CN106701176A - Method used for processing high temperature coal tar - Google Patents
Method used for processing high temperature coal tar Download PDFInfo
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- CN106701176A CN106701176A CN201510769230.9A CN201510769230A CN106701176A CN 106701176 A CN106701176 A CN 106701176A CN 201510769230 A CN201510769230 A CN 201510769230A CN 106701176 A CN106701176 A CN 106701176A
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- high temperature
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G67/00—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/205—Metal content
Abstract
The invention provides a method used for processing high temperature coal tar. The method comprises following steps: high temperature coal tar is subjected to fractionation so as to obtain a light fraction and a heavy fraction; the heavy fraction, vacuum 3st side cut of naphthenic crude, and a demulsifier are mixed, and are introduced into a pretreatment reactor, and an obtained mixture is stirred, is allowed to stand, and is separated so as to obtain a liquid phase and an insoluble substance; the liquid phase, solvent naphtha, and an alcoholic compound are mixed, and are introduced into a demetalization reactor; contact reaction with a filling material is carried out, an obtained reaction effluent is delivered into a water washing column, and is contacted with fresh water so as to obtain a mixed substance; the mixed substance is introduced into a dehydrating tower for separation so as to obtain metal-free high temperature coal tar and water. The method can be used for removing metal in high temperature coal tar under mild conditions, purifying coal tar raw material, and delaying metal inactivation of catalysts in hydrogenation reactors and increasing of bed pressure drop.
Description
Technical field
The invention belongs to field of coal tar deep processing, and in particular to the processing method of high temperature coal-tar.
Background technology
Coal tar is the fluid product that coal is obtained during destructive distillation and gasification.Difference according to pyrolysis temperature and method can
Obtain following several tar：Low temperature (450 DEG C~650 DEG C) retort tar；(600 DEG C~800 DEG C) generation oven cokes of low temperature and middle temperature
Oil；The vertical coke oven tar of middle temperature (900 DEG C~1000 DEG C)；High temperature (1000 DEG C) coking tar.No matter which kind of tar is with thorn
Swash the black of property stink or the thick liquid of dark brown., between 0.98~1.2g/cm3, its value is with temperature for density at 20 DEG C
Rising and reduce.Coal tar is the organic mixture based on aromatic hydrocarbon, containing 10,000 multiple compounds, extractible about 500
Kind.At present, there are about 50 kinds of value and extractable and economical rationality, light oil that its deep processing is obtained, phenol, naphthalene, wash
The series of products such as oil, anthracene, carbazole, indoles, pitch be synthetic plastic, synthetic fibers, agricultural chemicals, dyestuff, medicine, coating, auxiliary agent and
The basic material of fine chemical product, is also the base stock of the industries such as metallurgy, synthesis, construction, weaving, papermaking, traffic, many
Product is unavailable in petrochemical industry, therefore, coal tar processing can promote the development of these industries.And improve the utilization of resources
Rate, is conducive to environmental protection and develops a circular economy.
Because processing temperature is different, the composition and property of correspondence coal tar have very big difference, and especially high temperature coal-tar property is most
It is poor quality, middle coalite tar is two kinds of completely different tar with high temperature coal-tar, and composition is without water content is different, metal
Also difference is very big for content, and high temperature coal-tar is a kind of material of dark oil, there is special odor, compared with middle coalite tar,
High temperature coal-tar density is big, carbon residue is high, condensed-nuclei aromatics content is high, and especially high with the heavy constituent content such as colloid, asphalitine, metal contains
Amount is high.Containing 10%~30% moisture content in high temperature coal-tar, and the state of Water-In-Oil is presented.The coalite tar treatment side in
Method is not appropriate for processing high temperature coal-tar, it is necessary to find new process route and process conditions.
As economic development and light-weight fuel oil demand constantly increase, by coal tar hydrogenating production light-weight fuel oil increasingly
The favor of tar producer is obtained, middle coalite tar hydrogenation production light Fuel oil tech is relatively ripe, in the industry cycle promotes
It is more.But middle coalite tar and high temperature coal-tar are two kinds of completely different tar, and nature difference is very big, high temperature coal-tar mesh
The industrialized device of front-end hydrogenation is relatively fewer, it is reported that industrialized device has Qitaihe treasured ACE Semi Coal Chemical Industry limited at present
100,000 tons of industrialized units of company, it uses high temperature coal-tar back-end crop technology, by the colloid in coal tar, asphalitine and machinery
Impurity removal, hydrotreating is carried out by light component, and in addition, not yet document report has industrialized plant running.Cause height
Warm coal tar fails extensive industrialized reason and constitutes much relations with its property, and wherein one of reason is high temperature coal-tar restructuring
Point content is high, and especially the condensed-nuclei aromatics content such as colloid, asphalitine is high, and the tenor such as wherein corresponding Fe, Ca, Na is special
Height, in using traditional fixed bed hydrogenation processing procedure, these metals can be deposited on catalyst surface or bed after being removed
In layer space, catalyst is caused to inactivate or bed pressure drop rising, especially Hydrodemetalation catalyst superficial metal deposition amount is big,
Catalyst deactivation rate and pressure drop rise speed especially cause device shortening service cycle soon.
Patent CN1676583A describes a kind of high temperature coal tar hydrocracking technique, and wherein high temperature coal tar is introduced
Heating furnace mixes with hydrogen, and hydrofining reactor, then the hydrogen isolated into high-pressure separator through exchanging heat are entered after mixing
Hydrofining reactor is returned to through circulating hydrogen compressor, generation oil enters low pressure separator, enters after low point of fuel oil of sub-department
Deoxidation tower, fractionating column is entered after further taking off fuel gas, and gasoline, diesel oil and lubricating oil are obtained after fractionation, and tail oil enters to be hydrocracked
Reactor.In this patent in high temperature coal tar a large amount of metals of content etc. be easily caused catalyst inactivation and bed pressure drop rise
Component, is directly processed in the case where not anticipated to raw material using traditional hydrofining reactor, can cause to urge
Agent deactivation rate is accelerated and bed pressure drop rises, and then causes device shortening service cycle.
At present, there are a variety of drawbacks in domestic existing coal tar processing, and many enterprises are directly using coal tar as combustion
Material is sold, and do so poor product quality, added value are low and also extremely serious to the pollution of environment.With market competition not
The increasingly strict specification in terms of environmental protection of disconnected intensification and country and requirement, adequately and reasonably become people using tar resource
The hot issue increasingly paid close attention to.Hydrogenation of tar technology can haul out the thing of the post-combustion pollution environment such as sulphur, nitrogen in coal tar
Matter, improves smell, color and the stability of oil product, improves oil quality, is a kind of important means of coal tar comprehensive utilization.Coal
Tar had to pass through before hydrogenation plant is entered with treatment, remove the components, ability such as water therein, impurity, asphalitine, metal
It is normally carried out hydrogenation process.Therefore, to the research of coal tar preprocessing process, improve energy utilization rate, reduce energy consumption and
Increase enterprise profit aspect significant.
The content of the invention
It is big for current high temperature coal-tar studies on asphaltene, tenor, carry out hydrogenation reactor Nei Tuojin during hydrogenation reaction
The shortcoming that metal catalyst metal deposition capability is big, deactivation rate is fast, the present invention provides a kind of process for processing high temperature coal-tar,
The existence form and actual tests result of metal in the coal tar that Binding experiment research finds, remove high in the case where process conditions are relaxed
Metal in warm coal tar, purifies coal tar raw material, slows down the metal inactivation and bed pressure drop of catalyst in hydrogenation reactor
Rise, for high temperature coal-tar provides a kind of feasible processing method.
Found by studying, there be very the existence form of metal with the existence form of metal in traditional residual oil in high temperature coal-tar
Big difference, metal is mainly the metals such as Ni, V, and many presence in the form of porphyrin metal complex in residual oil, due to these metals
Be embedded in heavy constituent colloid and the asphalitine in residual oil, it is necessary in the presence of catalyst and hydrogen high temperature removal；And high temperature
Metal in coal tar is mainly and exists with metal oxide forms such as Fe, Ca, Na, Ni, V tenor seldom, this and its shape
Relevant into process, coal steam needs Water spray to cool down during High T-emperature Carbonization, and the salt such as Ca, Mg in water can enter in coal tar, together
When the dry distillation of coal during have substantial amounts of coal ash, furnace wall breakage thing and some mineral matters（Calcite, albite）Deng doping wherein,
These materials can carry substantial amounts of alkaline metal oxide（CaO, Na2O、MgO、Fe2O3）Into in high temperature coal-tar, while high
In warm coal tar storage and transportation, coal tar is entered because the reasons such as corrosive pipeline also result in the part metals ion such as Fe
Oil, as the above analysis, metal in high temperature coal-tar with the presence of be greatly with mineral form, so if
It is clearly contretemps to be applied on coal tar metal removal using traditional demetallated mode of residual oil again.But due to high temperature
Coal tar contains 10%~30% moisture, and the state that Water-In-Oil is presented more, there is a certain degree of emulsification, is sent out in process of the test
Now it is difficult to be demulsified coal tar and remove metal therein using the general demulsifier of tradition.
Based on above-mentioned discovery, the present invention provides a kind of process for processing high temperature coal-tar, and methods described includes as follows
Content：
（1）High temperature coal-tar is segmented to obtain light fraction and heavy distillat, and the cut-point is 330~400 DEG C, preferably 360~
380℃；
（2）Step（1）The line distillate that subtracts three of the heavy distillat for obtaining and naphthene base crude enters preatreating reactors after mixing, and fills
Divide standing, isolated liquid phase and insoluble matter after stirring；
（3）Step（2）Enter demetalization after the liquid phase that obtains, solvent naphtha, alcohols material mixing and preheated to 150~250 DEG C
Reactor, contacts with the filler loaded in demetalization reactor and is reacted；
（4）Step（3）The reaction effluent for obtaining enters water scrubber, is fully contacted with fresh water, is dissociateed in reaction effluent
The metal inorganic substance for coming is dissolved into water phase；
（5）Step（3）The mixture for obtaining enters dehydrating tower, carries out water-oil separating, obtains removing the high temperature coal-tar after metal
And water；
（6）Step（1）The insoluble matter for obtaining mixes with aromatic solvent, isolated aromatic hydrocarbons DDGS and aromatic hydrocarbons insoluble matter；
（7）By step（6）Aromatic hydrocarbons in the aromatic hydrocarbons DDGS for obtaining is distilled off, and obtains steaming excess；
（8）By step（1）Light fraction, the step for obtaining（5）The high temperature coal-tar and step for obtaining（7）The steaming excess mixing for obtaining
It is uniform to obtain pretreated high temperature coal-tar.
In the inventive method, the high temperature coal-tar is heating final temperature being obtained through destructive distillation or coking more than 900 DEG C
High temperature coal-tar.
In the inventive method, the line distillate that subtracts three of the naphthene base crude is 1 with the weight ratio of high temperature coal-tar：50~
1:10。
In the inventive method, step（2）In can also add demulsifier.
In the inventive method, step（2）In can also add auxiliary agent, the auxiliary agent is 1- butyl -3- methylimidazole tetrafluoros
Borate and/or 1- butyl -3- methylimidazole hexafluoro borates, the consumption are the 1/50000~1/ of high temperature coal-tar weight
15000。
In the inventive method, the boiling range of the solvent naphtha is 65~450 DEG C, preferably 120~400 DEG C, more preferably 150
~320 DEG C, can be specifically hydrofining diesel oil, hydrofinishing naphtha, hydrofinishing washing oil, hydrofinishing light oil, hydrogenation
One or several mixture in refined carbolic oil.
In the inventive method, step（3）Described in the weight ratio of solvent naphtha and high temperature coal-tar be 1:20~1:3, preferably
It is 1:10~1:5.
In the inventive method, the alcohols material can be one or more in methyl alcohol, ethanol, isopropanol, sec-butyl alcohol.
The addition of the alcohols material is the 1/10000~1/100 of high temperature coal-tar weight；It is preferred that 1/5000~1/500.
In the inventive method, in the demetalization reactor filler of filling can be ceramic ring, quartz sand, activated carbon,
One or several in diatomite, silica, aluminum oxide, zeolite, preferably ceramic ring, diatomite, activated carbon and titanium dioxide
Silicon；The aperture of the filler is 200nm~50 μm, preferably 300nm~10 μm.
In the inventive method, 2~5 layers of filling of filler point in the demetalization reactor preferably divide 3~4 layers of filling,
And along Flow of Goods and Materials direction filler aperture from large to small, while bed voidage is also from large to small, adjacent two layers filling
The pore size difference of thing is 50nm~1000nm, to those skilled in the art, when point multilayer loads filler, multilayer
The ratio of filler is that those skilled in the art can determine by existing knowledge.
In the inventive method, the demetalization reactor can be two and be arranged in parallel, when wherein one reactor reaches
During processing limit, switch another demetalization reactor.
In the inventive method, the filler of filling is different from traditional Hydrodemetalation catalyst in demetalization reactor, this
Filler has very strong appearance dirt and interception capacity in text, but does not have catalysis activity substantially；Therefore tradition can be avoided de-
When metallic catalyst is because of high-temperature hydrogenation caused by aromatic hydrocarbons polycondensation the problems such as catalyst coking.
Compared with prior art, the inventive method has the following advantages that：
1st, in the inventive method, high temperature coal-tar fractionation is obtained into light fraction and heavy distillat, impurity, metal, asphalitine etc. first
It is concentrated mainly in heavy distillat, can so reduces treating capacity, viable economically, the heavy distillat that will obtain and naphthene base crude
Precipitation is had after the line distillate that subtracts three is well mixed, through impurity, part colloid in the mainly coal tar of analysis precipitation
And asphalitine, meanwhile, a part of metal is also deposited and is carried out.
2nd, in the inventive method, it is found that the metal in high temperature coal-tar exists with inorganic salt form, using the inventive method
Can remove metal impurities therein under the relative operating condition for relaxing, it is to avoid conventional method using hydrogenation high temperature removal into
This problem high.
3rd, the inventive method operates the metal in removing coal tar at a lower temperature, can avoid alkadienes in coal tar
Deng unsaturated hydrocarbons, easy polycondensation causes the problem that catalyst is inactivated at high temperature.
4th, in the inventive method, the demetalization reactor inner stuffing is without carried metal, and aperture is big, and retention and appearance are dirty
Ability is strong, cost less than carried metal in conventional method catalyst for demetalation, while can effectively catching remove
Metallic salt.
5th, in the inventive method, dilution precipitating reagent is used as by using solvent naphtha, body can be destroyed by adding solvent naphtha
The colloidal stability of system, on the one hand reduces the viscous force between original component, on the other hand by the asphalitine in Jiao He centers
Parsed etc. heavy constituent, the components precipitate such as toluene insolubles and mechanical admixture for most being suspended in system at last gets off, while companion
As most precipitated metals get off.
6th, in the inventive method, add auxiliary agent alcohols material, because alcohols material contains hydroxyl, with coal tar in it is oxygen-containing
Compound aldehydes matter property is similar, can reach and dissolve each other, and the metal inorganic salt hydrophily come is dissociateed in such coal tar by force,
Can be dissolved into alcohols, in follow-up water scrubber, alcohols material carries salt can be mixed with excessive water, form new mixing
Thing, and new mixture is poor with coal tar intersolubility, and then realize that coal tar is separated with alcohol-water mixture.
Specific embodiment
Technical scheme is further illustrated below by specific embodiment, but is not limited to the embodiment.
High temperature coal-tar raw material that the embodiment of the present invention is used, naphthene base crude subtract three line distillate, solvent oil nature
Table 1 is listed in respectively, and demetalization processor process conditions are shown in Table 2.Direction is loaded respectively from top to bottom in the demetalization processor
Ceramic ring, diatomite, four kinds of fillers of activated carbon and silica, the aperture of four kinds of fillers be respectively 5~10 μm, 1~3
μm, 500nm~900nm, 300~500nm, the admission space ratio of four kinds of fillers is 30:25:25:20, solvent naphtha is
Naphtha and diesel fuel mixtures that hydrotreating is obtained, the demulsifier are the SLD-G031 model demulsifiers of triumph chemical industry.
The feedstock property of table 1
Embodiment 1
Test raw material is high temperature coal-tar and the line distillate that subtracts three described in table 1, and the alcohols material is ethanol, and reaction condition is shown in
Table 2, reaction result is referring to table 3.
Embodiment 2
Test raw material is high temperature coal-tar and the line distillate that subtracts three described in table 1, and the alcohols material is ethanol, while adding 1-
Butyl -3- methyl imidazolium tetrafluoroborates, ethanol consumption is 1 with the weight ratio of high temperature coal-tar:25000, reaction condition is shown in Table
2, reaction result is referring to table 3.
Embodiment 3
Test raw material is high temperature coal-tar and the line distillate that subtracts three described in table 1, and the alcohols material is methyl alcohol, while addition is helped
Agent 1- butyl -3- methylimidazole hexafluoro borates and demulsifier, auxiliary dosage are 1 with the weight ratio of high temperature coal-tar:25000,
The consumption of the demulsifier is the 1/20000 of coal tar weight, and reaction condition is shown in Table 2, and reaction result is referring to table 3.
Comparative example 1
Same as Example 1, difference is that line distillate does not mix high temperature coal-tar with subtracting three, and reaction condition is shown in Table 2, instead
Result is answered referring to table 3.
Comparative example 2
Same as Example 2, difference is to be added without alcohols material, and reaction condition is shown in Table 2, and reaction result is referring to table 3.
The reaction condition of table 2 and result
Claims (15)
1. it is a kind of process high temperature coal-tar process, methods described include following content：
（1）High temperature coal-tar is segmented to obtain light fraction and heavy distillat, and the cut-point is 330~400 DEG C,；
（2）Step（1）The line distillate that subtracts three of the heavy distillat for obtaining and naphthene base crude enters preatreating reactors after mixing, and fills
Divide standing, isolated liquid phase and insoluble matter after stirring；
（3）Step（2）Enter demetalization after the liquid phase that obtains, solvent naphtha, alcohols material mixing and preheated to 150~250 DEG C
Reactor, contacts with the filler loaded in demetalization reactor and is reacted；
（4）Step（3）The reaction effluent for obtaining enters water scrubber, is fully contacted with fresh water, is dissociateed in reaction effluent
The metal inorganic substance for coming is dissolved into water phase；
（5）Step（3）The mixture for obtaining enters dehydrating tower, carries out water-oil separating, obtains removing the high temperature coal-tar after metal
And water；
（6）Step（1）The insoluble matter for obtaining mixes with aromatic solvent, isolated aromatic hydrocarbons DDGS and aromatic hydrocarbons insoluble matter；
（7）By step（6）Aromatic hydrocarbons in the aromatic hydrocarbons DDGS for obtaining is distilled off, and obtains steaming excess；
（8）By step（1）Light fraction, the step for obtaining（5）The high temperature coal-tar and step for obtaining（7）The steaming excess mixing for obtaining
It is uniform to obtain pretreated high temperature coal-tar.
2. in accordance with the method for claim 1, it is characterised in that：The cut-point of the high temperature coal-tar is 360~380 DEG C.
3. in accordance with the method for claim 1, it is characterised in that：Step（2）Described in naphthene base crude the line cut that subtracts three
Oil is 1 with the mass ratio of high temperature coal-tar:50~1:10.
4. in accordance with the method for claim 1, it is characterised in that：Step（3）Described in alcohols material be methyl alcohol, ethanol, different
One or more in propyl alcohol, sec-butyl alcohol.
5. in accordance with the method for claim 1, it is characterised in that：The addition of the alcohols material is high temperature coal-tar weight
1/10000~1/100；It is preferred that 1/5000~1/500.
6. in accordance with the method for claim 1, it is characterised in that：Step（1）Middle addition auxiliary agent, the auxiliary agent be 1- butyl-
3- methyl imidazolium tetrafluoroborates and/or 1- butyl -3- methylimidazole hexafluoro borates.
7. in accordance with the method for claim 1, it is characterised in that：Step（1）Middle addition demulsifier.
8. in accordance with the method for claim 1, it is characterised in that：The boiling range of the solvent naphtha is 65~450 DEG C.
9. in accordance with the method for claim 1, it is characterised in that：The solvent naphtha is hydrofining diesel oil, hydrofinishing stone
One or several in cerebrol, hydrofinishing washing oil, hydrofinishing light oil, hydrofinishing carbolic oil.
10. in accordance with the method for claim 1, it is characterised in that：Step（2）Described in solvent naphtha and high temperature coal-tar weight
Amount is than being 1:20~1:3.
11. in accordance with the method for claim 1, it is characterised in that：The filler of filling is porcelain in the demetalization reactor
One or several in ring, quartz sand, activated carbon, diatomite, silica, aluminum oxide, zeolite.
12. in accordance with the method for claim 1, it is characterised in that：The filler of filling is porcelain in the demetalization reactor
Ring, diatomite, activated carbon and silica.
13. in accordance with the method for claim 1, it is characterised in that：The aperture of the filler is 200nm~50 μm.
14. in accordance with the method for claim 1, it is characterised in that：2~5 layers of filler point in the demetalization reactor
Filling, and along Flow of Goods and Materials direction filler aperture from large to small, while bed voidage is also from large to small.
15. in accordance with the method for claim 15, it is characterised in that：The pore size difference of the adjacent two layers filler is
50nm~1000nm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107188295A (en) * | 2017-06-02 | 2017-09-22 | 珠海路德通环保科技有限公司 | Preprocess method before a kind of coking chemical waste water is biochemical |
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| CN101629107A (en) * | 2008-09-22 | 2010-01-20 | 何巨堂 | Method for hydro-upgrading coal tar containing heavy distillate |
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| CN107188295A (en) * | 2017-06-02 | 2017-09-22 | 珠海路德通环保科技有限公司 | Preprocess method before a kind of coking chemical waste water is biochemical |
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