CN114774164A - Method for preparing oxidized wax - Google Patents
Method for preparing oxidized wax Download PDFInfo
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- CN114774164A CN114774164A CN202210345881.5A CN202210345881A CN114774164A CN 114774164 A CN114774164 A CN 114774164A CN 202210345881 A CN202210345881 A CN 202210345881A CN 114774164 A CN114774164 A CN 114774164A
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- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 93
- 230000003647 oxidation Effects 0.000 claims abstract description 57
- 238000006243 chemical reaction Methods 0.000 claims abstract description 51
- 239000003054 catalyst Substances 0.000 claims abstract description 44
- 239000002808 molecular sieve Substances 0.000 claims abstract description 37
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000002994 raw material Substances 0.000 claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 claims abstract description 27
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 18
- 239000010941 cobalt Substances 0.000 claims abstract description 18
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 18
- 230000003197 catalytic effect Effects 0.000 claims abstract description 17
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 12
- 239000011572 manganese Substances 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 5
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- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
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- SZINCDDYCOIOJQ-UHFFFAOYSA-L manganese(2+);octadecanoate Chemical compound [Mn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O SZINCDDYCOIOJQ-UHFFFAOYSA-L 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 229910021536 Zeolite Inorganic materials 0.000 claims description 5
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 5
- 239000012528 membrane Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 239000010457 zeolite Substances 0.000 claims description 5
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims description 4
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 4
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 4
- 239000002002 slurry Substances 0.000 claims description 4
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- AMFIJXSMYBKJQV-UHFFFAOYSA-L cobalt(2+);octadecanoate Chemical compound [Co+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AMFIJXSMYBKJQV-UHFFFAOYSA-L 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- 239000005639 Lauric acid Substances 0.000 claims description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
- 235000021314 Palmitic acid Nutrition 0.000 claims description 2
- 230000003213 activating effect Effects 0.000 claims description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- 235000010338 boric acid Nutrition 0.000 claims description 2
- 235000015165 citric acid Nutrition 0.000 claims description 2
- 229940044175 cobalt sulfate Drugs 0.000 claims description 2
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims description 2
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 2
- 229940099596 manganese sulfate Drugs 0.000 claims description 2
- 235000007079 manganese sulphate Nutrition 0.000 claims description 2
- 239000011702 manganese sulphate Substances 0.000 claims description 2
- SGGOJYZMTYGPCH-UHFFFAOYSA-L manganese(2+);naphthalene-2-carboxylate Chemical compound [Mn+2].C1=CC=CC2=CC(C(=O)[O-])=CC=C21.C1=CC=CC2=CC(C(=O)[O-])=CC=C21 SGGOJYZMTYGPCH-UHFFFAOYSA-L 0.000 claims description 2
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims description 2
- GEMHFKXPOCTAIP-UHFFFAOYSA-N n,n-dimethyl-n'-phenylcarbamimidoyl chloride Chemical compound CN(C)C(Cl)=NC1=CC=CC=C1 GEMHFKXPOCTAIP-UHFFFAOYSA-N 0.000 claims description 2
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 239000012286 potassium permanganate Substances 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims 1
- 239000002253 acid Substances 0.000 abstract description 5
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 abstract description 3
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- 238000011105 stabilization Methods 0.000 description 4
- 238000010924 continuous production Methods 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical group 0.000 description 2
- 230000001050 lubricating effect Effects 0.000 description 2
- -1 manganese stearate ethanol Chemical compound 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- 230000006872 improvement Effects 0.000 description 1
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- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000002023 wood 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
- C10G73/00—Recovery or refining of mineral waxes, e.g. montan wax
- C10G73/38—Chemical modification of petroleum
Landscapes
- 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)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of coal-to-liquid chemical industry, in particular to a preparation method of oxidized wax. The method comprises the steps of carrying out contact reaction on a wax raw material, an oxidation source and an optional catalytic promoter with a catalyst; the catalyst comprises an active component and a molecular sieve carrier, wherein the active component contains element manganese and/or element cobalt. The oxidized wax prepared by the method can obviously improve the yield of the oxidized wax, improve the product quality (uniform product, light color and high ester-acid ratio) of the oxidized wax, does not contain metal elements such as manganese, cobalt and the like in the product, can be continuously produced, and improves the production efficiency of the oxidized wax.
Description
Technical Field
The invention relates to the technical field of coal-to-liquid chemical industry, in particular to a preparation method of oxidized wax.
Background
The Fischer-Tropsch wax is a hydrocarbon product which is synthesized by using synthesis gas under the action of a catalyst and has a molecular weight of 200-2000 and takes normal hydrocarbon as a main component, and has the characteristics of low sulfur, low nitrogen, low aromatic hydrocarbon content and the like, but the unprocessed Fischer-Tropsch wax has low viscosity, poor flexibility, no ductility and difficulty in emulsification. In recent years, with the successive establishment of Fischer-Tropsch synthesis industrial devices of companies such as Ning coal, Yitai, Lu' an and future energy and the realization of long-period and full-load operation, the Fischer-Tropsch wax production capacity is continuously expanded, and the Fischer-Tropsch wax production capacity serving as one of important products in the domestic wax market also becomes a popular product from a scarce resource.
The oxidation of Fischer-Tropsch wax is the first choice way to research and prepare special wax products and to obtain high value-added oxidized wax. Polar groups such as-OH, -COOH, C ═ O, -COOR and the like are added in the oxidized Fischer-Tropsch wax product, and the polar groups endow the oxidized wax product with a plurality of new characteristics, such as emulsibility, lubricity, oil solubility, flexibility and better pigment dispersibility. A certain amount of oxidized wax is added during plastic processing, so that good external lubricating property and strong internal lubricating effect are achieved, the production efficiency can be improved, and the production cost can be reduced; wax emulsion products prepared from oxidized wax are widely used in petrochemical industry, automobile protection, wood processing, building industry, medical supplies, agricultural industry, paper making technology, explosive industry and other industries.
Disclosure of Invention
The invention aims to solve the problems of low production efficiency, poor product quality and low yield of oxidized wax in the prior art, and provides a preparation method of oxidized wax.
In order to achieve the above object, the present invention provides a process for producing an oxidized wax, which comprises contacting a wax raw material, an oxidizing source, optionally a catalyst promoter, with a catalyst to react;
the catalyst comprises an active component and a molecular sieve carrier, wherein the active component contains element manganese and/or element cobalt.
Through the technical scheme, the invention at least has the following advantages:
the oxidized wax prepared by the method can obviously improve the yield of the oxidized wax, improve the product quality (uniform product, light color and high ester-acid ratio) of the oxidized wax, and the product does not contain metal elements such as manganese, cobalt and the like, thereby realizing the continuous production of the oxidized wax and improving the production efficiency of the oxidized wax.
Drawings
FIG. 1 is a corresponding apparatus and flow diagram of a preferred method of producing oxidized wax according to the present invention.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and these ranges or values should be understood to encompass values close to these ranges or values. For numerical ranges, each range between its endpoints and individual point values, and each individual point value can be combined with each other to give one or more new numerical ranges, and such numerical ranges should be construed as specifically disclosed herein.
In the present invention, in the case where no reverse explanation is made, the use of an orientational term such as "upper" generally means a portion 30% of the total length of the reaction unit below the top of the reaction unit, and "lower" generally means a portion 30% of the total length of the reaction unit above the bottom of the reaction unit.
The invention provides a preparation method of oxidized wax, which comprises the steps of carrying out contact reaction on a wax raw material, an oxidation source, an optional catalytic promoter and a catalyst;
the catalyst comprises an active component and a molecular sieve carrier, wherein the active component contains and/or is elemental cobalt.
The oxidized wax prepared by the method can obviously improve the yield of the oxidized wax, improve the product quality (uniform product, light color and high ester-acid ratio) of the oxidized wax, and the product does not contain metal elements such as manganese, cobalt and the like, thereby realizing the continuous production of the oxidized wax and improving the production efficiency of the oxidized wax.
In the present invention, the average pore size of the molecular sieve support is not particularly required as long as the object of the present invention can be achieved, and according to a preferred embodiment of the present invention, the average pore size of the molecular sieve support is not less than 0.5 nm. By adopting the aforementioned preferred embodiment, the yield and quality of the oxidized wax can be further improved.
According to a preferred embodiment of the present invention, the molecular sieve support is selected from at least one of MCM-41 molecular sieves, large pore zeolite molecular sieves, HZSM-5 molecular sieves. By adopting the preferred scheme, the production efficiency, yield and quality of the oxidized wax can be further improved.
According to a preferred embodiment of the present invention, the catalyst has an average particle size of 60 to 80 mesh.
In the present invention, the contents of the active component and the molecular sieve support in the catalyst are not particularly limited as long as the object of the present invention can be achieved, and according to a preferred embodiment of the present invention, the content of the active component in terms of elements in the catalyst is 0.5 to 5 wt% and the content of the molecular sieve support is 55 to 80 wt% based on the total mass of the catalyst. By adopting the preferred scheme, the production efficiency, yield and quality of the oxidized wax can be further improved.
In the present invention, the oxidizing source may be a conventional choice in the art, and according to a preferred embodiment of the present invention, the oxidizing source is an oxygen-containing gas, preferably an oxygen-containing gas having an oxygen content of 20 to 100 vol.%, more preferably air and/or oxygen. By adopting the preferred scheme, the production efficiency, yield and quality of the oxidized wax can be further improved.
In the present invention, the catalytic promoter may be conventionally selected in the art, and according to a preferred embodiment of the present invention, the catalytic promoter is at least one selected from stearic acid, boric acid, oxalic acid, citric acid, palmitic acid, and lauric acid. By adopting the preferred scheme, the production efficiency, yield and quality of the oxidized wax can be further improved.
In the present invention, the wax raw material may be conventionally selected in the art, and according to a preferred embodiment of the present invention, the wax raw material is a fischer-tropsch wax, preferably at least one of a # 52 fischer-tropsch wax, a # 60 fischer-tropsch wax, a # 70 fischer-tropsch wax, a # 80 fischer-tropsch wax, a # 90 fischer-tropsch wax, a # 100 fischer-tropsch wax, a # 105 fischer-tropsch wax, and a # 110 fischer-tropsch wax. By adopting the preferred scheme, the production efficiency, yield and quality of the oxidized wax can be further improved.
In the present invention, the amount of the catalyst used is not particularly limited as long as the object of the present invention can be achieved, and according to a preferred embodiment of the present invention, the amount of the catalyst used is 0.1 to 5% by mass based on the amount of the wax raw material used. By adopting the preferred scheme, the production efficiency, yield and quality of the oxidized wax can be further improved.
In the present invention, the amount of the catalyst promoter to be added is not particularly limited as long as the object of the present invention can be achieved, and according to a preferred embodiment of the present invention, the amount of the catalyst promoter to be added is 0.5 to 6 wt%, preferably 2 to 4 wt% of the amount of the wax raw material to be added. By adopting the preferred scheme, the production efficiency, yield and quality of the oxidized wax can be further improved.
In the present invention, the flow rate of the oxidizing source is not particularly limited as long as the object of the present invention can be achieved, and according to a preferred embodiment of the present invention, the flow rate of the oxidizing source is 0.1 to 1.6L/(h.g wax), preferably 0.2 to 1.2L/(h.g wax). By adopting the preferred scheme, the production efficiency, yield and quality of the oxidized wax can be further improved.
In the present invention, the method for preparing the catalyst is not particularly limited as long as the object of the present invention can be achieved, and according to a preferred embodiment of the present invention, the method for preparing the catalyst comprises:
a. dissolving a manganese source and/or a cobalt source in a solvent to obtain a manganese solution and/or a cobalt solution;
b. roasting the molecular sieve carrier;
c. and loading a manganese solution and/or a cobalt solution on the molecular sieve carrier after roasting treatment, drying and forming to obtain the catalyst.
The catalyst prepared by the preparation method of the catalyst is particularly suitable for preparing oxidized wax, and can further improve the production efficiency, yield and quality of the oxidized wax.
In the present invention, the manganese source and/or the cobalt source may be conventional choices in the art, and according to a preferred embodiment of the present invention, the manganese source is selected from at least one of manganese stearate, manganese naphthenate, manganese sulfate, manganese dioxide, potassium permanganate, and the cobalt source is selected from at least one of cobalt stearate, cobalt sulfate, and cobalt naphthenate.
In the present invention, the solvent may be a conventional choice in the art, and according to a preferred embodiment of the present invention, the solvent is selected from at least one of ethanol, propanol, toluene, and xylene.
In the present invention, the molecular sieve support may be a conventional choice in the art, and according to a preferred embodiment of the present invention, the molecular sieve support is selected from at least one of an MCM-41 molecular sieve, a large pore zeolite molecular sieve, an HZSM-5 molecular sieve.
In the present invention, the conditions of the roasting treatment in step b may be conventionally selected in the art, and according to a preferred embodiment of the present invention, the conditions of the roasting treatment in step b include: the roasting temperature is 300-600 ℃, and the roasting time is 1-10 h, preferably 2-5 h.
In the present invention, the drying conditions in step c may be selected conventionally in the art, and according to a preferred embodiment of the present invention, the drying conditions in step c include: the drying temperature is 80-120 ℃, and the drying time is 6-18 h.
According to a preferred embodiment of the present invention, the method is carried out in an apparatus comprising a wax raw material feeding unit, an oxidation source feeding unit, a material mixing unit, an excitation reaction unit, a first oxidation reaction unit, a second oxidation reaction unit, an oxidized wax collecting unit, and an oxidized wax oil recovering unit;
the material mixing unit is provided with a catalytic assistant feeding hole;
the discharge hole of the oxidation source feeding unit is respectively communicated with the lower feed holes of the excitation reaction unit, the first oxidation reaction unit and the second oxidation reaction unit and is used for providing an oxidation source;
the upper part feed inlet of the oxidized wax oil recovery unit is respectively communicated with the top discharge outlets of the excitation reaction unit, the first oxidation reaction unit and the second oxidation reaction unit and is used for collecting and recovering oxidized wax oil;
the wax raw material feeding unit is communicated with the material mixing unit, so that the wax raw material and the catalytic assistant are mixed to obtain slurry; the material mixing unit is communicated with a feed inlet at the upper part of the excitation reaction unit, so that the slurry can be in countercurrent reaction with an oxidation source from a feed inlet at the lower part from top to bottom; a discharge hole at the bottom of the excitation reaction unit is communicated with a feed inlet at the upper part of the first oxidation reaction unit; the discharge port at the bottom of the first oxidation reaction unit is communicated with the feed inlet at the upper part of the second oxidation reaction unit; the bottom discharge port of the first oxidation reaction unit is communicated with the feed inlet of the oxidized wax collecting unit;
the method comprises the following steps:
s1, melting the wax raw material, mixing the melted wax raw material with a catalytic assistant, and introducing the wax raw material into an excitation reaction unit to perform catalytic excitation reaction with an oxidation source from an oxidation source feeding unit to obtain an excitation material and a first oxidized wax oil gas;
s2, introducing the excited material into a first oxidation reaction unit to perform a first catalytic reaction with an oxidation source from an oxidation source feeding unit to obtain a first reaction material and a second oxidized wax oil gas;
s3, introducing the first reaction material into a second oxidation reaction unit to perform a second catalytic reaction with an oxidation source from an oxidation source feeding unit to obtain a second reaction material and a third oxidized wax oil gas;
and S4, introducing the second reaction material into an oxidized wax collecting unit to obtain oxidized wax, and introducing the first oxidized wax oil gas, the second oxidized wax oil gas and the third oxidized wax oil gas into an oxidized wax oil recovery unit.
By adopting the preferred scheme, the production efficiency, yield and quality of the oxidized wax can be further improved. According to a preferred embodiment of the present invention, the lower feed inlets of the excitation reaction unit, the first oxidation reaction unit and the second oxidation reaction unit are respectively provided with a gas distributor, preferably a membrane gas distributor and/or a coil type distributor, more preferably a membrane gas distributor. By adopting the membrane type gas distributor, the bubbles with small and uniform size can be obtained, the gas-liquid transfer is promoted, and the reaction efficiency is high.
According to a preferred embodiment of the invention, the top discharge ports of the excitation reaction unit, the first oxidation reaction unit and the second oxidation reaction unit are provided with filter screens, and the size of the filter screens is smaller than 60 meshes.
According to a preferred embodiment of the present invention, the excitation reaction unit is provided with a baffle.
According to a preferred embodiment of the present invention, the melting conditions in step S1 include: the temperature is 100 ℃ to 140 ℃, preferably 110-130 ℃.
According to a preferred embodiment of the present invention, the mixing conditions in step S1 include: the temperature is 110-130 ℃.
According to a preferred embodiment of the present invention, the conditions for catalytically activating the reaction in step S1 include: the temperature is 150-190 ℃, the preferable temperature is 160-180 ℃, the pressure is 0-0.5 Mpa, the preferable pressure is 0.2-0.4 Mpa, the time is 0.5-3 h, the preferable time is 1-2 h, the gas flow of an oxidation source is 0.4-1.6L/(h.g wax), the preferable time is 0.8-1.2L/(h.g wax), and the space velocity of the mixed liquid raw material is 20-1000 g/1g catalyst/hour. The conditions of the first catalytic reaction in step S2 include: the temperature is 130-180 ℃, the preferred temperature is 150-170 ℃, the pressure is 0-0.5 Mpa, the preferred pressure is 0.1-0.3 Mpa, the time is 1-4 h, the preferred time is 2-3 h, the air flow of an oxidation source is 0.4-1.6L/(h.g wax), the preferred air flow is 0.8-1.2L/(h.g wax), and the space velocity of an excited material is 20-1000 g/(1g catalyst.h). According to a preferred embodiment of the present invention, the conditions of the second catalytic reaction in step S3 include: the temperature is 130-180 ℃, the preferred temperature is 150-170 ℃, the pressure is 0-0.5 Mpa, the preferred pressure is 0.1-0.3 Mpa, the time is 1-4 h, the preferred time is 2-3 h, the air flow of an oxidation source is 0.4-1.6L/(h.g wax), the preferred time is 0.6-1.2L/(h.g wax), the space velocity of a first reaction material is 20-1000 g/(1g catalyst.h), and the temperature of the excitation reaction is 10-20 ℃ higher than the temperature of the first catalytic reaction and the temperature of the first catalytic reaction.
In the invention, oxidized wax oil gas discharged from the tops of the excitation reaction unit, the first oxidation reaction unit and the second oxidation reaction unit is condensed in a recovery tank together with substances such as wax oil, water and the like, and non-condensable gas is discharged into atmosphere or a flare system.
As shown in fig. 1, the wax raw material feeding unit includes a raw material tank (containing a heating part, not shown) and a material pump; the material mixing unit comprises a material mixing tank and a material pump; the excitation reaction unit comprises an excitation reactor (comprising a heating part, not shown, and the aspect ratio of the excitation reactor to the excitation reactor is 5-25: 1, preferably 15-20: 1); the first oxidation reaction unit comprises a first oxidation reactor (comprising a heating part, not shown, and having an aspect ratio of 15-30: 1, preferably 20-25: 1); the second oxidation reaction unit comprises a second oxidation reactor (comprising a heating part, not shown, and the aspect ratio of the second oxidation reactor is 15-30: 1, preferably 20-25: 1); the oxidation source feeding unit comprises an air compressor and an air stabilization tank, a discharge port is respectively communicated with lower feed ports of the excitation reactor, the first oxidation reactor and the second oxidation reactor, and a flowmeter is arranged to control the feeding amount of the oxidation source; the oxidized wax oil recovery unit comprises an oxidized wax oil recovery tank, and an upper feed inlet of the oxidized wax oil recovery tank is communicated with top discharge outlets of the excitation reactor, the first oxidation reactor and the second oxidation reactor; the oxidized wax collection unit includes a molding device. Specifically, a wax raw material to be oxidized is added into a raw material tank, heated to 100 ℃ and 140 ℃, preferably melted at 110-130 ℃, then conveyed to a material mixing tank through a material pump, 0.5-6 wt%, preferably 2-4 wt% of a catalytic assistant is added into the material mixing tank, the materials are stirred at 110-130 ℃ to be uniformly mixed, then conveyed to an excitation reactor through the material pump, the pressure is controlled to be 0-0.5 MPa, preferably 0.2-0.4 MPa, 0.1-5 mass% of the dosage of the wax raw material is added, an air compressor is controlled, an oxidation source such as air (0.4-1.6L/(h.g wax), preferably 0.8-1.2L/(h.g wax)) is introduced into the excitation reactor through a stabilization tank, the temperature is controlled to be 150-190 ℃ in the excitation reactor, the reaction time of the materials in the excitation reactor is controlled to be 0.5-3 h, preferably 1-2 h, obtaining an excited material and a first oxidized wax oil gas; the excited material is introduced into a first oxidation reactor, an air compressor is controlled, an oxidation source such as air (the air flow is 0.4-1.6L/(h.g wax), preferably 0.8-1.2L/(h.g wax)) is introduced through a stabilization tank, the pressure is 0-0.5 MPa, preferably 0.1-0.3 MPa, a catalyst which is 0.1-5 mass% of the amount of the wax raw material is added, the temperature is 130-180 ℃, preferably 150-170 ℃, the time is 1-4 hours, preferably 2-3 hours, and a first reaction material and a second oxidized wax oil gas are obtained; introducing the first reaction material into a second oxidation reactor, controlling an air compressor, introducing an oxidation source such as air (0.4-1.6L/(h.g wax), preferably 0.6-1.2L/(h.g wax)) through a stabilization tank, wherein the pressure is 0-0.5 Mpa, preferably 0.1-0.3 Mpa, adding a catalyst accounting for 0.1-5 mass% of the wax raw material, the temperature is 130-180 ℃, preferably 150-170 ℃, and the time is 1-4 h, preferably 2-3 h, and obtaining a second reaction material and a third oxidation wax oil gas; and introducing the second reaction material flow into a forming device to obtain an oxidized Fischer-Tropsch wax product, introducing the first oxidized wax oil gas, the second oxidized wax oil gas and the third oxidized wax oil gas into an oxidized wax oil recovery tank to obtain an oxidized wax oil crude product, and further separating to obtain the oxidized wax oil product.
The present invention will be described in detail below by way of examples (using the apparatus and flow shown in FIG. 1). In the following examples, the acid value and the saponification value were measured by the method of NB/SH/T0809; the drop melting point is measured by a drop melting point tester according to the method of GB/T8026; the penetration is measured by a penetration tester according to the method of GB/T4985; the chromaticity is measured by a chromaticity measuring instrument according to the method of GB/T6540; the raw materials are all commercial products.
Example 1
Preparation of the catalyst:
a. dissolving 15g of manganese stearate in ethanol, and stirring to uniformly disperse the manganese stearate to obtain a manganese stearate ethanol solution;
b. roasting the prepared 20g of MCM-41 molecular sieve (the average pore diameter is 8nm) for 5h at the temperature of 450 ℃;
c. dropwise adding a manganese stearate ethanol solution onto a roasted MCM-41 molecular sieve, drying in a drying oven at 100 ℃ for 12 hours after dropwise adding is finished, and extruding to obtain a manganese stearate MCM-41 catalyst with the average particle size of 60-80 meshes (the content of active components is 3.8 wt% in terms of elements, and the content of a molecular sieve carrier is 57 wt%);
adding 60# Fischer-Tropsch wax to be oxidized into a raw material tank, heating to 110 ℃, completely melting a sample, conveying to a material mixing tank, adding 2 wt% of stearic acid catalytic aid, and stirring at 110 ℃ to uniformly mix the materials. Controlling the pressure of an excitation reactor to be 0.4Mpa, adding 1% of prepared manganese stearate MCM-41 catalyst, introducing air (the air flow is 1.0L/(h.g wax)), controlling the temperature of materials in the excitation reactor to be 175 ℃, controlling the reaction time of the materials in the excitation reactor to be 2h, controlling the introduced air (the air flow is 1.2L/(h.g wax)) in a first oxidation reactor and a second oxidation reactor to be 0.35Mpa, adding 1% of prepared manganese stearate MCM-41 catalyst, controlling the temperature to be 160 ℃, controlling the reaction time to be 2h, obtaining oxidized wax oil crude products in an oxidized wax oil recovery tank, and further separating to obtain oxidized wax oil; the oxidized fischer-tropsch wax product was obtained on a forming unit and the properties are given in table 1.
Example 2
The difference from example 1 is that:
in the preparation of the catalyst, an active component is cobalt, a cobalt source is cobalt stearate, a carrier is an HZSM-5 molecular sieve (the average pore diameter is 0.5nm), and the catalyst is prepared (the content of the active component is 2 wt% in terms of elements, and the content of the carrier of the molecular sieve is 77 wt%);
the wax raw material is 90# Fischer-Tropsch wax, the melting temperature is 120 ℃, the addition amount of the auxiliary agent is 3 wt%, the addition amount of the catalyst in the excitation reactor, the first oxidation reactor and the second oxidation reactor is 5%, and the gas flow of the oxidation source is 1.2L/(h.g wax), 1.0L/(h.g wax) and 1.0L/(h.g wax) respectively; controlling the temperature of the materials in the excitation reactor to be 170 ℃; an oxidized fischer-tropsch wax product was obtained, the properties of which are shown in table 1.
Example 3
The same as example 1, except that:
the carrier is a large pore zeolite (average pore size 11 nm).
The wax raw material is 105# Fischer-Tropsch wax, the melting temperature is 130 ℃, the addition amount of the auxiliary agent is 4 wt%, the addition amount of the catalyst in the excitation reactor, the first oxidation reactor and the second oxidation reactor is 2%, and the gas flow rates of the oxidation source are respectively 0.8L/(h.g wax), 0.8L/(h.g wax) and 0.6L/(h.g wax); controlling the temperature of the materials in an excitation reactor to be 180 ℃; an oxidized fischer-tropsch wax product was obtained, the properties of which are shown in table 1.
Example 4
The same as example 1, except that the temperature of the excitation reactor was controlled to 165 ℃. An oxidized fischer-tropsch wax product was obtained, the properties of which are shown in table 1.
Example 5
The same as example 1, except that the content of manganese element was 10%. An oxidized fischer-tropsch wax product was obtained, the properties of which are shown in table 1.
Example 6
The same as example 1, except that the temperature of the excitation reactor, the first oxidation reactor and the second oxidation reactor were controlled to 200 deg.C, 190 deg.C and 190 deg.C, respectively. The product properties are shown in Table 1
Example 7
The same as example 1, except that the temperature of the excitation reactor was controlled to be 160 deg.C (i.e., no excitation reactor was provided). An oxidized fischer-tropsch wax product was obtained, the properties of which are shown in table 1.
Example 8
The same as example 1, except that the average pore diameter of the MCM-41 molecular sieve was 2 nm. An oxidized fischer-tropsch wax product was obtained, the properties of which are shown in table 1.
Comparative example 1
The same as example 1, except that manganese stearate was directly used as a catalyst. The product properties are shown in Table 1.
TABLE 1
In conclusion, the method has the advantages of high reaction efficiency, light color of the obtained oxidized wax product, high quality, high ester-acid ratio, white or light yellow basically, continuous production, great improvement on production efficiency and avoidance of repeated loading and unloading in the production process of an intermittent kettle.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including various technical features being combined in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A preparation method of oxidized wax is characterized in that the method comprises the steps of contacting wax raw material, an oxidation source, and optional catalytic promoter with a catalyst for reaction;
the catalyst comprises an active component and a molecular sieve carrier, wherein the active component contains element manganese and/or element cobalt.
2. The preparation method according to claim 1, wherein the molecular sieve support has an average pore diameter of not less than 0.5 nm; preferably
The molecular sieve carrier is at least one selected from MCM-41 molecular sieves, large-pore zeolite molecular sieves and HZSM-5 molecular sieves.
3. The production method according to claim 1 or 2, wherein, in the catalyst,
the content of active components is 0.5-5 wt% calculated by elements; and/or
The content of the molecular sieve carrier is 55-80 wt%.
4. The production method according to any one of claims 1 to 3,
the oxidation source is an oxygen-containing gas, preferably an oxygen-containing gas with an oxygen content of 20-100 vol%, more preferably air and/or oxygen;
the catalytic promoter is at least one selected from stearic acid, boric acid, oxalic acid, citric acid, palmitic acid and lauric acid; and/or
The wax raw material is Fischer-Tropsch wax, and preferably at least one of No. 52 Fischer-Tropsch wax, No. 60 Fischer-Tropsch wax, No. 70 Fischer-Tropsch wax, No. 80 Fischer-Tropsch wax, No. 90 Fischer-Tropsch wax, No. 100 Fischer-Tropsch wax, No. 105 Fischer-Tropsch wax and No. 110 Fischer-Tropsch wax.
5. The production method according to any one of claims 1 to 4,
the dosage of the catalyst is 0.1 to 5 mass percent of the dosage of the wax raw material; and/or
The addition amount of the catalytic promoter is 0.5-6 wt% of the addition amount of the wax raw material, and preferably 2-4 wt%; and/or
The air flow of the oxidation source is 0.1-1.6L/(h.g wax), and preferably 0.2-1.2L/(h.g wax).
6. The production method according to any one of claims 1 to 5, wherein the catalyst production method comprises:
a. dissolving a manganese source and/or a cobalt source in a solvent to obtain a manganese solution and/or a cobalt solution;
b. roasting the molecular sieve carrier;
c. and loading a manganese solution and/or a cobalt solution on the molecular sieve carrier after roasting treatment, drying and forming to obtain the catalyst.
7. The production method according to claim 6, wherein,
the manganese source is selected from at least one of manganese stearate, manganese naphthenate, manganese sulfate, manganese dioxide and potassium permanganate; and/or
The cobalt source is selected from at least one of cobalt stearate, cobalt sulfate and cobalt naphthenate; and/or
The solvent is selected from at least one of ethanol, propanol, toluene and xylene; and/or
The molecular sieve carrier is at least one selected from MCM-41 molecular sieves, large-pore zeolite molecular sieves and HZSM-5 molecular sieves.
8. The production method according to claim 6 or 7,
in the step b, the roasting treatment conditions comprise: the roasting temperature is 300-600 ℃, and the roasting time is 1-10 h, preferably 2-5 h; and/or
In step c, the drying conditions comprise: the drying temperature is 80-120 ℃, and the drying time is 6-18 h.
9. The process of any one of claims 1 to 8, carried out in an apparatus comprising a wax feedstock feed unit, an oxidation source feed unit, a material mixing unit, an excitation reaction unit, a first oxidation reaction unit, a second oxidation reaction unit, an oxidized wax collection unit, and an oxidized wax oil recovery unit;
the material mixing unit is provided with a catalytic assistant feeding hole;
the discharge hole of the oxidation source feeding unit is respectively communicated with the lower feed inlets of the excitation reaction unit, the first oxidation reaction unit and the second oxidation reaction unit and is used for providing an oxidation source;
the upper part feed inlet of the oxidized wax oil recovery unit is respectively communicated with the top discharge outlets of the excitation reaction unit, the first oxidation reaction unit and the second oxidation reaction unit and is used for collecting and recovering oxidized wax oil;
the wax raw material feeding unit is communicated with the material mixing unit, so that the wax raw material and the catalytic assistant are mixed to obtain slurry; the material mixing unit is communicated with a feed inlet at the upper part of the excitation reaction unit, so that the slurry can be in countercurrent reaction with an oxidation source from a feed inlet at the lower part from top to bottom; a discharge hole at the bottom of the excitation reaction unit is communicated with a feed inlet at the upper part of the first oxidation reaction unit; the discharge port at the bottom of the first oxidation reaction unit is communicated with the feed inlet at the upper part of the second oxidation reaction unit; the bottom discharge port of the first oxidation reaction unit is communicated with the feed inlet of the oxidized wax collecting unit;
the method comprises the following steps:
s1, melting the wax raw material, mixing the melted wax raw material with a catalytic assistant, and introducing the wax raw material into an excitation reaction unit to perform catalytic excitation reaction with an oxidation source from an oxidation source feeding unit to obtain an excitation material and a first oxidized wax oil gas;
s2, introducing the excited material into a first oxidation reaction unit to perform a first catalytic reaction with an oxidation source from an oxidation source feeding unit to obtain a first reaction material and a second oxidized wax oil gas;
s3, introducing the first reaction material into a second oxidation reaction unit to perform a second catalytic reaction with an oxidation source from an oxidation source feeding unit to obtain a second reaction material and a third oxidized wax oil gas;
and S4, introducing the second reaction material into an oxidized wax collecting unit to obtain oxidized wax, and introducing the first oxidized wax oil gas, the second oxidized wax oil gas and the third oxidized wax oil gas into an oxidized wax oil recovery unit.
Preferably, the first and second electrodes are formed of a metal,
gas distributors are respectively arranged at the lower feed inlets of the excitation reaction unit, the first oxidation reaction unit and the second oxidation reaction unit, preferably membrane gas distributors and/or coil type distributors, and more preferably membrane gas distributors; and/or
Filter screens are arranged at discharge ports at the tops of the excitation reaction unit, the first oxidation reaction unit and the second oxidation reaction unit, and the size of each filter screen is smaller than 60 meshes; and/or
The excitation reaction unit is provided with a baffle.
10. The method of claim 9, wherein,
the conditions for melting in step S1 include: the temperature is 100-140 ℃, preferably 110-130 ℃; and/or
The conditions for mixing in step S1 include: the temperature is 110-130 ℃; and/or
The conditions for catalytically activating the reaction in step S1 include: the temperature is 150-190 ℃, the preferable temperature is 160-180 ℃, the pressure is 0-0.5 Mpa, the preferable pressure is 0.2-0.4 Mpa, the time is 0.5-3 h, the preferable time is 1-2 h, the gas flow of an oxidation source is 0.4-1.6L/(h.g wax), the preferable time is 0.8-1.2L/(h.g wax), and the space velocity of the mixed liquid raw material is 20-1000 g/1g catalyst/hour; and/or
The conditions of the first catalytic reaction in the step S2 include: the temperature is 130-180 ℃, the preferable temperature is 150-170 ℃, the pressure is 0-0.5 Mpa, the preferable pressure is 0.1-0.3 Mpa, the time is 1-4 h, the preferable time is 2-3 h, the gas flow of an oxidation source is 0.4-1.6L/(h.g wax), the preferable flow is 0.8-1.2L/(h.g wax), and the space velocity of an excited material is 20-1000 g/1g catalyst.h; and/or
The conditions of the second catalytic reaction in step S3 include: the temperature is 130-180 ℃, the preferred temperature is 150-170 ℃, the pressure is 0-0.5 Mpa, the preferred pressure is 0.1-0.3 Mpa, the time is 1-4 h, the preferred time is 2-3 h, the gas flow of an oxidation source is 0.4-1.6L/(h.g wax), the preferred time is 0.6-1.2L/(h.g wax), and the space velocity of a first reaction material is 20-1000 g/(1g catalyst.h);
wherein the temperature of the excitation reaction is 10-20 ℃ higher than the temperature of the first catalytic reaction and the temperature of the first catalytic reaction.
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| CN115584284A (en) * | 2022-10-28 | 2023-01-10 | 国家能源集团宁夏煤业有限责任公司 | Continuous catalytic oxidation-free Fischer-Tropsch wax system and method |
| CN116651499A (en) * | 2023-05-12 | 2023-08-29 | 国家能源集团宁夏煤业有限责任公司 | Method for producing Fischer-Tropsch wax oxidation catalyst and application thereof |
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| CN104607115A (en) * | 2015-02-01 | 2015-05-13 | 南京天诗新材料科技有限公司 | Method and device for preparing oxidized wax |
| CN112852486A (en) * | 2021-01-12 | 2021-05-28 | 国家能源集团宁夏煤业有限责任公司 | Oxidized wax and preparation method thereof |
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| CN116651499B (en) * | 2023-05-12 | 2024-09-17 | 国家能源集团宁夏煤业有限责任公司 | Method for producing Fischer-Tropsch wax oxidation catalyst and application thereof |
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