CN113845938A - Method for producing food-grade white oil from Fischer-Tropsch oil - Google Patents
Method for producing food-grade white oil from Fischer-Tropsch oil Download PDFInfo
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- CN113845938A CN113845938A CN202111320977.8A CN202111320977A CN113845938A CN 113845938 A CN113845938 A CN 113845938A CN 202111320977 A CN202111320977 A CN 202111320977A CN 113845938 A CN113845938 A CN 113845938A
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 26
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 104
- 239000003054 catalyst Substances 0.000 claims abstract description 69
- 239000000463 material Substances 0.000 claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 32
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 25
- 239000001257 hydrogen Substances 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 22
- 230000008569 process Effects 0.000 claims abstract description 21
- 238000000926 separation method Methods 0.000 claims abstract description 16
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 239000012071 phase Substances 0.000 claims abstract description 14
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 14
- 239000007791 liquid phase Substances 0.000 claims abstract description 11
- 239000003921 oil Substances 0.000 claims description 148
- 239000012752 auxiliary agent Substances 0.000 claims description 29
- 229910052751 metal Inorganic materials 0.000 claims description 27
- 239000002184 metal Substances 0.000 claims description 27
- 238000002156 mixing Methods 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 19
- 229910000510 noble metal Inorganic materials 0.000 claims description 19
- 238000002791 soaking Methods 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 11
- 238000010992 reflux Methods 0.000 claims description 10
- 229910052759 nickel Inorganic materials 0.000 claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 8
- 229910052796 boron Inorganic materials 0.000 claims description 8
- 229910052697 platinum Inorganic materials 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000005336 cracking Methods 0.000 claims description 5
- 239000002808 molecular sieve Substances 0.000 claims description 5
- 229910052763 palladium Inorganic materials 0.000 claims description 5
- 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 5
- 229910052721 tungsten Inorganic materials 0.000 claims description 5
- 229910052726 zirconium Inorganic materials 0.000 claims description 5
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 239000011959 amorphous silica alumina Substances 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 150000002739 metals Chemical class 0.000 claims description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims description 3
- 229910052703 rhodium Inorganic materials 0.000 claims description 3
- 229910052707 ruthenium Inorganic materials 0.000 claims description 3
- 239000012266 salt solution Substances 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 239000000047 product Substances 0.000 description 24
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 14
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 14
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 10
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 6
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 5
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 5
- 239000004327 boric acid Substances 0.000 description 5
- 239000002199 base oil Substances 0.000 description 4
- 238000004517 catalytic hydrocracking Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000003208 petroleum Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 239000010687 lubricating oil Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 2
- NWAHZABTSDUXMJ-UHFFFAOYSA-N platinum(2+);dinitrate Chemical compound [Pt+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O NWAHZABTSDUXMJ-UHFFFAOYSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- QDZRBIRIPNZRSG-UHFFFAOYSA-N titanium nitrate Chemical compound [O-][N+](=O)O[Ti](O[N+]([O-])=O)(O[N+]([O-])=O)O[N+]([O-])=O QDZRBIRIPNZRSG-UHFFFAOYSA-N 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical compound [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- FUECGUJHEQQIFK-UHFFFAOYSA-N [N+](=O)([O-])[O-].[W+4].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] Chemical compound [N+](=O)([O-])[O-].[W+4].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] FUECGUJHEQQIFK-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000010426 asphalt Substances 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
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 1
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000006392 deoxygenation reaction Methods 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000007327 hydrogenolysis reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- WFLYOQCSIHENTM-UHFFFAOYSA-N molybdenum(4+) tetranitrate Chemical compound [N+](=O)([O-])[O-].[Mo+4].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] WFLYOQCSIHENTM-UHFFFAOYSA-N 0.000 description 1
- MOWMLACGTDMJRV-UHFFFAOYSA-N nickel tungsten Chemical compound [Ni].[W] MOWMLACGTDMJRV-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Images
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
- 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
- C10G67/02—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only plural serial stages only
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/185—Phosphorus; Compounds thereof with iron group metals or platinum group metals
- B01J27/1853—Phosphorus; Compounds thereof with iron group metals or platinum group metals with iron, cobalt or nickel
-
- 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
- C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
- C10G2400/14—White oil, eating oil
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a method for producing food-grade white oil from Fischer-Tropsch oil, which comprises the following steps: the Fischer-Tropsch synthesis raw material firstly enters a hydrogenation unit, and a one-stage hydrogenation reaction is carried out in the presence of hydrogen and a hydrogenation catalyst; the hydrogenation product is subjected to gas-liquid separation by a high-temperature high-pressure separator, the first gas-phase material flow obtained by separation is circularly returned to the hydrogenation unit, the first liquid-phase material flow enters a low-pressure hot separator for continuous gas-liquid separation, the second gas-phase material flow obtained by separation is circularly returned to the hydrogenation unit, and the second liquid-phase material flow enters a fractionating tower for separating food-grade white oil products of different brands. The method for producing the food-grade white oil from the Fischer-Tropsch oil has the advantages of stronger adaptability, mild reaction conditions, simple and convenient process flow and lower production cost.
Description
Technical Field
The invention relates to the technical field of food-grade white oil production, in particular to a method for producing food-grade white oil from Fischer-Tropsch synthetic oil.
Background
The food-grade white oil has excellent photo-thermal stability, yellowing resistance, oxidation resistance and viscosity-temperature performance, and is safe and nontoxic to human bodies. Food-grade white oil products become important raw materials in the industries of food processing, medicine, daily chemicals, chemical fiber and the like. In recent years, the living standard of people is continuously improved, the quality requirement of people on white oil is higher and higher, and the demand of food-grade white oil is rapidly increased.
The hydrogenation method is a main process for producing food-grade white oil internationally at present, and the main principle is that a high-pressure hydrogenation process is adopted, under the conditions of a certain temperature and higher hydrogen partial pressure, non-hydrocarbon compounds such as sulfur, nitrogen, oxygen and the like in raw oil are subjected to hydrogenolysis, olefin and aromatic hydrocarbon are subjected to selective hydrogenation saturation, and impurities such as metal, asphalt colloid and the like can be removed. The main reactions in the hydrogenation process are desulfurization, denitrification, deoxygenation, saturation of olefins and aromatics, and hydrodemetallization.
The key indexes (carbon-prone compounds, ultraviolet absorbance and the like) of the food-grade white oil must meet the standard requirements of the national GB 1886.215-2016 on the food-grade white oil. With the continuous improvement of the high-grade white oil standard, the requirements on the production process are more and more strict. The requirements of the food-grade white oil on the content of aromatic hydrocarbon are extremely strict, and the hydrogenation of the aromatic hydrocarbon is difficult to be carried out at high temperature due to the limitation of thermodynamic balance, so that the food-grade white oil produced by a hydrogenation method adopts a high-pressure and low-temperature hydrogenation process. According to different raw materials, one-stage or multi-stage hydrogenation is adopted, and food-grade white oil can be obtained by one-stage hydrogenation on raw materials with better quality, such as hydrocracking tail oil or acid refined lubricating oil base oil, wherein the content of aromatic hydrocarbon is generally lower than 5%. The method is characterized in that common raw materials such as lubricating oil base oil or solvent refining dewaxing oil with the aromatic hydrocarbon content of 10-20 percent are subjected to two-stage hydrogenation, industrial-grade white oil can be obtained through one-stage hydrogenation, and food-grade white oil can be obtained through two-stage hydrogenation. If the raw material is worse, such as vacuum distillate, more than three stages of hydrogenation are needed.
Patent document US4072603 discloses a method for producing industrial white oil by one-stage hydrogenation, in which dewaxed hydrocracking tail oil is used as a raw material, and tungsten-nickel loaded on a silicon-aluminum carrier is used as a hydrogenation catalyst to produce industrial white oil.
Patent document CN1510110A discloses a method for producing high-viscosity food-grade white oil by using a one-stage hydrogenation method, and light or heavy food-grade white oil is produced by using non-noble metal or noble metal catalyst. The process conditions comprise that the hydrogen partial pressure is 8.0-20.0 MPa, the reaction temperature is 150-300 ℃, and the volume ratio of hydrogen to oil is 100: 1-1500: 1. the volume space velocity is 0.1-1.5 h-1. The method requires high hydrogen partial pressure and high equipment investment cost.
Patent document CN101148606A discloses a method for producing food-grade white oil by one-stage hydrogenation, which uses vacuum distillate oil, solvent refined deasphalted oil and the like as raw materials, and adopts a single-stage hydrogenation process, wherein the process conditions are that the hydrogen partial pressure is 8.0-18.0 MPa, the reaction temperature is 290-430 ℃, and the hydrogen-oil volume ratio is 300: 1-2500: 1. the volume space velocity is 0.4-10.0 h-1. Although the method is a one-stage method for producing the food-grade white oil, the hydrogen partial pressure and the reaction temperature are high, and the process conditions are harsh.
Patent document CN101265419A discloses a method for producing food-grade white oil by one-stage medium-pressure hydrogenation, which uses refined lubricant base oil or industrial white oil as raw material, and adopts non-noble metal catalyst system to produce food-grade white oil. The process conditions comprise that the hydrogen partial pressure is 4.0-10.0 MPa, the reaction temperature is 180-320 ℃, and the volume ratio of hydrogen to oil is 200: 1-1000: 1. the volume space velocity is 0.1-1.0 h-1. The catalyst used in the method of the patent is only limited to nickel supported catalysts in which nickel metal salts are supported on alumina, spinel or zeolite materials.
Patent document CN111518589A discloses a production process of food-grade white oil, which uses lubricant base oil, industrial white oil, hydrocracking tail oil, hydroisomerization dewaxing tail oil, etc. as raw material oil, and uses noble metal catalyst to perform one-stage series hydrogenation to obtain reaction product, wherein the process conditions are that hydrogen partial pressure is 12.0-20.0 MPa, reaction temperature is 180-320 ℃, and hydrogen-oil volume ratio is 300: 1-1000: 1. the volume space velocity is 0.3-1.5 h-1. The method uses petroleum-based oil as raw material and adopts precious goldBelongs to a catalyst, and the reaction condition is harsh.
The existing method for producing food-grade white oil by one-stage hydrogenation takes petroleum as a raw material, and has the problems of harsh reaction conditions, high production cost and the like.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide the method for producing the food-grade white oil from the Fischer-Tropsch oil, which has the advantages of stronger adaptability, mild reaction conditions, simple and convenient process flow and low production cost.
The technical scheme provided by the invention is as follows:
a method for producing food-grade white oil from Fischer-Tropsch oil comprises the following steps:
the Fischer-Tropsch synthesis raw material firstly enters a hydrogenation unit, and a one-stage hydrogenation reaction is carried out in the presence of hydrogen and a hydrogenation catalyst; and (4) separating the hydrogenation product into gas and liquid, and then feeding the hydrogenation product into a fractionating tower to separate food-grade white oil products with different brands.
Preferably, the hydrogenation product is first subjected to gas-liquid separation by a high-temperature high-pressure separator, the first gas-phase material flow obtained by separation is recycled to the hydrogenation unit, the first liquid-phase material flow enters a low-pressure hot separator for continuous gas-liquid separation, the second gas-phase material flow obtained by separation is recycled to the hydrogenation unit, and the second liquid-phase material flow enters a fractionating tower.
Preferably, the Fischer-Tropsch synthesis raw material is tail oil obtained from the bottom of a fractionating tower after the Fischer-Tropsch synthesis oil is subjected to hydroisomerization cracking, the carbon number is more than or equal to C11+, the distillation range is as follows: 200-690 ℃ and the content of isoparaffin is more than or equal to 70 percent.
Preferably, in the one-stage hydrogenation reaction, the reaction temperature is controlled to be 120-220 ℃, the reaction pressure is 3.0-10.0 MPa, and the volume ratio of hydrogen to oil is 200-1000: 1, the feeding volume airspeed is 0.1-3.0 h-1。
Preferably, the hydrogenation catalyst is a supported metal catalyst, and the active metal in the supported metal catalyst is a noble metal and/or a non-noble metal.
Further, the noble metal is any one or a combination of two of Pt, Pd, Ru and Rh, and the non-noble metal is any one or a combination of two of Ni, W, Co and Mo.
Further, the total mass percentage of active metals in the hydrogenation catalyst is 1-60%.
Further, the carrier of the hydrogenation catalyst is any one of alumina, silicon dioxide, a molecular sieve and amorphous silica-alumina which are modified by an auxiliary agent.
Further, the auxiliary agent contains any one of P, B, Ti and Zr.
Furthermore, the auxiliary agent element accounts for 0.1-10% of the mass fraction of the carrier.
Further, the production method of the hydrogenation catalyst is as follows,
s1, mixing the auxiliary agent and the carrier, soaking for 4-48 hours, drying for 3-12 hours at 100-120 ℃, and then roasting for 2-12 hours at 350-600 ℃ to obtain the carrier containing the auxiliary agent;
s2, mixing and soaking the metal salt solution and the carrier containing the auxiliary agent for 12-48 h, drying at 100-120 ℃ for 3-12 h, and then roasting at 350-650 ℃ for 2-12 h to obtain the metal-based catalyst.
Preferably, the number of theoretical plates of the fractionating tower is 15-60, the feeding position is 5-55 feeding, the reflux ratio is 0.5-10, the operation pressure at the top of the tower is 2-10 kPa, the operation temperature is 150-250 ℃, and the temperature of the bottom of the tower is 300-450 ℃.
The invention has the beneficial effects that:
the invention takes Fischer-Tropsch synthesis hydrogenation isomerization cracking tail oil as raw material, adopts noble metal or non-noble metal hydrogenation catalyst, and adopts a one-section hydrogenation deep dearomatization process to produce food-grade white oil under mild conditions. Compared with the existing method for producing the food-grade white oil by petroleum base, the method has the advantages of easily available raw materials, wide catalyst adaptability, simple process flow, mild hydrogenation reaction conditions and low production cost.
Drawings
FIG. 1 is a schematic flow diagram of the Fischer-Tropsch oil production process of food grade white oil.
The notations in the figures have the following meanings:
r-a hydrogenation reactor; v1-hot high-pressure separator; v2-hot low pressure separator; a T-fractionating tower.
1-fischer-tropsch synthesis of a hydroisomerized cracked tail oil stream; 2-a hydrogen stream; 3-a hydrogenation product stream; 4-a first vapor stream; 5-a first liquid phase stream; 6-a second gas phase stream; 7-a second liquid phase stream; 8-a gas phase stream; food grade No. 9-first white oil product; 10-second food grade white oil product; 11-third food-grade white oil product.
Detailed Description
The technical solution of the present invention will be clearly and completely described below with reference to the specific embodiments. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
According to an embodiment provided by the invention, shown in fig. 1, the method for producing food-grade white oil from fischer-tropsch oil comprises the following steps:
the Fischer-Tropsch synthesis raw material firstly enters a hydrogenation unit, and a one-stage hydrogenation reaction is carried out in the presence of hydrogen and a hydrogenation catalyst; and (4) separating the hydrogenation product into gas and liquid, and then feeding the hydrogenation product into a fractionating tower T to separate food-grade white oil products with different brands.
According to the embodiment, the Fischer-Tropsch synthetic oil is used as the raw material, after hydrogenation is carried out by a one-stage method, gas-liquid separation is carried out on the hydrogenation product, the separated liquid substance enters the fractionating tower T, and then the multi-level food-grade white oil product can be separated.
Preferably, the hydrogenation product is first subjected to gas-liquid separation by a hot high-pressure separator V1, the separated first gas phase material flow 4 is recycled to the hydrogenation unit, the first liquid phase material flow 5 is then introduced into a hot low-pressure separator V2 to be subjected to gas-liquid separation, the separated second gas phase material flow 6 and the first gas phase material flow 4 together form a gas phase material flow 8, the gas phase material flow is recycled to the hydrogenation unit, and the second liquid phase material flow 7 is introduced into the fractionating tower T.
In order to obtain more excellent reaction effect:
the Fischer-Tropsch synthesis raw material is tail oil obtained from the bottom of a fractionating tower after the Fischer-Tropsch synthesis oil is subjected to hydroisomerization cracking, the carbon number is more than or equal to C11+, the distillation range is as follows: 200-690 ℃ and the content of isoparaffin is more than or equal to 70 percent.
Controlling the reaction temperature to be 120-220 ℃ in the one-stage hydrogenation reaction; the reaction pressure is 3.0-10.0 MPa; the volume ratio of hydrogen to the hydrogen oil of the Fischer-Tropsch synthesis raw material is 200-1000: 1; the feeding volume airspeed is 0.1-3.0 h-1。
In order to improve the hydrogenation catalytic effect of the catalyst, the hydrogenation catalyst adopts a supported metal catalyst, and the active metal in the supported metal catalyst is noble metal and/or non-noble metal. Non-noble metals are preferred.
Further, the noble metal is any one or a combination of two of Pt, Pd, Ru and Rh, and the non-noble metal is any one or a combination of two of Ni, W, Co and Mu. The total mass percentage of active metals in the hydrogenation catalyst is 1-60%.
Further, the carrier of the hydrogenation catalyst is any one of alumina, silicon dioxide, a molecular sieve and amorphous silica-alumina which are modified by an auxiliary agent.
Further, the auxiliary agent contains any one of P, B, Ti and Zr elements; b is preferred.
Furthermore, the auxiliary agent element accounts for 0.1-10% of the mass fraction of the catalyst carrier.
Based on the catalyst design, the aromatic hydrocarbon in the Fischer-Tropsch synthetic oil can be deeply hydrogenated and saturated by a one-stage hydrogenation deep dearomatization process under mild conditions to produce the food-grade white oil.
Wherein, the production method of the hydrogenation catalyst comprises the following steps,
s1, mixing the auxiliary agent and the carrier, soaking for 4-48 hours, drying for 3-12 hours at 100-120 ℃, and then roasting for 2-12 hours at 350-600 ℃ to obtain the carrier containing the auxiliary agent;
s2, mixing and dipping the salt solution of the active metal and the carrier containing the auxiliary agent for 12-48 h, drying at 100-120 ℃ for 3-12 h, and then roasting at 350-650 ℃ for 2-12 h to prepare the metal-based catalyst, namely the metal-based catalyst is used as a hydrogenation catalyst in hydrogenation reaction, and the aromatic hydrocarbon in the Fischer-Tropsch synthetic oil is subjected to deep hydrogenation saturation.
In a preferred embodiment, the number of theoretical plates of the fractionating tower T is 15-60, the feeding position is 5-55 feeding from the top, the reflux ratio is 0.5-10, the operation pressure at the top of the tower is 2-10 kPa, the operation temperature is 150-250 ℃, and the temperature at the bottom of the tower is 300-450 ℃. And a plurality of measuring lines are arranged on the fractionating tower T, and food-grade white oil products with different brands are extracted.
Example 1
Preparing a hydrogenation catalyst: mixing and soaking boric acid aqueous solution and amorphous silicon-aluminum according to the mass ratio of boron-containing mass to amorphous silicon-aluminum of 3.5:96.5 for 24 hours, drying at 100 ℃ for 4 hours, and roasting at 450 ℃ for 4 hours to obtain the catalyst carrier containing the assistant P. Mixing and soaking a nickel nitrate solution with a certain concentration and a carrier for 24 hours according to the mass ratio of nickel to carrier of 1:3, then drying for 6 hours at 120 ℃, and then roasting for 4 hours at 500 ℃ to obtain the metal hydrogenation catalyst with the assistant P element accounting for 3.5% of the mass fraction of the catalyst carrier and the total mass fraction of nickel accounting for 25%.
Producing food-grade white oil by using Fischer-Tropsch oil: loading a catalyst into a hydrogenation reactor R, mixing a Fischer-Tropsch synthesis hydroisomerization cracking tail oil material flow 1 and a hydrogen material flow 2 after reduction pretreatment, preheating, and then feeding the mixture into the hydrogenation reactor R, wherein the reaction temperature is 150 ℃, the pressure is 6.0MPa, the hydrogen-oil volume ratio is 800, and the volume space velocity is 0.6h-1Under the condition of (1), deep hydrofining is carried out to remove aromatic hydrocarbon; and after the hydrogenation product material flow 3 is subjected to gas-liquid separation by a hot high-pressure separator V1 and a hot low-pressure separator V2, a gas phase material flow 8 is circulated to a hydrogenation reactor R, a second liquid phase material flow 7 enters a fractionating tower T for cutting, under the conditions that the number of theoretical plates is 40, the reflux ratio is 4, the feeding position is 20 th, the operation requirement of the tower top is 5kPa, the temperature of the tower top is 180-200 ℃, and the temperature of a tower kettle is 350-400 ℃, a first food-grade white oil material flow 9, a second food-grade white oil material flow 10 and a third food-grade white oil material flow 11 are respectively obtained from different measuring lines, and the indexes of the food-grade white oil products are shown in Table 1.
Table 1 example 1 food grade white oil index
Example 2
This embodiment is substantially the same as embodiment 1 except that:
preparing a hydrogenation catalyst: mixing and soaking the boric acid aqueous solution and the molecular sieve for 24 hours according to the mass ratio of boron-containing mass to molecular sieve of 4.5:95.5, then drying for 4 hours at 100 ℃, and then roasting for 4 hours at 450 ℃ to obtain the catalyst carrier containing the auxiliary agent. Mixing and soaking a cobalt nitrate solution with a certain concentration and a carrier for 24 hours according to the mass ratio of cobalt to carrier of 7:13, then drying for 6 hours at 120 ℃, and then roasting for 4 hours at 500 ℃ to obtain the metal hydrogenation catalyst with the auxiliary agent P accounting for 4.5% of the mass fraction of the catalyst carrier and the total mass fraction of cobalt accounting for 35%.
Producing food-grade white oil: in a hydrogenation reactor, the reaction temperature is 180 ℃, the pressure is 8.0MPa, the volume ratio of hydrogen to oil is 800, and the volume space velocity is 0.5h-1Under the condition of (1), deep hydrofining is carried out to remove aromatic hydrocarbon; in the fractionating tower, under the conditions that the number of theoretical plates is 50, the reflux ratio is 4, the feeding position is 25, the operation requirement on the top of the tower is 5kPa, the temperature of the top of the tower is 180-200 ℃, and the temperature of a tower kettle is 350-400 ℃, a first food-grade white oil material flow, a second food-grade white oil material flow and a third food-grade white oil material flow are respectively obtained from different measuring lines, and the indexes of the food-grade white oil products are shown in table 2.
Table 2 example 2 food grade white oil index
Example 3
This embodiment is substantially the same as embodiment 1 except that:
preparing a hydrogenation catalyst: zirconium nitrate and alumina are mixed and impregnated for 24 hours according to the mass ratio of zirconium-containing mass to alumina being 6.5:93.5, then the mixture is dried for 4 hours at the temperature of 100 ℃, and then the mixture is roasted for 4 hours at the temperature of 450 ℃ to obtain the catalyst carrier containing the auxiliary agent. Mixing and soaking nickel nitrate and tungsten nitrate solution with certain concentration and a carrier for 24 hours according to the mass ratio of nickel and tungsten to the carrier of 7:2:11, then drying for 6 hours at 120 ℃, and roasting for 8 hours at 500 ℃ to obtain the metal hydrogenation catalyst with the auxiliary agent zirconium element accounting for 6.5% of the mass fraction of the catalyst carrier and the total mass fraction of nickel and tungsten accounting for 45%.
Producing food-grade white oil: in a hydrogenation reactor, the reaction temperature is 160 ℃, the pressure is 6.0MPa, the volume ratio of hydrogen to oil is 600, and the volume space velocity is 0.8h-1Under the condition of (1), deep hydrofining is carried out to remove aromatic hydrocarbon; in the fractionating tower, under the conditions that the number of theoretical plates is 60, the reflux ratio is 4, the feeding position is 30 th from the top, the operation requirement on the tower top is 5kPa, the temperature on the tower top is 180-200 ℃, and the temperature of a tower kettle is 350-400 ℃, a first food-grade white oil material flow, a second food-grade white oil material flow and a third food-grade white oil material flow are respectively obtained from different measuring lines, and the indexes of the food-grade white oil products are shown in table 3.
Table 3 example 3 food grade white oil index
Example 4
This embodiment is substantially the same as embodiment 1 except that:
preparing a hydrogenation catalyst: mixing titanium nitrate and alumina according to the mass ratio of titanium to alumina of 1:9, soaking for 24h, drying at 100 ℃ for 4h, and roasting at 450 ℃ for 4h to obtain the catalyst carrier containing the auxiliary agent. Mixing and soaking a palladium nitrate solution with a certain concentration and a carrier for 24 hours according to the mass ratio of palladium to carrier of 1:19, then drying for 6 hours at 120 ℃, and roasting for hours at 500 ℃ to obtain the hydrogenation catalyst with the auxiliary agent titanium element accounting for 10% of the mass fraction of the catalyst carrier and the total mass fraction of palladium accounting for 5%.
Producing food-grade white oil: in a hydrogenation reactor, the reaction temperature is 140 ℃, the pressure is 6.0MPa, the volume ratio of hydrogen to oil is 600, and the volume space velocity is 0.5h-1Under the condition of (1), deep hydrofining is carried out to remove aromatic hydrocarbon; in the fractionating column, the number of theoretical platesThe method comprises the steps of respectively obtaining a first food-grade white oil material flow, a second food-grade white oil material flow and a third food-grade white oil material flow from different measuring lines under the conditions that 30 blocks are adopted, the reflux ratio is 4, the feeding position is the 15 th block from the top, the tower top operation is 5kPa, the tower top temperature is 180-200 ℃, and the tower bottom temperature is 350-400 ℃, wherein the indexes of the food-grade white oil products are shown in Table 4.
Table 4 example 4 food grade white oil index
Example 5
This embodiment is substantially the same as embodiment 1 except that:
preparing a hydrogenation catalyst: mixing boric acid aqueous solution and amorphous silicon-aluminum according to the mass ratio of boron-containing mass to amorphous silicon-aluminum of 1:999, soaking for 24h, drying for 4h at 100 ℃, and roasting for 4h at 450 ℃ to obtain the catalyst carrier containing the auxiliary agent. Mixing a platinum nitrate solution with a certain concentration with a carrier according to the mass ratio of platinum to carrier of 1:99, soaking for 24h, drying for 6h at 120 ℃, and roasting for h at 500 ℃ to obtain the hydrogenation catalyst with the auxiliary agent P accounting for 0.1% of the mass fraction of the catalyst carrier and the total mass fraction of metal platinum accounting for 1%.
Producing food-grade white oil: in a hydrogenation reactor, the reaction temperature is 130 ℃, the pressure is 8.0MPa, the volume ratio of hydrogen to oil is 600, and the volume space velocity is 0.5h-1Under the condition of (1), deep hydrofining is carried out to remove aromatic hydrocarbon; in the fractionating tower, under the conditions that the number of theoretical plates is 50, the feeding position is 25, the reflux ratio is 4, the operation requirement on the top of the tower is 5kPa, the temperature on the top of the tower is 180-200 ℃, and the temperature of a tower kettle is 350-400 ℃, a first food-grade white oil material flow, a second food-grade white oil material flow and a third food-grade white oil material flow are respectively obtained from different measuring lines, and the indexes of the food-grade white oil products are shown in Table 5.
Table 5 example 5 food grade white oil index
Example 6
This example is substantially the same as example 1 except that:
preparing a hydrogenation catalyst: preparing a hydrogenation catalyst: mixing boric acid aqueous solution and amorphous silicon-aluminum according to the mass ratio of boron-containing mass to amorphous silicon-aluminum of 1:999, soaking for 4h, drying for 3h at 100 ℃, and roasting for 2h at 350 ℃ to obtain the catalyst carrier containing the auxiliary agent. Mixing a platinum nitrate solution with a certain concentration with a carrier according to the mass ratio of platinum to carrier of 1:99, soaking for 12h, drying for 3h at 100 ℃, and roasting for 2h at 350 ℃ to obtain the hydrogenation catalyst with the auxiliary agent P accounting for 0.1% of the mass fraction of the catalyst carrier and the total mass fraction of metal platinum accounting for 1%.
Producing food-grade white oil: in a hydrogenation reactor, the reaction temperature is 120 ℃, the pressure is 3MPa, the volume ratio of hydrogen to oil is 200, and the volume space velocity is 0.1h-1Under the condition of (1), deep hydrofining is carried out to remove aromatic hydrocarbon; in the fractionating tower, under the conditions that the number of theoretical plates is 30, the feeding position is 15, the reflux ratio is 4, the operation requirement on the top of the tower is 2kPa, the temperature on the top of the tower is 180-200 ℃, and the temperature of a tower kettle is 350-400 ℃, a first food-grade white oil material flow, a second food-grade white oil material flow and a third food-grade white oil material flow are respectively obtained from different measuring lines, and the indexes of the food-grade white oil products are shown in Table 6.
Table 6 example 6 food grade white oil index
Example 7
This example is substantially the same as example 1 except that:
preparing a hydrogenation catalyst: mixing boric acid aqueous solution and amorphous silicon-aluminum according to the mass ratio of boron-containing mass to amorphous silicon-aluminum of 10:90, soaking for 48h, drying at 100 ℃ for 12h, and roasting at 600 ℃ for 12h to obtain the catalyst carrier containing the auxiliary agent. Mixing and soaking a molybdenum nitrate solution with a certain concentration and a carrier for 48 hours according to the mass ratio of molybdenum to the carrier of 3:2, then drying for 12 hours at the temperature of 120 ℃, and roasting for 12 hours at the temperature of 650 ℃ to obtain the metal hydrogenation catalyst with the assistant P element accounting for 10% of the mass fraction of the catalyst carrier and the total mass fraction of molybdenum accounting for 60%.
Producing food-grade white oil: in a hydrogenation reactor, the reaction temperature is 220 ℃, the pressure is 10MPa, the volume ratio of hydrogen to oil is 1000, and the volume space velocity is 3h-1Under the condition of (1), deep hydrofining is carried out to remove aromatic hydrocarbon; in the fractionating tower, under the conditions that the number of theoretical plates is 60, the feeding position is the 30 th block from the top, the reflux ratio is 10, the operation requirement of the tower top is 10kPa, the temperature of the tower top is 190-210 ℃, and the temperature of a tower kettle is 350-400 ℃, a first food grade white oil material flow, a second food grade white oil material flow and a third food grade white oil material flow are respectively obtained from different measuring lines, and the indexes of the food grade white oil products are shown in Table 7.
Table 7 example 7 food grade white oil index
It should be noted that the above embodiments can be freely combined as necessary. The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The method for producing food-grade white oil from Fischer-Tropsch oil is characterized by comprising the following steps:
the Fischer-Tropsch synthesis raw material firstly enters a hydrogenation unit, and a one-stage hydrogenation reaction is carried out in the presence of hydrogen and a hydrogenation catalyst; and (4) separating the hydrogenation product into gas and liquid, and then feeding the hydrogenation product into a fractionating tower to separate food-grade white oil products with different brands.
2. The process for producing food grade white oil from fischer-tropsch oil according to claim 1, wherein:
the hydrogenation product is subjected to gas-liquid separation by a high-temperature high-pressure separator, the first gas-phase material flow obtained by separation is circularly returned to the hydrogenation unit, the first liquid-phase material flow enters a low-pressure hot separator for continuous gas-liquid separation, the second gas-phase material flow obtained by separation is circularly returned to the hydrogenation unit, and the second liquid-phase material flow enters a fractionating tower.
3. The process for producing food grade white oil from fischer-tropsch oil according to claim 1, wherein:
the Fischer-Tropsch synthesis raw material is tail oil obtained from the bottom of a fractionating tower after the Fischer-Tropsch synthesis oil is subjected to hydro-isomerism cracking, the carbon number is more than or equal to C11+, the distillation range is 200-690 ℃, and the content of isoparaffin is more than or equal to 70%.
4. The process for producing food grade white oil from fischer-tropsch oil according to claim 1, wherein:
in the one-stage hydrogenation reaction, the reaction temperature is controlled to be 120-220 ℃, the reaction pressure is 3.0-10.0 MPa, and the volume ratio of hydrogen to oil is 200-1000: 1, the feeding volume airspeed is 0.1-3.0 h-1。
5. The process for producing food grade white oil from fischer-tropsch oil according to claim 1, wherein:
the hydrogenation catalyst adopts a supported metal catalyst, and active metal in the supported metal catalyst is noble metal and/or non-noble metal.
6. A process for producing food grade white oil from Fischer-Tropsch oil according to claim 5, wherein:
the noble metal is any one or the combination of two of Pt, Pd, Ru and Rh, and the non-noble metal is any one or the combination of two of Ni, W, Co and Mo;
and/or;
the total mass percentage of active metals in the hydrogenation catalyst is 1-60%.
7. A process for producing food grade white oil from Fischer-Tropsch oil according to claim 5, wherein:
the carrier of the hydrogenation catalyst is any one of alumina, silicon dioxide, molecular sieve and amorphous silica-alumina which are modified by an auxiliary agent.
8. A process for producing food grade white oil from Fischer-Tropsch oil according to claim 7, wherein:
the auxiliary agent contains any one of P, B, Ti and Zr elements;
the mass fraction of the auxiliary agent element in the carrier is 0.1-10%.
9. A process for producing food grade white oil from Fischer-Tropsch oil according to any one of claims 5 to 8, wherein the hydrogenation catalyst is produced by a process comprising,
s1, mixing the auxiliary agent and the carrier, soaking for 4-48 hours, drying for 3-12 hours at 100-120 ℃, and then roasting for 2-12 hours at 350-600 ℃ to obtain the carrier containing the auxiliary agent;
s2, mixing and soaking the metal salt solution and the carrier containing the auxiliary agent for 12-48 h, drying at 100-120 ℃ for 3-12 h, and then roasting at 350-650 ℃ for 2-12 h to obtain the metal-based catalyst.
10. The process for producing food grade white oil from fischer-tropsch oil according to claim 1, wherein:
the number of theoretical plates of the fractionating tower is 15-60, the feeding position is 5-55 feeding, the reflux ratio is 0.5-10, the operation pressure at the top of the tower is 2-10 kPa, the operation temperature is 150-250 ℃, and the temperature of the tower kettle is 300-450 ℃.
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