CN102021045A - Method for separating mixed gas containing tar - Google Patents
Method for separating mixed gas containing tar Download PDFInfo
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- CN102021045A CN102021045A CN2010101910627A CN201010191062A CN102021045A CN 102021045 A CN102021045 A CN 102021045A CN 2010101910627 A CN2010101910627 A CN 2010101910627A CN 201010191062 A CN201010191062 A CN 201010191062A CN 102021045 A CN102021045 A CN 102021045A
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- 238000000034 method Methods 0.000 title claims abstract description 43
- 239000007789 gas Substances 0.000 claims abstract description 184
- 239000011269 tar Substances 0.000 claims abstract description 125
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 112
- 239000003960 organic solvent Substances 0.000 claims abstract description 66
- 239000000047 product Substances 0.000 claims abstract description 46
- 239000012263 liquid product Substances 0.000 claims abstract description 36
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000011280 coal tar Substances 0.000 claims abstract description 17
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 239000001257 hydrogen Substances 0.000 claims abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 9
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910002091 carbon monoxide Inorganic materials 0.000 claims abstract description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 6
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims abstract 2
- 239000000203 mixture Substances 0.000 claims description 108
- 238000000926 separation method Methods 0.000 claims description 24
- 238000009835 boiling Methods 0.000 claims description 17
- 235000011089 carbon dioxide Nutrition 0.000 claims description 4
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- 239000001569 carbon dioxide Substances 0.000 abstract 1
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- 239000003921 oil Substances 0.000 description 31
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Abstract
The invention discloses a method for purifying a mixed gas containing tar, wherein the mixed gas containing tar comprises carbon monoxide, hydrogen, methane, carbon dioxide, tar and water. The method comprises the following steps of: 1. contacting the mixed gas containing tar with an organic solvent for 10s-120s to obtain a fist gaseous product and a fist liquid product, wherein the temperature of the organic solvent is 70-200 DEG C; 2. separating out the first liquid product; and 3. cooling the fist mixed gas to obtain purified gas and a second liquid product, and separating out the second liquid product. By using the method for purifying a mixed gas containing tar, coal tar oil and light oil with water content of lower than 1wt% can be obtained directly, and oil content of separated water is lower than 200mg/L.
Description
Technical field
The invention relates to a kind of separation method that contains the gas mixture of tar.
Background technology
Coal preparing natural gas technological line is representative with the international coal preparing natural gas of big plain in u.s.a demonstration unit (having moved 20 years) and Datang project at present, mainly adopt the Shandong strange/crushed coal pressure gasifying, the oil resistant of anti-sulphur conversion, low-temperature rectisol purify and methanation.Typical technical process is that first coal with extraction in the colliery carries out the coal choosing, is divided into broken coal, coal dust and coal gangue, and broken coal is used for pressurized gasification, and coal dust is used for destructive distillation, and coal gangue cooperates with coal dust and/or broken coal and is used for boiler generation steam and generating.The principal reaction of crushed coal pressure gasifying is coal and water generation water-gas reaction, obtains raw gas, and the main component of raw gas is synthetic gas (comprising carbon monoxide, hydrogen and methane), also has the undecomposed water of part, and a spot of coal tar component.The fine coal destructive distillation is that fine coal is heated under secluding air, makes it to be decomposed into the process of gas such as coal gas, liquid such as tar and solid (as coke).General destructive distillation is carried out in upright furnace, and this upright furnace generally comprises dryer section, retort section and cooling section from top to bottom.Feed coal at first enters the dryer section on stove top, the hot gas flow that utilizes retort section to produce carries out preheating to feed coal, be displaced downwardly to retort section then and carry out destructive distillation, solid product high temperature semicoke that destructive distillation obtains immerses and extinguishes in the water and produce a large amount of water vapour, the water vapour rising combines with the high temperature semicoke and produces a large amount of water-gas, water-gas rises to the airway of furnace roof and derives, the gas of deriving from airway is commonly referred to as raw gas, the coal gas that raw gas is mainly produced by destructive distillation in the stove, hot waste gas after the heating, from the water-gas of cooling section rising and the steam of dried feed coal generation, specifically can be referring to the disclosed low-temperature coal carbonization manufacturing technique of CN1966612A.
From foregoing description as can be known, the crushed coal pressure gasifying and the dry distillation of coal all produce carbon monoxide and hydrogen is the raw gas of main component, and the further methanation of carbon monoxide and hydrogen obtains methane gas (being SNG).The content of methane can be up to 96% in the product gas of coal preparing natural gas technology gained, calorific value 35564kJ/m
3More than.
Yet by the flow process of foregoing description as can be seen, the pressurized gasification of broken coal all must separate to come product raw gas or raw gas to obtaining to separate by chilling with the dry distillation of coal.In the chilling separating technology, the general water that adopts is as refrigerant, for example, CN1318550C discloses a kind of process for pressurized gasification of dry coal fines, wherein water is directly contacted with raw gas or raw gas, the material that makes all boiling points be higher than normal temperature comprises that dust all enters subsider together, collect gas-phase product, light oil flows out from the surface, and tar-bitumen is told from the lower end, the centre is the oily(waste)water that contains phenol and ammonia, and oily(waste)water is mainly by the part oil phase and water is miscible forms.Come from water contained in the gas mixture because water comprises, also comprise the water that comes from as the chilling agent, therefore, the amount of oily(waste)water is bigger.The aftertreatment of oily(waste)water is generally handled the coal tar of removing wherein by multistage sedimentation.Yet the water after multistage sedimentation is handled also contains the oil that nearly 1000mg/ rises, and also needs further to carry out follow-up deamination dephenolizing process after removing coal tar again, thereby reaches process water reuse or emission standard.This shows that the processing of oily(waste)water causes the water treatment expense to increase, therefore, oily(waste)water is treated as the main weak point of selecting crushed coal pressure gasifying in the coal preparing natural gas project for use.
In addition, US4324643 discloses a kind of method that is prepared stable hydro carbons by the solid particulate carbonaceous material, this method comprises 1) be enough to produce the described solid particulate carbonaceous material of thermo-cracking under the temperature and pressure condition of gas-solid mixture, described gas-solid mixture contains granular solids and hot pyrolysis gas product, and described gas products contains the above macromole hydrocarbon of 4 carbon atoms and the instant volatile hydrocarbon free radical that generates in reaction; 2) gas solid separation obtains not containing substantially the solid gaseous mixture; 3) the described solid gaseous mixture that do not contain is substantially mixed with the quench liquid that contains end-capping reagent, the condition of chilling makes that the instant volatile hydrocarbon free radical that generates almost can all react and termination reaction with end-capping reagent simultaneously in reaction, and the condensation simultaneously of feasible most of at least described macromole hydrocarbon, thereby obtain gas and condensation and stable hydrocarbon.And the temperature that further discloses condensation especially preferably is lower than 200 °F (promptly 95 ℃), and condensed fluid is mainly hydrocarbon.
Although adopt hydrocarbon can reduce the amount of water in the system to be separated, yet aforesaid method can not really solve the oily(waste)water problem as the main component of condensing agent.
Summary of the invention
The objective of the invention is in order to overcome the above-mentioned defective of prior art, a kind of separation method of the gas mixture that contains tar newly is provided.
In order to solve the oily(waste)water problem of above-mentioned prior art, the present inventor has carried out a large amount of research, found that, by adopting temperature is that 70-200 ℃ organic solvent (promptly oily) contacts with the gas mixture that contains tar, and the time that the control raw gas contacts with organic solvent is 10 seconds to 120 seconds, successfully realized being separated between the organism that water in the raw gas and coal tar wet goods produce oily(waste)water, make water and coal tar enter gas phase and liquid phase respectively, and by making gas phase further cooling and oily water separation, system's waste water oleaginousness is reduced to below the 200mg/L, even be low to moderate below the 50mg/L.
The invention provides a kind of purifying method that contains the gas mixture of tar, this gas mixture that contains tar contains carbon monoxide, hydrogen, methane, carbonic acid gas, tar and water, and this method may further comprise the steps:
(1) the described gas mixture that contains tar is contacted with organic solvent, the condition of contact comprises that the temperature of organic solvent is 70-200 ℃, and the time is 1 second to 120 seconds, obtains first gaseous product and first liquid product;
(2) isolate first liquid product;
(3) with described first gaseous product cooling, obtain the purified gas and second liquid product, isolate second liquid product.
The separation method that contains the gas mixture of tar provided by the invention directly contacts with the gas mixture that contains tar by adopting oil, and the temperature and time of control contact, make the tar that causes forming oily(waste)water form different phases respectively with water, be separated with realization, directly obtain coal tar and the light oil of water content less than 1 weight %, oil-contg only contains a spot of ammonia and phenol less than 200 mg/litre in the isolated water.Thereby efficiently solve the oily(waste)water problem.This shows, adopt method provided by the invention can reduce the cost of wastewater treatment.Method provided by the invention can be used for the various separation that can produce the mixed gas that contains tar of oily(waste)water problem.
Experimental results show that, when the temperature of organic solvent is lower than 70 ℃, although in theory by foreshortening to the duration of contact that makes organic solvent and raw gas when being less than 10 seconds, also can realize and can realize the described cooling that contains the gas mixture of tar fast, the condensing temperature (being liquefaction temperature) that makes the described temperature that contains the gas mixture of tar be reduced to be lower than tar and be higher than the dew-point temperature of water, but, because the temperature of organic solvent is low excessively, heat exchange between gas mixture and the organic solvent is too rapid, cause between gas mixture and the organic solvent contact abundant inadequately, thereby dissolving or the moisture that is included in the tar of gas mixture have little time to overflow from tar, and be separated with water in oil liquid phase emulsion droplet form and the gas phase composition of having overflowed, thereby the liquid phase that obtains is a large amount of water in oil liquid phase emulsion droplet, separating fully of tar and water can not be really realized, also just the oily(waste)water problem can not be really solved.
On the contrary, when the temperature of organic solvent is higher than 200 ℃, although the duration of contact by prolonging organic solvent and gas mixture is during more than 120 seconds, also can realize the described cooling that contains the gas mixture of tar, the condensing temperature (being liquefaction temperature) that the described temperature that contains the gas mixture of tar is reduced to be lower than tar and be higher than the dew-point temperature of water, but, because the temperature of organic solvent is too high, described gas mixture and the heat exchange between the organic solvent that contains tar is too slow, cause the described gas mixture that contains tar to be in the condition of high temperature for a long time, and owing to contain a large amount of unsaturated hydrocarbons in the tar, these unsaturated hydrocarbons are easy to take place further polymerization under the above-mentioned condition of high temperature, cause the viscosity of tar further to increase, form Jiao who is more prone to the thickness attitude, the content of oil then further reduces.In this case, the water that does not have enough time to overflow in the tar just is covered by among Jiao of this thickness attitude, and more difficult realization separates.
Description of drawings
Fig. 1 is the process flow sheet of the separation method of the gas mixture that contains tar provided by the invention.
Embodiment
Among the present invention, the described gas mixture that contains tar can be the various gas mixtures that contain tar, water and carbon monoxide that boiling point is higher than water, hydrogen, methane, carbonic acid gas simultaneously, for example, can be the gas mixture that crushed coal pressure gasifying produces, also can be the gas mixture that coal medium temperature carbonization, low-temperature pyrolysis produce.
The described starting temperature that contains the gas mixture of tar is not particularly limited, as long as water wherein exists with vapor form, is generally 80-750 ℃, is preferably 100-650 ℃; Pressure can high pressure, normal pressure, also can be pressure-fired, for example can be the 0.08-6 MPa, is preferably the 0.1-4 MPa.For different sources, the condition of gas mixture that contains tar is different.For example, for the gas mixture that crushed coal pressure gasifying produces, temperature is generally 150-750 ℃, is preferably 250-650 ℃; Pressure is generally the 1-10 MPa, is preferably the 2-6 MPa, more preferably the 2-4 MPa.For the gas mixture that the dry distillation of coal produces, temperature is generally 80-200 ℃, is preferably 90-180 ℃, and pressure is generally the 0.08-0.3 MPa, is preferably the 0.1-0.13 MPa.
Among the present invention, tar can be various boiling point height and the big black organism of viscosity, and its boiling point is generally up to more than 160 ℃.Carbon monoxide in the gas mixture, hydrogen, methane, carbonic acid gas are gaseous component at normal temperatures.
Except above-mentioned normal temperature descends to the component of gaseous component and tar and the water, also containing boiling point in the common described gas mixture is lower than water or ought for example be no more than 180 ℃ organic constituent with water, different because of the gas mixture source that contains tar, concrete component can be different.For example, for the crushed coal pressure gasifying and the dry distillation of coal, gained contains light component in the gas mixture of tar and also comprises usually under the normal temperature for liquid liquid ingredient such as phenol, biphenol, formic acid, gasoline, boiling point and be lower than in 180 ℃ the petroleum naphtha one or more.Therefore these components all are present in described first gaseous product with gas form under the condition of described contact owing to more volatile or very easily water-soluble.In order to make full use of the various useful components oil particularly in the above-mentioned gas mixture that contains tar, under the preferable case, method provided by the invention also comprises carries out oily water separation with second liquid product.
According to the separation method that contains the gas mixture of tar provided by the invention, although as long as the temperature of the organic solvent that control contacts with described raw gas is 70-200 ℃, time is 10 seconds to 120 seconds, can obtain first gas-phase product and first liquid product, reaches purpose of the present invention.But under the preferable case, in order further to improve separating of coal tar and water in the raw gas, the condition that described raw gas contacts with organic solvent comprises that the temperature of organic solvent is 80-180 ℃, and the time is 10-100 second, further preferred temperature is 80-150 ℃, and the time is 20-50 second.
And experimental results show that, when the described temperature that contains the gas mixture of tar is 150-750 ℃, when pressure was the 2-6 MPa, the temperature of controlling described organic solvent was that 70-200 ℃, duration of contact are 10-120 second, the consumption of described organic solvent be the described gas mixture weight that contains tar 1-15 doubly; The preferred described temperature that contains the gas mixture of tar is 250-650 ℃, and pressure is the 2-4 MPa, and the temperature of controlling described organic solvent is that 80-150 ℃, duration of contact are 10-50 second, the consumption of described organic solvent be the described gas mixture weight that contains tar 1-5 doubly.In above-mentioned scope particularly in the optimum condition scope, can prevent because the temperature of organic solvent is low excessively, the gas mixture and the heat exchange between the organic solvent that contain tar are too rapid, contacting between the gas mixture that contains tar that causes and the organic solvent may be abundant inadequately, thereby dissolving or the moisture that is included in the tar of the gas mixture that contains tar may have little time to overflow from tar, and be separated with water in oil liquid phase emulsion droplet form and the gas phase composition of having overflowed, thereby the liquid phase that obtains is a large amount of water in oil liquid phase emulsion droplet, separating fully of tar and water can not be really realized, also just the oily(waste)water problem may not be really solved; Can also prevent because the temperature of organic solvent is too high, the gas mixture and the heat exchange between the organic solvent that contain tar are too slow, the gas mixture that contains tar that causes may be in the condition of high temperature for a long time, and owing to contain a large amount of unsaturated hydrocarbons in the tar, these unsaturated hydrocarbons are easy to take place further polymerization under the above-mentioned condition of high temperature, cause the viscosity of tar further to increase, form Jiao who is more prone to the thickness attitude, the content of oil then further reduces.In this case, the water that does not have enough time to overflow in the tar just is covered by among Jiao of this thickness attitude, and more difficult realization separates.
The above-mentioned gas mixture that contains tar is a raw gas for the crushed coal pressure gasifying product for example, this contains in the gas mixture of tar, the content of described water is generally the described 10-60 weight % that contains the raw gas of tar, 25-50 weight % more preferably, the 0.1-20 weight % of the raw gas total amount outside the content of tar is generally and dewaters, be preferably 2-10 weight %, more preferably 3-6 weight %.That is to say that suppose that the content of water in the described gas mixture that contains tar is 30 weight %, the content of tar is the described 0.7-14 weight % that contains tar gas mixture total amount for the 0.1-20 weight % among the remaining 70 weight % then, preferred 0.35-10.5 weight %.
Owing to make the water in the described raw gas keep gaseous state temperature required closely related, make the water in the described raw gas keep gaseous state temperature required also different under the different pressures with pressure.In order to reduce consumption as far as possible as the organic solvent of refrigerant, the present invention preferably uses the big as far as possible organic solvent of gasification latent heat, the gasification latent heat of concrete preferred described organic solvent is greater than 50 kilojoule per kilogram, 50-2000 kilojoule per kilogram for example, the gasification latent heat of further preferred organic solvent is the 150-1000 kilojoule per kilogram.When the gasification latent heat of described organic solvent is the 50-2000 kilojoule per kilogram, the condition of described contact comprise the consumption of described organic solvent be described raw gas weight 1-15 doubly, the time of contact is can realize making that the temperature of described raw gas was reduced to 200-300 ℃ in 10 seconds to 120 seconds; When the gasification latent heat of described organic solvent is the 150-1000 kilojoule per kilogram, the condition of described contact comprises that the consumption of described organic solvent is 2-10 a times of described raw gas weight, and the time of contact can realize making that the temperature of described raw gas is reduced to 200-300 ℃ for 10-45 second.
Among the present invention, unless stated otherwise, described gasification latent heat is meant 1 gasification latent heat under the normal atmosphere.Boiling point is meant the boiling point under the standard state.
And the temperature that ought describedly contain the gas mixture of tar is 80-200 ℃, pressure is the 0.08-0.3 MPa, the temperature of control organic solvent is 80-120 ℃, be 10-120 second duration of contact, the consumption of described organic solvent be the described gas mixture that contains tar weight 0.5-5 doubly, the preferred described temperature that contains the gas mixture of tar is 90-180 ℃, pressure is the 0.1-0.13 MPa, the temperature of control organic solvent is 80-120 ℃, be 5-50 second duration of contact, and the consumption of described organic solvent also can effectively prevent above-mentioned organic solvent temperature too high or duration of contact of the oversize oily(waste)water problem that causes when being 1-3 times of the described gas mixture weight that contains tar.
The described gas mixture that contains tar can be various destructive distillation products such as the dry distillation of coal, such as biomass carbonization, shale oil destructive distillation, the pyrogenous product of oil-sand of stalk etc.In above-mentioned destructive distillation obtains the described gas mixture that contains tar, described outside the content of tar is generally and dewaters contains the 1-25 weight % of total amount of the gas mixture of tar, and the content of water is generally 1-30 weight %.
According to the present invention, higher when the described mixture temperature that contains tar, when particularly tar wherein was gas phase, described organic solvent was refrigerant or chilling agent with respect to the described gas mixture that contains tar; And the mixture temperature that ought describedly contain tar is lower, and when being lower than the boiling temperature of water especially, described organic solvent is a thermal source with respect to the described gas mixture that contains tar.
On the other hand, in the above two kinds of cases, described organic solvent also plays washing composition or extraction agent, by contacting between described organic solvent and the described gas mixture that contains tar, described organic solvent with the organic composition in the described gas mixture that contains tar particularly tar wash or extract.
Among the present invention, described organic solvent can be a single solvent, also can be the mixed solvent of multiple organic solvent.Industrial preferred use boiling range as in 180-500 ℃ coal tar, hydrocracking tail oil, diesel oil and the wax oil one or more as described organic solvent.
Further under the preferable case, to the described organic solvent of small part for by separating the tar that the described gas mixture that contains tar obtains, the liquid product that also is about to described step (1) gained is partly or entirely as described organic solvent, can reduce the amount of outsourcing organic solvent so on the one hand, save production cost, the liquid product that has also solved step (1) gained on the other hand is the emission problem of tar.
According to method provided by the invention, the contacting of the described gas mixture that contains tar and described organic solvent is that the direct method of contact, the mode of described direct contact can be that the described gas mixture that contains tar is with the organic solvent counter current contact or and stream contact or adverse current also flows the mode of carrying out simultaneously.
For organic solvent is fully contacted with the gas mixture that contains tar, effectively carry out heat exchange, washing (tar in the described gas mixture that contains tar being washed by organic solvent), the present invention preferably can make described organic solvent contact with the gas mixture that contains tar with vaporific form by accessory in liquid distributor or spraying gun or other tower containers.
According to method provided by the invention, the further cooling of product that the gained cat head is overflowed is in order to make oil phase and the gas delivery in water and the light component, therefore the refrigerative temperature preferably is cooled to 10-60 ℃, further preferred 20-50 ℃ so that water can be cooled to liquid state is as the criterion.Can realize separating of gaseous fraction, lightweight oil phase and water simultaneously like this, improve the yield of separation efficiency and lightweight oil phase.
Because the present invention only relates to the improvement to the separation method of the gas mixture that contains tar, therefore, the described preparation method that contains the gas mixture of tar can be a method well known in the art, for example, can adopt crushed coal pressure gasifying method well known in the art to obtain or adopt dry distillation of coal method well known in the art to obtain.Described broken coal can be to be not less than 5 millimeters various broken coal pieces, and for example size is the broken coal piece of 5-80 millimeter.Described pressurized gasification condition comprises that the bottom temp of plus-pressure furnace is 1000-1500 ℃, and outlet mixed gas temperature can be 150-750 ℃, and pressure can be the 2-6 MPa, and preferred temperature is 250-650 ℃, and pressure is the 2-4 MPa.Described pressurized gasification can carry out in the various vapourizing furnaces known in the art, for example, can carry out in pressurized-gasification furnace, upright furnace, lurgi gasifier at crushed coal pressure gasifying.The method of the described dry distillation of coal can be low-temperature pyrolysis, also can medium temperature carbonization, and can also be high temperature carbonization.The destructive distillation condition comprises that the bottom temp of gas retort is 800-1100 ℃, and the top gas temperature out can be the 0.08-0.3 MPa for 500-750 ℃, pressure.Being used for pyrogenous coal can be fine coal and/or broken coal, and described fine coal can be that all size is no more than 5 millimeters fine coal.Described destructive distillation can be carried out in the various vapourizing furnaces known in the art, for example, can carry out in conventional upright furnace, lurgi gasifier or the fluidized bed dry distillation technology stove that uses in destructive distillation field.
According to one embodiment of the present invention, the separation method of the described gas mixture that contains tar as shown in Figure 1.The gas mixture such as the raw gas that will contain tar directly contact with organic solvent in gas-liquid separator such as chilling separator, obtain first gaseous product and first liquid product, composition in the described gas mixture that contains tar except that tar as be under water and the normal temperature gasiform component substantially or all as described in first gaseous product, whole or most tar are in described first liquid product, after further heat exchange is promptly cooled off in interchanger such as condenser with described first gaseous product, obtain second gaseous product (mainly being to be the gasiform component under the normal temperature) and second liquid product (mainly being water and lightweight oil), by further oily water separation, obtain water and lightweight oil.Water can circulate and be used for pressurized gasification or distillation process.
The following examples will the present invention is described further.
Embodiment 1
This embodiment is used to illustrate the separation method that contains the gas mixture of tar provided by the invention.
Adopt technology shown in Figure 1, water vapor is carried out pressurized gasification with big or small sending at 1: 1 with weight ratio for the brown coal broken coal of 5-50 millimeter (relevant rerum natura sees table 1 for details) in the vapourizing furnace, the bottom temp of vapourizing furnace is 1200 ℃, head temperature is 500 ℃, base pressure is 3.5MPa, top pressure is 3MPa, obtain pressure and be 3MPa, temperature and be the gas mixture that 500 ℃ crushed coal pressure gasifying product promptly contains tar and discharge (composition outside dewatering is as shown in table 2, and the content of water is 30 weight % of crushed coal pressure gasifying product total amount) from top of gasification furnace.
Be 3 MPas with this pressure then, temperature is that 500 ℃ crushed coal pressure gasifying product is 100 ℃ with 1000 kilograms/hour flow and temperature, boiling range is 180-500 ℃, flow is that 2800 kilograms/hour coal tar contacts in the chilling separator, contact after 25 seconds, with liquid product is that first liquid product (temperature is 280 ℃) is discharged at the bottom of tower, in contact process, gas-phase product i.e. first gaseous product (temperature is 200 ℃) is overflowed from cat head, gas-phase product is further sent in the subsider by behind the interchanger indirect heat exchange to 50 ℃, collection is from subsider top escaping gas component (synthetic gas), liquid in the subsider is left standstill natural layering, isolate wherein water and organic phase.The result is that water is transparent, and oleaginousness is 50mg/L.Liquid product learns that by analysis water content is 0.2 weight % at the bottom of the tower.
Embodiment 2
This embodiment is used to illustrate the separation method that contains the gas mixture of tar provided by the invention.
Adopt technology shown in Figure 1, water vapor is carried out pressurized gasification with big or small sending at 1: 1 with weight ratio for the brown coal broken coal of 5-50 millimeter (relevant rerum natura sees table 1 for details) in the vapourizing furnace, the bottom temp of vapourizing furnace is 1000 ℃, head temperature is 300 ℃, base pressure is 3MPa, top pressure is 2.5MPa, the crushed coal pressure gasifying product that obtains pressure and be 2.5 MPas, temperature and be 300 ℃ is discharged (composition outside dewatering is as shown in table 2, and the content of water is 50 weight % of crushed coal pressure gasifying product total amount) from the top.
Be 2.5 MPas with this pressure then, temperature is that 300 ℃ crushed coal pressure gasifying product is 150 ℃ with 1500 kilograms/hour flow and temperature, boiling range is 280-480 ℃, flow is that 2200 kilograms/hour hydrocracking tail oil contacts in the chilling separator, contact after 40 seconds, liquid product (temperature is 280 ℃) is discharged at the bottom of tower, gas-phase product (temperature is 210 ℃) is overflowed from cat head, gas-phase product is further sent in the subsider by behind the interchanger indirect heat exchange to 40 ℃, collection is from subsider top escaping gas component (synthetic gas), liquid in the subsider is left standstill natural layering, isolate wherein water and organic phase, the discovery water is transparent, and oleaginousness is 100mg/L.Liquid product learns that by analysis water content is 0.3 weight % at the bottom of the tower.
Embodiment 3
This embodiment is used to illustrate the separation method that contains the gas mixture of tar provided by the invention.
Adopt technology shown in Figure 1, water vapor is carried out pressurized gasification with big or small sending at 1: 1 with weight ratio for the brown coal broken coal of 5-50 millimeter (relevant rerum natura sees table 1 for details) in the vapourizing furnace, the bottom temp of vapourizing furnace is 1300 ℃, head temperature is 650 ℃, base pressure is 4MPa, top pressure is 3.5MPa, the crushed coal pressure gasifying product that obtains pressure and be 3.5 MPas, temperature and be 650 ℃ is discharged (composition outside dewatering is as shown in table 2, and the content of water is 20 weight % of crushed coal pressure gasifying product total amount) from the top.
Be 3.5 MPas with this pressure then, temperature is that 650 ℃ crushed coal pressure gasifying product is 80 ℃ with 800 kilograms/hour flow and temperature, boiling range is 180-500 ℃, flow is that 2500 kilograms/hour coal tar contacts in the chilling separator, contact after 30 seconds, liquid product (temperature is 260 ℃) is discharged at the bottom of tower, gas-phase product (temperature is 190 ℃) is overflowed from cat head, gas-phase product is further sent in the subsider by behind the interchanger indirect heat exchange to 40 ℃, collection is from subsider top escaping gas component (synthetic gas), liquid in the subsider is left standstill natural layering, isolate wherein water and organic phase, the discovery water is transparent, and oleaginousness is 150mg/L.Liquid product is learnt water content 0.4 weight % by analysis at the bottom of the tower.
Comparative Examples 1
Method according to embodiment 1 is obtained synthetic gas, and different is, the temperature of coal tar is 50 ℃, and the time of contact is 10 seconds, obtains gaseous fraction (synthetic gas), water and oil phase.The result is that water is opaque, and oleaginousness is 500mg/L.Liquid product learns that by analysis water content is 2 weight % at the bottom of the tower.
Embodiment 4
This embodiment is used to illustrate the separation method that contains the gas mixture of tar provided by the invention.
Adopt technology shown in Figure 1, with size is that the long-flame coal lump coal (relevant rerum natura see table 1 for details) of 25-80mm carries out destructive distillation in upright furnace, the bottom temp of upright furnace is 900 ℃, temperature after the raw gas ammonia spray is 100 ℃, base pressure is 0.14MPa, and top pressure is 0.11MPa, obtains pressure and be 0.11MPa, temperature and be the gas mixture that 100 ℃ raw gas promptly contains tar, composition outside raw gas dewaters is as shown in table 3, and water-content is 30 weight % of raw gas total amount.
Then with this raw gas with double centner/hour flow and temperature be 180 ℃, boiling range is 180-500 ℃, flow is 200 kilograms/hour coal tar contact, contact after 100 seconds, liquid product i.e. first liquid product is discharged at the bottom of tower, gas-phase product is that (temperature is 100 ℃ to first gaseous product, pressure is 0.11 MPa) overflow from cat head, gas-phase product is further sent in the subsider by behind the interchanger indirect heat exchange to 50 ℃, collection is purified gas from subsider top escaping gas component, liquid in the subsider is left standstill natural layering, isolate wherein water and organic phase.The discovery water is transparent, oleaginousness 60mg/L.At the bottom of the tower liquid product by analysis, water content is 0.1 weight %.
Embodiment 5
This embodiment is used to illustrate the separation method that contains the gas mixture of tar provided by the invention.
Adopt technology shown in Figure 1, with size is that the long-flame coal lump coal (relevant rerum natura see table 1 for details) of 25-80mm carries out destructive distillation in upright furnace, the bottom temp of upright furnace is 700 ℃, temperature after the raw gas ammonia spray is 160 ℃, base pressure is 0.12MPa, and top pressure is 0.106MPa, and obtaining pressure is that 0.108MPa, temperature are 160 ℃ raw gas, composition outside raw gas dewaters is as shown in table 3, and water-content is 0.05 times of weight of the total amount of the described gas mixture that contains tar.
Then with this raw gas with double centner/hour flow and temperature be 90 ℃, boiling range is 180-500 ℃, flow be double centner/hour coal tar contact, contact after 60 seconds, liquid product is discharged at the bottom of tower, (temperature is 160 ℃ to gas-phase product, pressure is 0.106 MPa) overflow from cat head, gas-phase product is further sent in the subsider by behind the interchanger indirect heat exchange to 50 ℃, collection is synthetic gas from subsider top escaping gas component, liquid in the subsider is left standstill natural layering, isolate wherein water and organic phase, the discovery water is transparent, and oleaginousness is 110mg/L.At the bottom of the tower liquid product by analysis, water content is 0.5 weight %.
Embodiment 6
This embodiment is used to illustrate the separation method that contains the gas mixture of tar provided by the invention.
Adopt technology shown in Figure 1, with size is that the long-flame coal lump coal (relevant rerum natura see table 1 for details) of 25-80mm carries out destructive distillation in upright furnace, the bottom temp of upright furnace is 850 ℃, temperature after the raw gas ammonia spray is 180 ℃, base pressure is 0.13MPa, and top pressure is 0.102MPa, and obtaining pressure is that 0.102MPa, temperature are 180 ℃ raw gas, composition outside raw gas dewaters is as shown in table 3, and water-content is 0.1 times of weight of purified gas total amount.
Then with this raw gas with double centner/hour flow and temperature be 100 ℃, boiling range is 180-500 ℃, flow be double centner/hour coal tar contact, contact after 20 seconds, liquid product is discharged at the bottom of tower, (temperature is 180 ℃ to gas-phase product, pressure is 0.102 MPa) overflow from cat head, gas-phase product is further sent in the subsider by behind the interchanger indirect heat exchange to 50 ℃, collection is synthetic gas from subsider top escaping gas component, liquid in the subsider is left standstill natural layering, isolate wherein water and organic phase, the discovery water is transparent, and oleaginousness is 120mg/L.At the bottom of the tower liquid product by analysis, water content is 0.3 weight %.
Comparative Examples 2
Method according to embodiment 4 is obtained raw gas, and different is, the temperature of coal tar is 300 ℃, and the time of contact is 300 seconds, obtains gaseous fraction (synthetic gas), water and oil phase.The result is that water is translucent, and oleaginousness is 1200mg/L.At the bottom of the tower liquid product by analysis, water content is 3 weight %.
Table 1
| Project | Brown coal | Long-flame coal (sub-bituminous coal) |
| Technical analysis (weight %) War Wad Aad Vad Sad | 36.90 17.81 12.02 29.49 1.21 | 8.00 7.39 21.90 35.17 0.36 |
| Ultimate analysis (weight %) Car Har Oar Nar Sar | 52.23 3.20 12.06 0.61 1.21 | 53.75 4.15 11.43 1.02 0.36 |
| Ash fusion point (℃) T1 T2 T3 | 1160 1200 1220 | 1420 greater than 1500 greater than 1500 |
Annotate:
War---represent coal-fired as received basis moisture; Wad---the coal-fired dry basic moisture of expression; Har---represent coal-fired as received basis hydrogen branch; Aad---the coal-fired dry basic ash content of expression; Vad---the coal-fired dry basic volatile matter of expression; Sad---the coal-fired dry basic sulphur content of expression; Car---represent coal-fired as received basis carbon branch; Oar---represent coal-fired as received basis oxygen branch; Nar---represent coal-fired as received basis nitrogen branch; Sar---represent coal-fired as received basis sulphur content; T1---softening temperature, ℃; T2---hemispherical temperature, ℃; T3---melt temperature, ℃.
Table 2
| Form (weight %) | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative Examples 1 |
| H 2 | 3.59 | 3.61 | 3.58 | 3.59 |
| CO | 19.68 | 19.75 | 19.56 | 19.68 |
| CO 2 | 62.88 | 63.09 | 62.71 | 62.88 |
| CH 4 | 7.57 | 7.35 | 7.65 | 7.57 |
| N 2 | 0.34 | 0.34 | 0.34 | 0.34 |
| C 2 | 0.39 | 0.36 | 0.39 | 0.39 |
| C 3 | 0.39 | 0.35 | 0.39 | 0.39 |
| H 2S | 0.50 | 0.50 | 0.51 | 0.50 |
| NH 3 | 0.17 | 0.17 | 0.17 | 0.17 |
| HCN | 0.01 | 0.01 | 0.01 | 0.01 |
| C 6H 6O | 0.39 | 0.39 | 0.39 | 0.39 |
| C 6H 6O 2 | 0.26 | 0.26 | 0.26 | 0.26 |
| Petroleum naphtha (＜180 ℃) | 0.41 | 0.38 | 0.41 | 0.41 |
| Middle oil (180-360 ℃) | 1.60 | 1.57 | 1.70 | 1.60 |
| Heavy oil (＞360 ℃) | 1.82 | 1.87 | 1.93 | 1.82 |
| ∑ | 100.00 | 100.00 | 100.00 | 100.00 |
| The oil product total amount | 4.48 | 4.47 | 4.69 | 4.48 |
Table 3
| Form (weight %) | Embodiment 4 | Embodiment 5 | Embodiment 6 | Comparative Examples 2 |
| H 2 | 5.73 | 5.50 | 5.69 | 5.73 |
| CO | 30.89 | 30.85 | 30.83 | 30.89 |
| CO 2 | 14.00 | 13.84 | 13.97 | 14.00 |
| CH 4 | 23.50 | 23.93 | 23.67 | 23.50 |
| N 2 | 7.96 | 7.85 | 7.94 | 7.96 |
| C 2 | 1.52 | 1.55 | 1.51 | 1.52 |
| C 3 | 1.99 | 2.02 | 1.99 | 1.99 |
| H 2S | 0.92 | 0.91 | 0.92 | 0.92 |
| NH 3 | 0.26 | 0.24 | 0.24 | 0.26 |
| HCN | 0.02 | 0.02 | 0.02 | 0.02 |
| C 6H 6O | 0.13 | 0.13 | 0.13 | 0.13 |
| C 6H 6O 2 | 0.07 | 0.07 | 0.07 | 0.07 |
| Petroleum naphtha (＜180 ℃) | 1.97 | 1.99 | 1.98 | 1.97 |
| Middle oil (180-360 ℃) | 4.29 | 4.28 | 4.30 | 4.29 |
| Heavy oil (＞360 ℃) | 6.75 | 6.82 | 6.74 | 6.75 |
| ∑ | 100.00 | 100.00 | 100.00 | 100.00 |
| The oil product total amount | 13.21 | 13.29 | 13.22 | 13.21 |
Annotate: in the table 2-table 3, the oil product total amount is meant C
6H
6O+C
6H
6O
2The amount of+petroleum naphtha+middle oil+heavy oil
Table 4
From the result of table 4 as can be seen, adopt method provided by the invention can effectively realize oily water separation in raw gas and the raw gas, thereby effectively solve the oily(waste)water problem, and Comparative Examples 1 and Comparative Examples 2 are respectively because the temperature of quenching oil is too low and too high, W/O content after the separation is than higher, oil-contg can not be realized oily water separation well, thereby can not solve the oily(waste)water problem than higher in the water.This shows that can the temperature of quenching oil and duration of contact be the key points that solve the oily(waste)water problem.
Claims (10)
1. treatment process that contains the gas mixture of tar, this gas mixture that contains tar contains carbon monoxide, hydrogen, methane, carbonic acid gas, tar and water, and this method may further comprise the steps:
(1) the described gas mixture that contains tar is contacted with organic solvent, the condition of contact comprises that the temperature of organic solvent is 70-200 ℃, and the time is 10 seconds to 120 seconds, obtains first gaseous product and first liquid product;
(2) isolate first liquid product;
(3) with described first gaseous product cooling, obtain the purified gas and second liquid product, isolate second liquid product.
2. method according to claim 1, wherein, the condition that the described gas mixture that contains tar contacts with organic solvent comprises that the temperature of organic solvent is 80-180 ℃, the time is 10-100 second.
3. method according to claim 1 and 2, wherein, the described temperature that contains the gas mixture of tar is 150-750 ℃, pressure is the 2-6 MPa, the consumption of described organic solvent be the described gas mixture weight that contains tar 1-15 doubly.
4. method according to claim 3, wherein, the described temperature that contains the gas mixture of tar is 250-650 ℃, pressure is the 2-4 MPa, the consumption of described organic solvent be the described gas mixture weight that contains tar 1-5 doubly.
5. method according to claim 3, wherein, in the described gas mixture that contains tar, the content of water is 10-60 weight %, the content of tar is the 0.1-20 weight % of the total amount of described outside the dewatering gas mixture that contains tar.
6. method according to claim 1 and 2, wherein, the described temperature that contains the gas mixture of tar is 80-200 ℃, pressure is the 0.08-0.3 MPa, the consumption of described organic solvent be the described gas mixture weight that contains tar 0.5-5 doubly.
7. method according to claim 6, wherein, the described temperature that contains the gas mixture of tar is 90-180 ℃, pressure is the 0.1-0.13 MPa, the consumption of described organic solvent be the described gas mixture that contains tar weight 1-3 doubly.
8. method according to claim 6, wherein, in the described gas mixture that contains tar, the content of tar is the 1-25 weight % of the total amount of described outside the dewatering gas mixture that contains tar, the content of water is 1-30 weight %.
9. method according to claim 1, wherein, this method also comprises carries out oily water separation with second liquid product.
10. method according to claim 1, wherein, described organic solvent is that boiling range is one or more in 180-500 ℃ coal tar hydrocracking tail oil, diesel oil and the wax oil.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103292575A (en) * | 2012-03-02 | 2013-09-11 | 林德股份公司 | Method and apparatus for obtaining gas product and liquid methane from synthesis gas |
| CN103771338A (en) * | 2014-01-09 | 2014-05-07 | 上海鑫兴化工科技有限公司 | Transformation method and transformation system of water gas containing light oil |
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| US4286971A (en) * | 1979-10-05 | 1981-09-01 | Bethlehem Steel Corporation | Removal of naphthalene from recirculated wash oil |
| CN1043334A (en) * | 1988-12-14 | 1990-06-27 | 克鲁普科普斯有限公司 | From the coal gas of partial oxidation, remove the method for hydrogen sulfide |
| US6312505B1 (en) * | 1999-11-19 | 2001-11-06 | Energy Process Technologies, Inc. | Particulate and aerosol remover |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4286971A (en) * | 1979-10-05 | 1981-09-01 | Bethlehem Steel Corporation | Removal of naphthalene from recirculated wash oil |
| CN1043334A (en) * | 1988-12-14 | 1990-06-27 | 克鲁普科普斯有限公司 | From the coal gas of partial oxidation, remove the method for hydrogen sulfide |
| US6312505B1 (en) * | 1999-11-19 | 2001-11-06 | Energy Process Technologies, Inc. | Particulate and aerosol remover |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103292575A (en) * | 2012-03-02 | 2013-09-11 | 林德股份公司 | Method and apparatus for obtaining gas product and liquid methane from synthesis gas |
| CN103771338A (en) * | 2014-01-09 | 2014-05-07 | 上海鑫兴化工科技有限公司 | Transformation method and transformation system of water gas containing light oil |
| CN103771338B (en) * | 2014-01-09 | 2016-06-01 | 上海尧兴投资管理有限公司 | Containing lightweight oil water-gas shift method with containing lightweight oil water-gas shift system |
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