CN109456793B - Synchronous industrial co-production method - Google Patents
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- CN109456793B CN109456793B CN201811180755.9A CN201811180755A CN109456793B CN 109456793 B CN109456793 B CN 109456793B CN 201811180755 A CN201811180755 A CN 201811180755A CN 109456793 B CN109456793 B CN 109456793B
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- 230000001360 synchronised effect Effects 0.000 title description 3
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000007788 liquid Substances 0.000 claims abstract description 32
- 239000003245 coal Substances 0.000 claims abstract description 29
- 239000001993 wax Substances 0.000 claims abstract description 25
- 239000012188 paraffin wax Substances 0.000 claims abstract description 21
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 20
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 15
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 8
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 8
- 229940094933 n-dodecane Drugs 0.000 claims abstract description 8
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 4
- 238000000926 separation method Methods 0.000 claims description 55
- 238000000034 method Methods 0.000 claims description 19
- 238000001179 sorption measurement Methods 0.000 claims description 19
- 239000002808 molecular sieve Substances 0.000 claims description 15
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 15
- 238000004821 distillation Methods 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- OKTJSMMVPCPJKN-IGMARMGPSA-N Carbon-12 Chemical compound [12C] OKTJSMMVPCPJKN-IGMARMGPSA-N 0.000 claims description 2
- OKTJSMMVPCPJKN-BJUDXGSMSA-N carbon-11 Chemical compound [11C] OKTJSMMVPCPJKN-BJUDXGSMSA-N 0.000 claims description 2
- 239000012847 fine chemical Substances 0.000 abstract description 4
- 238000010992 reflux Methods 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000003795 desorption Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 229940057995 liquid paraffin Drugs 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000003208 petroleum Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000010117 shenhua Substances 0.000 description 2
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- -1 acrylic ester Chemical class 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000004523 catalytic cracking Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000000271 synthetic detergent Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Classifications
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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
- C10G53/00—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes
- C10G53/02—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only
- C10G53/08—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only including at least one sorption step
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention relates to the field of fine chemicals, in particular to an industrial co-production method for synchronously preparing light liquid wax, heavy liquid wax, n-dodecane, n-decane, n-heptane, n-hexane and a series of isoparaffin, which is characterized in that the adopted raw materials are normal stable light hydrocarbon, a coal indirect liquefied first Fischer-Tropsch product and a coal indirect liquefied second Fischer-Tropsch product which are blended according to a certain proportion, so that the weight ratio of the normal paraffin to the isoparaffin is (0.8-1.1) to 1. The invention realizes that high-purity light liquid wax and heavy liquid wax are obtained and simultaneously high-purity isoalkane, normal heptane and normal hexane are obtained.
Description
Technical Field
The invention relates to the field of fine chemicals, in particular to separation and refining of various alkanes.
Background
In order to ensure the petroleum safety of China, maintain the healthy development of economy and break the situation of petroleum shortage faced by China, the coal-to-liquid technology has become a very important national strategy in China. The coal indirect liquefaction method (F-T synthesis) is one of effective ways for supplementing domestic petroleum supply and efficiently utilizing coal.
In the environment of oil shortage, coal indirect liquefaction is greatly developed due to the characteristic that the coal indirect liquefaction can produce alternative liquid fuel, however, the coal indirect liquefaction cannot be limited to synthetic oil products only and is limited by the petroleum market. Coal-to-oil system is almost impossible to make profit when the price of oil drops below $ 60/barrel under the condition that the price of coal is 400 yuan/ton. If the structure diversification of the indirect coal liquefaction product can be realized, namely various special chemicals are produced by adopting the indirect coal liquefaction process, the improvement of the economic benefit of the indirect coal liquefaction process is undoubtedly very significant.
In order to improve the added value of products and increase the economic benefit of enterprises, the Sasol company in south africa adds a catalytic cracking device and a synthesis device of higher alcohols, olefins, acrylamide, acrylic ester, ethylene oxide and the like at the rear end of the products to produce fine chemicals. The ratio of oil product yield to chemical product yield is about 3: 2. In 2013, the chemical yield of the Sasol company accounts for 40% of the total yield, and the profit accounts for 70% of the total profit of the company, wherein the profit accounts for more than 200 billion yuan.
The normal paraffin in the F-T synthetic oil phase product has considerable occupation ratio, and the normal paraffin-liquid paraffin can be widely applied to the production of surfactants, synthetic detergents, synthetic feed proteins and the like, and can also be rapidly applied to the petrochemical industry and the microbial industry. In addition, n-alkanes are also common solvents for n-alkenes, and therefore, the separation of n-alkanes from the F-T synthetic oil product phase is an effective way to achieve its high value utilization. Meanwhile, the content of isoparaffin in the F-T synthetic oil phase product is very low and is far lower than that of normal paraffin, so that when the normal paraffin is recovered, the recovery and utilization of the isoparaffin are neglected in the production process in practice, and the application value of the isoparaffin is well known.
The Shenhua group is explored on the aspect of preparing light liquid paraffin by coal indirect liquefaction, and CN106675649A (published in 5.17.2017) discloses a method for preparing light liquid paraffin by coal indirect liquefaction, which specifically adopts a hydrogenation process flow, normal pressure fractionation and molecular sieve dewaxing, and the target product is light liquid paraffin. The molecular sieve dewaxing process sequentially comprises an adsorption process and a desorption process, wherein the adsorption conditions are as follows: the temperature of a bed layer is 280-350 ℃, the adsorption pressure is 0-1.0 MPa, the mass ratio of the screened oil is 8-20, and the adsorption airspeed is 0.2-0.6 h-1(ii) a Then desorbing by using a desorption agent under the following desorption conditions: the desorption temperature is 360-380 ℃, and the desorption airspeed is 0.2-0.6 h-1. It can be seen that the process is only targeted to obtain normal paraffins.
Shenhua group CN108102694A (published 6.1.2018) discloses a reprocessing system and method of Fischer-Tropsch synthesis diesel fraction, which can obtain a mixture of C10-C14 normal paraffins and a mixture of C10-C14 isoparaffins through different fractionating towers. However, the process has not performed effective cutting separation on the normal paraffin mixture and isoparaffin mixture to obtain single high-purity normal paraffin or isoparaffin, and the economic benefit is far from sufficient.
The Fischer-Tropsch synthesis product typically contains small amounts of naphthenes, for example less than 10% of naphthenes containing from 9 to 20 carbon atoms in the Fischer-Tropsch synthesis oil disclosed in CN 105505347A; CN106255740A discloses a Fischer-Tropsch derived gasoil containing in the range of 0-2 wt% naphthenes.
The inner Mongolia Guyitai group is used as one of leading enterprises in the coal indirect liquefaction oil production industry in China, F-T synthetic oil products are diversified, diversified and high-purity special chemical products are produced to realize industrialization, and light liquid wax, heavy liquid wax, n-dodecane, n-decane, n-heptane, n-hexane and a series of isoparaffins are prepared through synchronous co-production, so that 50 ten thousand tons of isoparaffins are produced annually.
Technical scheme
The invention aims to solve the technical problems of realizing and optimizing diversification of F-T synthetic oil products, producing diversified and high-purity special chemical products, realizing industrialization and synchronously co-producing and preparing various fine chemical products.
The technical scheme of the invention is as follows:
an industrial co-production method for synchronously preparing light liquid wax, heavy liquid wax, n-dodecane, n-decane, n-heptane, n-hexane and a series of isoparaffins is characterized in that the adopted raw materials are normal stable light hydrocarbons, a coal indirect liquefied first Fischer-Tropsch product and a coal indirect liquefied second Fischer-Tropsch product which are blended according to a certain proportion, so that the weight ratio of the normal paraffins to the isoparaffins is (0.8-1.1) to 1, and no cycloparaffins are contained. The specific process steps are as follows: (1) the blended mixed hydrocarbon is divided into three feed liquids after light component removal and heavy component removal treatment, and the three feed liquids respectively enter a light component fractionating tower, a first light white oil separation tower, an adsorption tower and a second light white oil separation tower; (2) the feed liquid entering the light component fractionating tower passes through a first separation tower, a second separation tower and a third separation tower in sequence to respectively obtain normal hexane and normal heptane; (3) separating the feed liquid entering a first light white oil separation tower and a second light white oil separation tower to obtain light white oil; (4) the feed liquid enters an adsorption tower, and the overhead distillate components enter a first isoparaffin separation tower, a second isoparaffin separation tower and an isoparaffin side stripper to respectively obtain four kinds of high-purity isoparaffins with different flash points; and (3) enabling the distillate components at the bottom of the tower to enter a re-distillation tower and a coarse distillation tower to respectively obtain light liquid wax containing carbon 11, carbon 10-11, carbon 12 and carbon 10-13 and heavy liquid wax containing carbon 14-15.
Further, the adsorption tower is a fixed bed reactor filled with a 5A molecular sieve, and the fixed bed reactor adopts a simulated moving bed process to selectively adsorb the feed liquid.
Further, the feedstock may be free of normal stable light hydrocarbons.
Further, the first light white oil separation tower receives the overhead distillate of the raw material passing through the light component removal tower, and the second light white oil separation tower receives the bottom distillate of the raw material passing through the light component removal tower and the heavy component removal tower.
Further, the top pressure of the first light white oil separation tower is 0.02-0.04MPa, the temperature of the top of the tower is 150-; the top pressure of the second light white oil separation tower is 8-15KPa, the temperature at the top of the tower is 190-20 KPa, the pressure at the bottom of the tower is 15-20KPa, and the temperature at the bottom of the tower is 250-258 ℃.
Further, the top pressure of the first light white oil separation tower is 0.03MPa, the temperature at the top of the tower is 156 ℃, the pressure at the bottom of the tower is 0.05-0.07MPa, and the temperature at the bottom of the tower is 180-; the top pressure of the second light white oil separation tower is 11KPa, the temperature of the tower top is 192 ℃, the pressure of the tower bottom is 16KPa, and the temperature of the tower bottom is 255 ℃.
Further, the content of the normal paraffin in the first Fischer-Tropsch product of coal indirect liquefaction is more than 90 percent, wherein the normal paraffin of C9-C18 accounts for more than 96 percent of the total mass of the normal paraffin.
Further, the content of isoparaffin in the second Fischer-Tropsch product of coal indirect liquefaction is more than 85%, wherein the isoparaffin of C9-C20 accounts for more than 96% of the total mass of the isoparaffin.
Further, the series of isoparaffins each have a purity of greater than 96%.
Further, the flash points of the series of isoparaffins are respectively more than 45 ℃, more than 61 ℃, more than 80 ℃ and more than 95 ℃.
The beneficial technical effects obtained by the invention are as follows:
(1) the composition condition of the raw materials directly determines the purity of the product, two or three raw materials are preferably selected for blending, and the normal paraffin and isoparaffin (0.8-1.1) to 1 ratio are preferably selected, so that the light liquid wax and the heavy liquid wax with high purity can be obtained, and simultaneously, the series of isoparaffins with high purity can be obtained.
(2) The optimal technological parameters for separating high-purity isoparaffin are selected. The selection of separation parameters in commercial practice is very difficult, especially for large industrial production of 50 ten thousand tons/year, and the confirmation of the cutting parameters of high purity isoparaffin is directly related to the success or failure and the benefit of the production.
(3) The project obtains good economic benefit in actual operation, meanwhile, the whole process realizes cleanness and environmental protection, is really a re-upgrade of coal clean utilization technology, and provides a good scheme for improving the added value of products of the national indirect coal liquefaction process.
Drawings
FIG. 1 is a flow chart of industrial co-production of light liquid wax, heavy liquid wax, n-dodecane, n-decane, n-heptane, n-hexane and series of isoparaffins prepared synchronously
Detailed Description
The technical solution and effects of the present invention will be further described below by way of specific embodiments.
As shown in the attached figure 1, the raw materials are pretreated, wherein the pretreatment process comprises light component removal in a light component removal tower and heavy component removal in a heavy component removal tower, the pressure at the top of the light component removal tower is 0.01-0.05MPa, the pressure at the bottom of the light component removal tower is 0.02-0.06MPa, the temperature at the top of the light component removal tower is 155-; the tower top pressure of the heavy component removal tower is 9-13KPa, the tower bottom pressure is 15-25KPa, the tower top temperature is 110-130 ℃, and the tower bottom temperature is 220-250 ℃. The raw material passing through the light component removal tower enters a light component fractionating tower and a first light white oil separation tower, and the raw material after light component removal and heavy component removal enters a molecular sieve adsorption separation device. Refined naphtha is synchronously introduced into a light component fractionating tower, the tower top pressure of the light component fractionating tower is 195-minus-one 205kPaA, and the temperature is 65-70 ℃. The top gas is condensed and cooled to 40 ℃ by a condenser at the top of the light component fractionating tower and enters a reflux tank of the light component fractionating tower, the top pressure of the tower is controlled by adopting nitrogen seal at the top of the tank, part of oil at the bottom of the tank is pumped into the top of the light component fractionating tower by a pump to be used as reflux, and part of oil is taken as stable light hydrocarbon to be discharged out of the device. And the light component fractionating tower is pressurized by a tower bottom pump and then enters the normal hexane tower. The top pressure of the n-hexane column was 120kPaA at 74.5 ℃. The n-hexane tower bottom oil is pressurized by a n-hexane tower bottom pump, passes through a carbon-seven fractionating tower feeding heat exchanger to exchange heat with the tower bottom oil to 134 ℃, and then enters a carbon-seven fractionating tower. The column top pressure of the n-heptane column was 125kPaA and the temperature was 104.2 ℃. The overhead gas is condensed and cooled to 60 ℃ by an air cooler (AC-302) at the top of the normal heptane tower, and enters a reflux tank of the normal heptane tower, and the pressure of the tower top is controlled by adopting nitrogen seal at the top of the reflux tank. The n-heptane tower bottom oil is pressurized by an n-heptane tower bottom pump, then cooled to 40 ℃ by an n-heptane tower feeding heat exchanger and an n-heptane cooler, and then pressed to a tank area.
After the raw materials enter a light component removal tower, the distillate at the top of the tower enters a first light white oil separation tower; and (3) feeding the bottom distillate of the light and heavy removal treated raw materials into a second light white oil separation tower, and separating the feed liquid of the first light white oil separation tower and the second light white oil separation tower to obtain light white oil. The top pressure of the first light white oil separation tower is 0.02-0.04MPa, the temperature of the tower top is 150-160 ℃, the pressure of the tower bottom is 0.05-0.07MPa, and the temperature of the tower bottom is 180-185 ℃; the top pressure of the second light white oil separation tower is 8-15KPa, the temperature at the top of the tower is 190-20 KPa, the pressure at the bottom of the tower is 15-20KPa, and the temperature at the bottom of the tower is 250-258 ℃. The top pressure of the first light white oil separation tower is 0.03MPa, the temperature of the tower top is 156 ℃, the pressure of the tower bottom is 0.05-0.07MPa, and the temperature of the tower bottom is 180-; the top pressure of the second light white oil separation tower is 11KPa, the temperature of the tower top is 192 ℃, the pressure of the tower bottom is 16KPa, and the temperature of the tower bottom is 255 ℃.
The distillate at the top of the tower after the light and heavy removal treatment of the raw material enters a molecular sieve adsorption tower, and in the molecular sieve adsorption process, the feeding temperature of a molecular sieve material is 176-.
Introducing the isoparaffin raffinate after molecular sieve adsorption into a first isoparaffin separation tower, wherein the top pressure of the first isoparaffin separation tower is 0.08-0.11MPa, the bottom pressure of the first isoparaffin separation tower is 0.12-0.15MPa, the top temperature is 198-290 ℃ and the bottom temperature is 270-290 ℃. The isoparaffin product with the flash point of more than 45 ℃ is distilled from the top of the first isoparaffin separation tower, the material flows are extracted from the middle upper part of the 5 th layer, the 9 th layer and the 15 th layer of the side tray of the first isoparaffin separation tower and enter a isoparaffin side stripping tower, the stripping steam at the top of the tower returns to the isoparaffin separation tower, and the isoparaffin product with the flash point of more than 61 ℃ is obtained from the bottom of the stripping tower. The top pressure of the isoparaffin side stripper is 0.09-0.12MPa, the bottom pressure is 0.10-0.13MPa, the top temperature is 200-220 ℃, and the bottom temperature is 205-225 ℃. The tower kettle discharge of the first isoparaffin separation tower is conveyed to a second isoparaffin separation tower, the top of the second isoparaffin separation tower distills off isoparaffin products with flash point more than 80 ℃, and the tower kettle discharge is isoparaffin products with flash point more than 95 ℃. The top pressure of the second isoparaffin separation column is 8-13KPa, the bottom pressure is 14-19KPa, the top temperature is 135-150 ℃, and the bottom temperature is 180-195 ℃. The purity of each isoparaffin is more than 96%.
The n-alkane extract after molecular sieve adsorption enters an n-alkane redistillation tower, the n-alkane (C10-12) in the light wax redistillation tower is distilled out from the tower top, and the n-alkane extract enters a light wax redistillation tower reflux tank after sequentially passing through a raffinate-light wax redistillation tower top heat exchanger and a light wax redistillation tower top working air cooler for condensation and cooling. The light wax redistillation tower reflux pump pumps out normal paraffin (C10-12) from the reflux tank, the outlet is divided into two paths, one path is pumped back to the top of the tower to be used as top reflux, and the other path is fed to the normal decane tower through the cascade control regulating valve of the liquid level and the flow of the tank. And (3) pressurizing the discharged material at the tower bottom by a light wax re-distillation tower bottom pump, then exchanging heat by a light wax-light wax re-distillation tower bottom oil heat exchanger, feeding the material to an n-dodecane tower, distilling the n-decane in the n-decane tower from the tower top, and distilling the n-dodecane in the n-dodecane tower from the tower top.
The first Fischer-Tropsch product of the indirect coal liquefaction does not contain naphthenes and can comprise 5-15% of C5-C9 normal paraffins, 0.1-0.5% of C5-C9 isoparaffins, 35-60% of C10-C13 normal paraffins, 1-5% of C10-C13 isoparaffins, 15-40% of C14-C16 normal paraffins, 1-5% of C14-C16 isoparaffins, 5-20% of C17+ normal paraffins and 1-5% of C17+ isoparaffins. It can also comprise 7-16% of C5-C9 normal paraffin, 0.1-0.6% of C5-C9 isoparaffin, 40-60% of C10-C13 normal paraffin, 1-4% of C10-C13 isoparaffin, 20-30% of C14-C16 normal paraffin, 0.5-3% of C14-C16 isoparaffin, 8-15% of C17+ normal paraffin and 0.8-2% of C17+ isoparaffin.
The second Fischer-Tropsch product of indirect coal liquefaction contains no naphthenes and can comprise 0.5-2.5% of C5-C9 normal paraffins, 1-5% of C5-C9 isoparaffins, 3-10% of C10-C13 normal paraffins, 40-60% of C10-C13 isoparaffins, 1-5% of C14-C16 normal paraffins, 15-25% of C14-C16 isoparaffins, 3-6% of C17+ normal paraffins and 8-15% of C17+ isoparaffins. It can also comprise 0.2-0.8% of C5-C9 normal paraffin, 0.3-1% of C5-C9 isoalkane, 2-10% of C10-C13 normal paraffin, 40-55% of C10-C13 isoalkane, 2-4% of C14-C16 normal paraffin, 20-30% of C14-C16 isoalkane, 2-5% of C17+ normal paraffin and 9-13% of C17+ isoalkane.
The molecular sieve adsorption efficiency can be improved and the purity and yield of isoparaffin products can be improved by controlling the proportion of the normal paraffin to the isoparaffin within the range of (0.8-1.1) to 1.
In addition to controlling the ratio of normal paraffins to isoparaffins, the ratio of the volume of molecular sieve cavities to the volume of normal paraffins in the feedstock during adsorption of the molecular sieve is preferably 1.15 to 1.55 to improve the isoparaffin product purity.
In the raw materials, the content of aromatic hydrocarbon is controlled to be less than or equal to 20ppm, the content of oxygen is controlled to be less than or equal to 1ppm, the content of water is controlled to be less than or equal to 40ppm, the content of nitrogen is controlled to be less than or equal to 0.3ppm, the content of sulfur is controlled to be less than or equal to 1ppm, the content of chlorine is controlled to be less than or equal to 5ppm, the bromine index is controlled.
Claims (10)
1. An industrial co-production method for synchronously preparing light liquid wax, heavy liquid wax, n-dodecane, n-decane, n-heptane, n-hexane and a series of isoparaffins is characterized in that the adopted raw materials are normal stable light hydrocarbons, a coal indirect liquefied first Fischer-Tropsch product and a coal indirect liquefied second Fischer-Tropsch product are blended according to a certain proportion, the weight ratio of the normal paraffins to the isoparaffins is (0.8-1.1):1, the coal indirect liquefied first Fischer-Tropsch product and the coal indirect liquefied second Fischer-Tropsch product do not contain naphthenes, and the specific process steps are as follows: (1) the blended mixed hydrocarbon is subjected to lightness removal by a lightness removal tower, and then respectively enters a light component separation distillation tower, a first light white oil separation tower and a weight removal tower, the distillate at the top of the weight removal tower enters an adsorption tower, and the distillate at the bottom of the weight removal tower enters a second light white oil separation tower; (2) the feed liquid entering the light component fractionating tower passes through a first separation tower, a second separation tower and a third separation tower in sequence to respectively obtain normal hexane and normal heptane; (3) separating the feed liquid entering a first light white oil separation tower and a second light white oil separation tower to obtain light white oil; (4) the feed liquid enters an adsorption tower, and the overhead distillate components enter a first isoparaffin separation tower, a second isoparaffin separation tower and an isoparaffin side stripper to respectively obtain four kinds of high-purity isoparaffins with different flash points; and (3) enabling the distillate components at the bottom of the tower to enter a re-distillation tower and a coarse distillation tower to respectively obtain light liquid wax containing carbon 11, carbon 10-11, carbon 12 and carbon 10-13 and heavy liquid wax containing carbon 14-15.
2. The industrial co-production method according to claim 1, wherein the adsorption tower is a fixed bed reactor filled with a 5A molecular sieve, the ratio of the cavity volume of the molecular sieve to the volume of normal paraffin in the raw material in the adsorption process of the molecular sieve is 1.15-1.55, and the fixed bed reactor adopts a simulated moving bed process to perform selective adsorption on the feed liquid.
3. Industrial co-production process according to claim 2, characterized in that the feedstock is free of normal stable light hydrocarbons.
4. Industrial co-production process according to one of claims 1 to 3, characterized in that the first light white oil separation column receives the overhead of the feedstock passing through a light ends removal column and the second light white oil separation column receives the bottoms of the feedstock passing through a light ends removal column and a heavy ends removal column.
5. The industrial co-production process as claimed in any one of claims 1 to 3, wherein the top pressure of the first light white oil separation column is 0.02 to 0.04MPa, the top temperature is 150-160 ℃, the bottom pressure is 0.05 to 0.07MPa, and the bottom temperature is 180-185 ℃; the top pressure of the second light white oil separation tower is 8-15KPa, the temperature at the top of the tower is 190-20 KPa, the pressure at the bottom of the tower is 15-20KPa, and the temperature at the bottom of the tower is 250-258 ℃.
6. The industrial co-production process as claimed in claim 5, wherein the top pressure of the first light white oil separation column is 0.03MPa, the top temperature is 156 ℃, the bottom pressure is 0.05-0.07MPa, and the bottom temperature is 180-185 ℃; the top pressure of the second light white oil separation tower is 11KPa, the temperature of the tower top is 192 ℃, the pressure of the tower bottom is 16KPa, and the temperature of the tower bottom is 255 ℃.
7. The industrial co-production process of any one of claims 1-3 and 6, wherein the coal indirect liquefaction first Fischer-Tropsch product has an n-alkane content of greater than 90%, wherein the n-alkanes from C9 to C18 account for more than 96% of the total mass of the n-alkanes.
8. The industrial co-production process of any one of claims 1-3 and 6, wherein the content of isoparaffin in the coal indirect liquefaction second Fischer-Tropsch product is more than 85%, wherein the content of isoparaffin of C9-C20 accounts for more than 96% of the total mass of isoparaffin in the coal indirect liquefaction second Fischer-Tropsch product.
9. Industrial co-production process according to one of claims 1-3, 6, characterized in that the series of isoparaffins each have a purity of more than 96%.
10. Industrial co-production process according to one of claims 1-3, 6, characterized in that the series of isoparaffins have a flash point of more than 45 ℃, more than 61 ℃, more than 80 ℃ and more than 95 ℃ respectively.
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| CN114797523A (en) * | 2022-04-25 | 2022-07-29 | 内蒙古伊泰宁能精细化工有限公司 | Method for uniformly mixing n-isoparaffin in raw material |
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