore is intended to realize and preferably change
The proper ratio of matter effect, the two incorporation is particularly important.
For reducing the severe of reaction condition for actual in the process change of current coal tar heavy component
Significant in operating process, the present invention may be implemented heavy component is light using 320 DEG C or 360 DEG C, the reaction condition of 6MPa
The effect of matter.To verify reaction result of the invention, in designed experiment, reduction reaction pressure is investigated and reaction has been tied
The influence of fruit, thus it is speculated that be reduced to 4MPa also and can get preferable reaction result.
The present invention has chosen different reaction systems, after only being mixed by the biomass pine sawdust after drying with heavy component
It is reacted, and saves and biomass is first pyrolyzed to the process that system coke participates in reaction again.
The raw material that the present invention uses is middle coalite tar heavy component (hereinafter referred to as heavy more than 350 DEG C of fractions
Oil), which belongs to a part of product liquid in pyrolytic process.Because the part material molecular weight is bigger, structure is complicated, contains
There are a large amount of aromatic compounds, therefore is very limited in processing upgrading or use aspects.Heavy component in hydrogenation process,
Fragment is generated free radicals by thermal cracking, if can not be stablized by small molecule free radical, mutually condensation can be serious between larger free radical
Influence the lighting of upgrading processes.But heavy component largely belongs to bigger molecule, mostly uses catalysis to split greatly in close work
Macromolecular thermal cracking or catalytic pyrolysis are generated the free radical fragment compared with small molecule, later, with active stabilized hydrogen institute by the means such as change
The free radical of generation, so that raw material lighting.Such as during DCL/Direct coal liquefaction, correlative study person using biomass mix with
It is expected that by this and stablizes the free radical fragment generated in coal thermal cracking processes, improve the ratio of light components in tar.
And for heavy component hydrogenation system, it innovatively proposes for biomass to be added and react.This patent is innovative
Ground proposes that the simple and mechanical mixing of first two raw material will be reacted, then carries out hydrogenation reaction to the mixed raw material, can be obtained the two
The changing effect of promotion.So for complicated technical process, such raw material method of disposal greatly reduces technological operation
Complexity, while better Conversion Methods are provided for the process change of heavy component.
For the thought for directly mixing the two raw material, it is possible potentially for weight that removing is desirable with biomass
In matter component except the facilitation for adding hydrogen of fused ring compound.Biomass becomes semicoke without pyrolysis, but directly participates in
Reaction, the process will be for entirely reacting, because providing more active the characteristics of biomass high volatile itself
The free radical fragment of small molecule.Whereby, it in the hydrogenation process, is generated freely because be used to stablize heavy component cracking in environment
The lesser free radical debris concentration of base is significantly improved, which significantly promotes the lighting process of heavy component.
Characteristic high containing oxygen element using biomass itself simultaneously, according to pertinent literature, in heavy component hydrogenation process,
Its oxygenatedchemicals generated can have the process apparent promotion cracking process.Therefore, in heavy component hydrogenation process
Biomass, which is innovatively added, has apparent facilitation for lighting.
Meanwhile based on this analysis, in the thermal conversion processes of biomass, more small molecule free radical can be generated and be used for surely
Determine the free radical during heavy component, then during this cotransformation, because of the addition of biomass, the amount of product water
There is more apparent decline.It therefore, is also an important innovations point of this patent for producing water ratio decline during cotransformation.
For the process of biomass and other components cotransformation, because biomass itself has stronger liquefaction energy
Power, therefore the addition of biomass will be greatly reduced the severe of reaction condition.The heavy component and biomass corotation of this patent
In the system of change, after biomass is added as raw material, reaction temperature is reduced, is still had for entire reaction result
There are quite high liquefying conversion rate and n-hexane soluble matter yield.It is indicated above that biomass adds in lower reaction temperature
Enter and still plays a big part for heavy component cracking and hydrogenation process.Therefore, for reaction condition angle, by heavy group
Divide after mixing with biomass to have the severe of reaction process and be substantially reduced.
The present invention need not be handled raw material, and 350 DEG C of coal tar or more of fraction can be directly used as hot-working conversion and mention
Matter raw material；The present invention does not add any catalyst, the economy of heavy component upgrading is improved, simultaneously as containing in tar mink cell focus
Some sulphur, nitrogen heteroatom can generate side effect to catalyst, therefore be added without catalyst and light materialization of heavy oil can be realized, together
When the problem of catalyst inactivation is namely not present；The present invention adds a small amount of biomass during mink cell focus hydro-upgrading, control
The purpose of enhancing mink cell focus hydro-upgrading lighting degree can be realized in both systems corresponding proportion (2:1)；Pass through tar heavy group
Point, biomass, hydrogen supply dissolvent three determine ratio to obtain optimal lighting conversion results.To 400 DEG C -320 DEG C, with 40 DEG C
It for gradient, probes into the section, pine sawdust adds the influence converted to heavy component.Use 320 DEG C for the reaction of reaction temperature
The result shows that biomass addition can reduce the severe of heavy component hydro-upgrading condition really.
After the addition of biomass pine sawdust, the n-hexane soluble matter yield of reaction raw material is by 66.63%(heavy component
N-hexane soluble matter yield) rise to 75.46%, while further analysis shows, the addition of biomass pine sawdust is obviously promoted weight
The lighting process of matter component, and product component Relatively centralized.
Detailed description of the invention
Fig. 1 is the synchronous fluorescence result of biomass pine sawdust addition front and back and biomass pine sawdust；
Fig. 2 is mixed for reaction raw materials and is mixed fluorescence results with product result；
Synchronous fluorescence result under the reaction condition that Fig. 3 is 320 DEG C and 360 DEG C.
Specific embodiment
Embodiment 1: a kind of no catalyst coal base heavy component method for upgrading, heavy component use in coalite tar 350
DEG C or more fraction, biomass is using 100 DEG C of drying, 12 hours 40-60 mesh pine sawdusts；Hydrogen supply dissolvent be analyze pure naphthane into
Row coal base heavy component upgrading.
Specific method for upgrading are as follows: (1) heavy component and biomass are mixed according to the ratio of 2:1, raw material 1 is made；(2) will
Hydrogen supply dissolvent is added in raw material 1, is mixed after stirring to slurry, reaction raw materials 2 is made；(3) addition of reaction raw materials 2 high pressure is anti-
It answers in kettle, it is closed and after tightening nut, hydrogen is injected into kettle, pressure is 6MPa under room temperature in reaction kettle；(4) reaction kettle is controlled
Temperature rises to 320 DEG C or 360 DEG C by room temperature with 5 DEG C/min speed, maintains 60 minutes under the conditions of final temperature, entirely reacted
Journey is stirred with the revolving speed of 300r/min；(5) after reaction, autoclave Temperature fall is cooled to room temperature, respectively
Solid, liquid, gas product is collected for analyzing.It is not necessary that catalyst is added in whole process, the lightweight of tar heavy component can be realized
Change, reaches upgrading effect.
The heavy component (350 DEG C or more fractions) of present invention centering coalite tar by way of adding biomass carries out
Hydro-upgrading.Reaction result shows that the addition of biomass helps to realize the lighting degree of heavy component.To verify in biology
After the incorporation of matter pine sawdust, can be realized the effect of heavy component lighting without the addition of catalyst, design test as follows into
Row verifying: main to investigate the yield that point includes n-hexane soluble matter, and the aromatic hydrocarbons of the liquid product with fluorescence spectrum characterization
Number of rings.
1 mass balance of table
The analysis of 2 reaction product of table
Above-mentioned experiment 2,3 is the blank assay for testing 1, is excluded after biomass is added with expectation to entire liquefaction reaction oil product
Directly contribute.In the heavy component hydrogenation reaction participated in by the direct phenomenon of experimental result, biomass pine sawdust, entire reaction is produced
The liquid of flowing is presented in object (degasification is external in kettle) appearance.Be computed show biomass be added after oil yield (n-hexane is solvable
Object) it significantly increases, and also its absolute content is greater than the two and is individually superimposed under the conditions of.Therefore it could be assumed that, the addition of biomass
Help to improve the yield of n-hexane soluble matter in coalite tar mink cell focus hydroconversion process.
The lighting of mink cell focus process change process is had an impact really after being added for detection biomass, by product liquid
Using tetrahydrofuran as solvent after mixing, the solution that general concentration is 1mg/mL is configured.By sepectrophotofluorometer to the result
Carry out aromatic hydrocarbon number of rings characterization, the result is shown in Figure 1.
According to synchronous fluorescent spectrum analysis principle, the more long corresponding aromatic hydrocarbon number of rings of wavelength is more.From 1 series of Fig. 1 experiment
In can be shown that the transfer of number of rings lesser direction is presented in the hydro-conversion of heavy component after addition biomass really.
But biomass itself can also participate in liquefaction process as liquefaction raw material, therefore individually liquefy to exclude biomass
The incorporation of the oil of generation directly results in the lighting of mixing oil product, and it is the two (weight that two groups of experiments, which are arranged, to exclude experimental result only
Matter component, biomass pine sawdust) direct liquefaction simple superposition: the liquefaction products and heavy group for generation that biomass is individually liquefied
Divide the liquefaction products mixing for individually adding hydrogen, mixed proportion is that (1:1) and (1:3) is respectively labeled as testing 4 and testing 5(setting herein
If setting the ratio is for the mixture for being heavy component and biomass pine sawdust in analysis raw material, it is assumed that the result is that the letter of the two
Single superposition, that biomass oil productivity under the liquefaction condition is 1/4 or so, and the oil-producing contribution rate of heavy component is 7/10 or so,
In addition being mixed by raw material of 2:1, then biomass pine sawdust direct liquefaction oil-producing contribution rate substantially 5/28 in reaction product
Left and right, therefore the product result for configuring 1/4 and 1/2 accounting is compared with mix products result, to illustrate that the process is sent out really
Both raw collaboration facilitation).By two groups of experimental results according to being configured to tetrahydrofuran solution (1mg/ in proportion with previous experiments
), mL two groups of results and the synchronous fluorescence result of experiment 1 are shown in Fig. 2.
It is less than experiment 4 and experiment 5 according to the number of rings of synchronous fluorescence analysis experiment 1, illustrates to remove after biomass addition
Except the light oil of liquefaction contribution itself, the effect that a part promotes heavy component lighting is contributed to really.Therefore, biomass
The facilitation of the heavy end hydro-upgrading of centering coalite tar after sawdust addition.
In the reaction raw materials being composed of mink cell focus and biomass and hydrogen supply dissolvent, the ratio of each component is to product
It is affected.Correlative study thinks that hydrogen-rich solvent is considered as an important factor for directly affecting heavy oil thermal cracking process.Exist simultaneously
Under the conditions of the present invention, the experiment of not hydrogen supply dissolvent is designed, as a result there are many coking amount, almost without the generation of oil product, especially exist
In the experiment that biomass is added, coking phenomenon is more significant.Therefore under the conditions of this patent, hydrogen supply dissolvent naphthane is indispensable raw material
One of.In the system of the heavy component and biomass that are added due to naphthane, configurable raw material is mixed to slurry, this slurry raw material
For the main place of hot-working conversion process radical reaction.Meanwhile exactly because also hydrogen supply dissolvent is mixed in the slurry raw material
Enter, and forms liquid hydrogen-rich system, in the case where heating the reaction condition with hydrogen high pressure, heavy component lighting significant effect.
To investigate three's best relation, using 10g heavy component, the mixture of 2g biomass and 10g naphthane is previous experiments
Under same experimental conditions, hydro-upgrading experiment is done.The experimental results showed that the yield of n-hexane soluble matter drops compared with experiment 1
It is low, but both lighting degree of obtained oil product are close.By a series of experiments the result shows that, it is molten to hydrogen supply in mixed raw material
Agent optimal proportion should be at least more than 2.
It tests in 1-3, institute's exploratory response temperature is 400 DEG C, the Hydrogen Vapor Pressure of 6MPa.In view of still for " heavy component
Lighting process condition is harsh " the improvement of technological problems be not the addition of biomass it is obvious that relevant research is pointed out simultaneously
Guarantee that reaction result there are biggish contribution, is based on this simultaneously for reducing reaction temperature, supplement reaction condition is 320 DEG C (real
6) and the Hydrogenation Experiment of the heavy component under 360 DEG C (experiment 7) and biomass hybrid reaction it tests.
The experimental data are shown in the following table:
The experimental results showed that the oil yield in reaction result is also at the result greater than 75% under conditions of 320 DEG C with 360 DEG C.
Therefore it can be proved that 320 DEG C, under conditions of 6MPa, the hydrogenation process of the mixed raw material of heavy component and biomass pine sawdust, according to
So there is apparent facilitation.To judge lighting degree simultaneously, the oil product obtained to reaction continues to have done Fluorescent Characterization
Analysis.Such as Fig. 3.
According to Fig. 3 fluorescence results, although experiment 6(320 DEG C) in reaction result than experiment 7(360 DEG C) lighting
Degree is poor, but the result of the two is above experiment 5, is based on Such analysis, if the lighting degree of reaction result is greater than experiment 5
It can be shown that the two is acted synergistically.Therefore this experiment the results show that altogether add hydrogen reaction system in, exist really
Within the temperature range of 320 DEG C -400 DEG C, there are apparent facilitations.Based on this, the result of study of this patent is proved, biomass
Addition, can reduce the severe of heavy component lighting conversion reaction conditions.
Claims (2)
1. a kind of no catalyst coal base heavy component method for upgrading, it is characterised in that: coalite tar 350 in heavy component use
DEG C or more fraction, biomass is using 100 DEG C of drying, 12 hours 40-60 mesh pine sawdusts；Hydrogen supply dissolvent be analyze pure naphthane into
Row coal base heavy component upgrading.
2. a kind of no catalyst coal base heavy component method for upgrading according to claim 1, it is characterised in that: specific upgrading
Method are as follows: (1) heavy component and biomass are mixed according to the ratio of 2:1, raw material 1 is made；(2) hydrogen supply will be added in raw material 1
Solvent mixes to slurry after stirring, reaction raw materials 2 is made；(3) reaction raw materials 2 are added in autoclave, it is closed and twist
After tight nut, hydrogen is injected into kettle, pressure is 6MPa under room temperature in reaction kettle；(4) control temperature of reaction kettle is by room temperature
320 DEG C or 360 DEG C are risen to 5 DEG C/min speed, is maintained 60 minutes at 320 DEG C or 360 DEG C, entire reaction process is with 300r/
The revolving speed of min is stirred；(5) after reaction, autoclave Temperature fall is cooled to room temperature, respectively collect solid, liquid,
Gas product is for analyzing.
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Application publication date: 20190910 |
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