CN114196440B - Apparatus and method for producing Fischer-Tropsch wax product - Google Patents
Apparatus and method for producing Fischer-Tropsch wax product Download PDFInfo
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- CN114196440B CN114196440B CN202010977805.7A CN202010977805A CN114196440B CN 114196440 B CN114196440 B CN 114196440B CN 202010977805 A CN202010977805 A CN 202010977805A CN 114196440 B CN114196440 B CN 114196440B
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- 238000002425 crystallisation Methods 0.000 claims abstract description 62
- 230000008025 crystallization Effects 0.000 claims abstract description 62
- 238000002156 mixing Methods 0.000 claims abstract description 32
- 239000002904 solvent Substances 0.000 claims description 83
- 238000001914 filtration Methods 0.000 claims description 53
- 239000000047 product Substances 0.000 claims description 42
- 239000000706 filtrate Substances 0.000 claims description 34
- 238000000034 method Methods 0.000 claims description 23
- 239000012065 filter cake Substances 0.000 claims description 22
- 238000000926 separation method Methods 0.000 claims description 20
- 238000011084 recovery Methods 0.000 claims description 16
- 238000001704 evaporation Methods 0.000 claims description 12
- 238000007639 printing Methods 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 9
- 230000008020 evaporation Effects 0.000 claims description 7
- 230000008929 regeneration Effects 0.000 claims description 7
- 238000011069 regeneration method Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000010409 thin film Substances 0.000 claims description 5
- 238000005984 hydrogenation reaction Methods 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 3
- 239000004744 fabric Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000005292 vacuum distillation Methods 0.000 claims description 2
- 239000003759 ester based solvent Substances 0.000 claims 2
- 239000005453 ketone based solvent Substances 0.000 claims 2
- 238000011010 flushing procedure Methods 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 abstract description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 18
- 238000009826 distribution Methods 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 6
- 239000004215 Carbon black (E152) Substances 0.000 abstract description 2
- 229930195733 hydrocarbon Natural products 0.000 abstract description 2
- 150000002430 hydrocarbons Chemical class 0.000 abstract description 2
- 239000001993 wax Substances 0.000 description 95
- 238000002844 melting Methods 0.000 description 21
- 230000008018 melting Effects 0.000 description 21
- 238000001816 cooling Methods 0.000 description 13
- 239000000203 mixture Substances 0.000 description 12
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 10
- 230000004927 fusion Effects 0.000 description 9
- 230000035900 sweating Effects 0.000 description 8
- 238000004821 distillation Methods 0.000 description 5
- 239000012467 final product Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 230000035515 penetration Effects 0.000 description 5
- 230000000630 rising effect Effects 0.000 description 5
- 238000000967 suction filtration Methods 0.000 description 5
- 238000009529 body temperature measurement Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 238000010790 dilution Methods 0.000 description 4
- 239000012895 dilution Substances 0.000 description 4
- 210000004243 sweat Anatomy 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000012188 paraffin wax Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000010023 transfer printing Methods 0.000 description 2
- GTJOHISYCKPIMT-UHFFFAOYSA-N 2-methylundecane Chemical compound CCCCCCCCCC(C)C GTJOHISYCKPIMT-UHFFFAOYSA-N 0.000 description 1
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 1
- SGVYKUFIHHTIFL-UHFFFAOYSA-N Isobutylhexyl Natural products CCCCCCCC(C)C SGVYKUFIHHTIFL-UHFFFAOYSA-N 0.000 description 1
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 125000000753 cycloalkyl group Chemical group 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- VKPSKYDESGTTFR-UHFFFAOYSA-N isododecane Natural products CC(C)(C)CC(C)CC(C)(C)C VKPSKYDESGTTFR-UHFFFAOYSA-N 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- 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
- C10G73/42—Refining of petroleum waxes
-
- 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
- C10G73/42—Refining of petroleum waxes
- C10G73/44—Refining of petroleum waxes in the presence of hydrogen or hydrogen-generating compounds
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)
- Fats And Perfumes (AREA)
Abstract
The production device comprises a crystallization filter device, wherein the crystallization filter device comprises N stages of crystallization filter units connected in series, N > =2, each stage of crystallization filter unit comprises a mixing tank, a crystallizer and a filter, the crystallizer is connected with the mixing tank, the filter is connected with the crystallizer, and the outlet temperature of the crystallizer in each stage of crystallization filter unit is the same, similar or sequentially reduced. The invention can effectively reduce the width of the carbon number distribution of the product, reduce the content of the isomerism hydrocarbon and other oil and fat substances, and improve the performance of the product.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a production device and a production method of a Fischer-Tropsch wax product, which can be used for reducing the carbon number distribution width and the oil content of wax, and are particularly suitable for producing wax for printing ink.
Background
Fischer-Tropsch wax is mainly composed of straight-chain, saturated, high-carbon alkanes having a relative molecular mass of 500-1000. The composition is relatively simple, the content of normal straight-chain alkane can reach more than 90%, the rest is basically branched alkane, cyclic hydrocarbon and aromatic hydrocarbon are basically not contained, and compared with isoparaffin and cycloparaffin, the normal alkane has high hardness, the Fischer-Tropsch wax mainly has a C-C, C-H structure, has small surface tension (polarity) and low viscosity, can improve the flowability of the ink, enhances the wettability to the printing surface, and has stable chemical property, no corrosiveness, no pollution and no taste, so the Fischer-Tropsch wax is an ideal raw material for producing the environment-friendly ink wax.
The Fischer-Tropsch wax has a wide carbon number distribution range, is applied to the field of printing ink, and needs to be subjected to hydrogenation, separation and other related procedures, and then the crude wax is separated into waxes with different melting points, wherein the light components and the oil content in the crude wax are main factors influencing the hardness of the Fischer-Tropsch wax.
The molecular short-range distillation technology is directly adopted to separate the wax narrow fraction for the ink, and the separation technology of molecular evaporation ensures that the carbon number concentration of the separated product is not high; the adoption of the true boiling point precise separation has higher requirement on the hardware cost of the rectifying device.
The preparation method of the special wax for thermal transfer printing comprises the following steps: slowly heating paraffin to 125-135 deg.C, and completely melting paraffin; slowly adding Fischer-Tropsch wax into melted paraffin while stirring to make the Fischer-Tropsch wax account for 5-15% of the mixture by weight, always controlling the temperature of the mixture to be 125-135 ℃, uniformly stirring the mixture for 3 hours after the Fischer-Tropsch wax is added, uniformly mixing the mixture, always controlling the temperature of the mixture to be 125-135 ℃, filtering the mixture, and granulating to form the special wax for thermal transfer printing.
The prior art also discloses a method for producing the wax for the ink by adopting an improved sweating process, although the sweat separation efficiency is improved, the limitation of the sweating process makes the target product oil content difficult to achieve the target of 0.1 percent, and the sweating process has long production period and low product yield.
In a process for deoiling Fischer-Tropsch wax, a methyl isobutyl ketone solvent is used as a single solvent to dilute the oily Fischer-Tropsch wax; after dilution, cooling and crystallization for a plurality of times, obtaining crystallization liquid containing solvent; filtering the crystallization liquid by a filter to obtain deoiled wax paste, and evaporating the deoiled wax paste to recover the solvent to obtain the product wax. The method adopts multistage dilution crystallization and one-time filtration to obtain the Fischer-Tropsch wax product with the oil content less than 1 percent and no requirement on the melting range.
Disclosure of Invention
In order to solve the problems in the prior art, the invention takes Fischer-Tropsch wax as a raw material, provides a low-energy-consumption solvent deoiling method for improving the carbon number concentration of the Fischer-Tropsch wax and reducing the oil content, and is particularly suitable for preparing the Fischer-Tropsch ink wax with narrow melting range and high hardness.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the utility model provides a production device of Fischer-Tropsch wax product, includes crystallization filter equipment, crystallization filter equipment includes N grades of serial connection's crystallization filter units, and wherein N > = 2, and every grade of crystallization filter unit includes compounding jar, crystallizer and filter, the crystallizer with the compounding jar links to each other, the filter with the crystallizer links to each other, and the exit temperature of crystallizer is near or reduces in proper order in each grade of crystallization filter unit.
In some embodiments, in the crystallization filtering device, after the cold energy is recovered by heat exchange between the N-level filtrate from the N-level filter and the N-level crystallizer, the N-level filtrate is sent to the N-1 level mixing tank as N-1 level solvent, wherein N > =2 and N < =n, the first-level filtrate from the first-level filter and the first-level crystallizer are sent to the first solvent recovery device for solvent regeneration, and the regenerated solvent is sent to the N-level mixing tank of the N-level crystallization filtering unit.
In some embodiments, the crystallizer of each stage comprises at least two heat exchangers in series.
In some embodiments, the heat exchanger is a double-pipe heat exchanger or a shell-and-tube heat exchanger.
In some embodiments, the heat exchanger is a shell-and-tube crystallizer, and the crystallized material is conveyed using a high pressure pump.
In some embodiments, the production apparatus includes a second solvent recovery apparatus coupled to the filter of the N-stage crystallization filtration unit for evaporating solvent in the recovered filter cake and obtaining product wax.
In some embodiments, the filter uses nitrogen as a safety gas and is used to blow back the filter cloth.
In some embodiments, the production unit further comprises a hydrogenation unit and/or a separation unit.
In some embodiments, the separation device is a thin film evaporator, short path evaporator, or reduced pressure rectification column.
A process for the production of a fischer-tropsch wax product comprising:
performing multistage crystallization and filtration treatment on Fischer-Tropsch wax or narrow fraction wax thereof;
in each stage of crystallization and filtration treatment, the narrow fraction wax is dissolved and then crystallized and filtered in sequence, and the outlet temperatures of the crystallization and the filtration are similar or gradually reduced.
In some embodiments, the Fischer-Tropsch wax is separated by thin film evaporation, short path evaporation, and vacuum distillation.
In some embodiments, in each stage of crystallization filtration treatment, the filtrate is used as a solvent in the previous stage of crystallization filtration treatment after heat exchange with the crystallizer, and in the stage of crystallization filtration treatment, the filtrate is subjected to solvent regeneration after heat exchange with the crystallizer, and the regenerated solvent is used as a solvent in the final stage of crystallization filtration treatment.
In some embodiments, the method further comprises evaporating the solvent in the final stage filter cake.
In some embodiments, the solvent in the multistage crystallization filtration process is one or more of a ketone solvent, an ester solvent, an isoparaffinic solvent.
In some embodiments, the narrow fraction wax is obtained by hydrofinishing a Fischer-Tropsch wax followed by separation.
In some embodiments, the Fischer-Tropsch wax product is an ink wax, and the narrow cut wax has a first point of distillation greater than 350 ℃ and a final point of distillation less than 550 ℃.
Compared with the prior art, the invention has the following beneficial effects:
1. in the prior art, on one hand, the width of carbon number distribution and the oil content are reduced by sweating the Fischer-Tropsch wax narrow fraction wax, but the sweating process has long production period and low product yield, and on the other hand, the oil content is reduced by traditional solvent deoiling, but the concentration of the carbon number cannot be improved, and the hardness of the final product is affected.
According to the invention, the Fischer-Tropsch refined wax or the narrow fraction wax is mixed with the preferable solvent, and the carbon number distribution width of the product is effectively reduced in a mode of combining high-temperature filtering separation and low-temperature filtering separation, and simultaneously the content of the isomerism hydrocarbon and other oily substances are reduced, so that the low oil content and high hardness of the product are realized, and finally, the performance of the product meets the technical requirements of the wax for the high-performance printing ink.
2. In the multistage cooling crystallization and filtration operation, the invention reduces the recovery energy of the solvent by recovering the cold energy of the filtrate and countercurrent washing of the solvent. And the innovative application of the crystallizer reduces the equipment cold consumption of the crystallizer.
Drawings
The following drawings are only for purposes of illustration and explanation of the present invention and are not intended to limit the scope of the invention. Wherein:
FIG. 1 is a schematic diagram of an apparatus for producing Fischer-Tropsch wax product in accordance with an embodiment of the invention.
Detailed Description
The present invention will be further described in detail below with reference to specific embodiments and with reference to the accompanying drawings, in order to make the objects, technical solutions and advantages of the present invention more apparent.
Reference throughout this specification to "one embodiment" or "an embodiment" means that a particular feature, structure, or parameter, step, or the like described in the embodiment is included in at least one embodiment according to the present invention. Thus, references to "one embodiment according to the present invention," "in an embodiment," and the like, in this specification are not intended to specify the presence of stated features but rather are intended to be included in particular embodiments, if they are used in the same sense. It will be appreciated by those of skill in the art that the specific features, structures or parameters, steps, etc. disclosed in one or more of the embodiments of the invention may be combined in any suitable manner.
In the description of the present invention, it should be noted that, unless explicitly specified and limited otherwise, the terms "connected," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; can be directly connected or indirectly connected through an intermediate medium. The specific meaning of the above terms in the present invention can be understood as appropriate by those of ordinary skill in the art.
The Fischer-Tropsch refined wax in the invention refers to a product of the Fischer-Tropsch synthetic wax, which is subjected to hydrofining to effectively remove olefin, oxygen-containing compounds and other substances.
The wax for the ink is used as a main raw material in the ink, and after the ink is coated on the surface of a plastic base or a paper base, the wax can float on the surface of an ink layer to play a role in preventing smudging. In the printing process, the wax film is melted under the action of heat and printing pressure, so that the printing ink can transfer images and texts to the surface of the printing material.
According to the embodiment of the invention, aiming at the index requirement of the wax for the ink, the Fischer-Tropsch wax is first hydrofined, and then all fractions with initial distillation points of more than 350 ℃ and final distillation points of less than 550 ℃ are separated. Mixing the narrow fraction with proper solvent (single solvent or mixed solvent of ketone, ester, isoparaffin, etc.), cooling, crystallizing and filtering by N-stage (N > =2), to obtain wax for ink with melting point of 50-90 deg.C, and oil content of less than 0.1%. Since trace amounts of residual materials also affect the product application, benzene solvents should be avoided.
As shown in FIG. 1, the Fischer-Tropsch wax product production device in the embodiment of the invention comprises a hydrogenation device, a separation device and a crystallization and filtration device which are sequentially connected, wherein the separation device can be a thin film evaporator, a short-range evaporator, a vacuum rectification tower and the like. The crystallization filtering device comprises N stages of crystallization filtering units (N > =2) which are connected in series, wherein each stage of crystallization filtering unit comprises a mixing tank, a crystallizer and a filter which are connected in sequence. Namely, the first-stage mixing tank, the first-stage crystallizer, the first-stage filter, the second-stage mixing tank, the second-stage crystallizer and the second-stage filter … … are sequentially connected. The outlet temperatures of the crystallizers in the crystallization filtration units of each stage are the same, close or decreasing in sequence, preferably decreasing in sequence, i.e. the temperature of the N-stage crystallizer is lower than the outlet temperature of the N-1 stage crystallizer, N > =2, and N < =n.
The temperature of the high-temperature material from the mixing tank is gradually reduced to the target temperature in the crystallizer. Each stage of crystallizer can comprise more than two heat exchangers connected in series, wherein the first heat exchanger is used for recovering the filtered liquid, and the second or subsequent heat exchangers are used for controlling the temperature through the modes of circulating water, the flow of cold medium such as an ice maker and the like. The heat exchanger can be a sleeve heat exchanger or a shell-and-tube heat exchanger, preferably a shell-and-tube heat exchanger, so that heat brought by rotation of a scraper in the sleeve crystallizer is avoided, and the cold consumption is increased. When the shell-and-tube crystallizer is used, in order to avoid the influence of condensation of the cooling crystallization material on the inner surface of the heat exchanger tube array on the heat exchange effect, the crystallization material can be conveyed by a high-pressure pump, and the material residence time is reduced. Each stage of filter is provided with nitrogen as a safety gas and is used for back blowing the filter cloth. The filter can be filtered by suction filtration.
In the crystallization filtering device, after the cold energy is recovered by heat exchange between N-level filtrate from an N-level filter and an N-level crystallizer, the N-level filtrate is used as N-1 level solvent to be sent to an N-1 level mixing tank, in the N-1 level mixing tank, the N-1 level solvent is heated to dissolve a filter cake of N-2 level, the first-level filtrate from a first-level filter and the first-level crystallizer are subjected to heat exchange and then sent to a first solvent recovery device to be subjected to solvent regeneration, the regenerated solvent is sent to an N-level mixing tank of an N-level crystallization filtering unit, and the regenerated solvent can be used as cold solvent to wash the residual filtrate on the surface of the filter cake in the N-level filtering device. The filter cake obtained in the N-stage filtering device can be evaporated in a second solvent recovery device to recover the solvent in the filter cake, so that a final product is obtained.
In the N-level cooling crystallization filtering operation, the temperature is stepped to be cooled, and the high-temperature filtering separation is mainly used for removing low-carbon components, so that the concentration of carbon numbers is improved; the low-temperature filtration separation is used for removing oil components, the countercurrent washing is adopted for the solvent in the multistage cooling crystallization process, the heat exchange between filtrate and molten mixture is realized, the cooling energy consumption and the solvent recovery energy consumption are reduced, and finally the wax product with narrow melting range, low oil content and high hardness is realized. The invention is especially suitable for the wax products for the ink with higher requirement on the carbon number concentration.
The embodiment of the invention utilizes the better solubility of the solvent to the Fischer-Tropsch wax oil lipid component, and the solvent can effectively dissolve low-carbon alkane (light component) along with the rising of the temperature, so that the Fischer-Tropsch refined wax or the coarsely separated narrow fraction wax is adopted to remove the light component through the high-temperature separation of the solvent, and the low-temperature filtration is adopted to remove the oil component, thereby realizing the performances of narrow carbon number distribution, low oil content and high hardness of the Fischer-Tropsch wax, and leading the Fischer-Tropsch wax to have outstanding performances in the application field of ink.
When the Fischer-Tropsch wax product is produced by using the production device, the Fischer-Tropsch wax is firstly hydrofined into Fischer-Tropsch refined wax, a small amount of olefin is saturated, a small amount of oxygen-containing organic matters in the Fischer-Tropsch wax are reduced, and the substances influence the quality (including color, oil content and penetration) of the Fischer-Tropsch wax and are easy to deteriorate in subsequent processing.
The Fischer-Tropsch refined wax is coarsely separated into narrow fractions with different melting points, and the separation modes can be film evaporation, short-range evaporation, vacuum rectification and the like. In one embodiment, the narrow-cut wax obtained after separation has an initial point of greater than 350 ℃ and an end point of less than 550 ℃ and contains 3-5% of the oil component (the oil content in the wax is that 1g of wax is dissolved in 15ml of butanone, and the dissolved part accounts for the mass fraction of the wax when the temperature is reduced to-31.9 ℃), and the light component in the separated narrow-cut wax also affects the hardness of the Fischer-Tropsch wax.
The narrow fraction wax is subjected to multistage cooling crystallization filtration treatment in a crystallization filtration device, so that the carbon number concentration is improved, the oil content is reduced, and the final product can be used as wax for printing ink.
It should be noted that the present invention is not limited to the preparation of waxes for ink, and the apparatus and method of the present invention may be applied to any application that reduces the carbon number distribution and reduces the oil content.
Example 1
The method comprises the steps of taking Fischer-Tropsch refined wax as a raw material, separating fraction wax with a melting point of 60.3 ℃ in a short distance, mixing the fraction wax with isododecane in a first-stage mixing tank (the wax agent ratio is 1:4, the melting point is reduced to 50 ℃ after mixing), exchanging heat between a molten mixed material and a first-stage filtrate, cooling circulating water to 30 ℃, crystallizing, filtering in a first-stage filter, exchanging heat between the first-stage filtrate and a first-stage crystallizer, recovering cold energy, and sending the recovered cold energy to a first solvent recovery device to realize solvent regeneration (the purity of recovered solvent is more than 99%).
The first-stage filter cake is sent to a second-stage mixing tank to be mixed with third-stage filtrate, the molten mixture exchanges heat with the second-stage filtrate, a refrigerating unit cools and crystallizes to 10 ℃, the second-stage filtrate is filtered in a second-stage filter, and the second-stage filtrate exchanges heat with a second-stage crystallizer to recover cold energy as a first-stage solvent and is sent to the first-stage mixing tank. And (3) sending the secondary filter cake into a tertiary mixing tank to be mixed with a regenerated solvent, exchanging heat between the molten mixed material and tertiary filtrate, cooling and crystallizing to 0 ℃ by a refrigerating unit, performing suction filtration in a tertiary filter, and sending the tertiary filtrate and tertiary crystallization into the secondary mixing tank as the secondary solvent after exchanging heat cold energy.
Melting the three-stage filter cake in a wax melting tank, feeding the melted three-stage filter cake into a second solvent recovery device to achieve product purification, wherein the final product yield is 82%, the product melting point is 62.8 ℃, the oil content (solubility in butanone) is less than 0.1%, the penetration is 4.6 (1/10) mm@25 ℃, and the viscosity is 3.8mm 2 And/s@100℃. The heat of fusion in the temperature measurement zone (55-75 ℃) is analyzed by a Differential Scanning Calorimeter (DSC), and the larger the heat of fusion is, the more concentrated the carbon number is, and the test conditions are: the sample is weighed to be 5mg, the temperature rising rate is 5 ℃/min, and the detection result is 228J/g.
Example 2
The method comprises the steps of taking Fischer-Tropsch refined wax as a raw material, separating fraction wax with a melting point of 81.3 ℃ in a short distance, mixing the fraction wax with butyl acetate in a first-stage mixing tank (the wax agent ratio is 1:4), carrying out heat exchange on the molten mixture and first-stage filtrate, cooling circulating water to crystallize to 40 ℃, carrying out suction filtration in a first-stage filter, carrying out heat exchange on the first-stage filtrate and a first-stage crystallizer, recovering cold energy, and sending the recovered cold energy into a first solvent recovery device to realize solvent regeneration (the recovered solvent purity is more than 99%).
The first-stage filter cake is sent to a second-stage mixing tank to be mixed with third-stage filtrate, the molten mixture exchanges heat with the second-stage filtrate, a refrigerating unit cools and crystallizes to 20 ℃, the second-stage filtrate is filtered in a second-stage filter, and the second-stage filtrate exchanges heat with a second-stage crystallizer to recover cold energy as a first-stage solvent and is sent to the first-stage mixing tank. And (3) sending the second-stage filter cake into a third-stage mixing tank to be mixed with the regenerated solvent, cooling to be crystallized to 10 ℃, carrying out suction filtration in a third-stage filter, and sending the third-stage filtrate into the second-stage mixing tank as the second-stage solvent.
Melting the three-stage filter cake in a wax melting tank, feeding the melted three-stage filter cake into a second solvent recovery device to achieve product purification, wherein the final product yield is 80%, the product melting point is 83 ℃, the oil content (solubility in butanone) is less than 0.1%, the penetration is 2.6 (1/10) mm@25 ℃, and the viscosity is 7.9mm 2 And/s@100℃. The heat of fusion in the temperature measurement zone (55-75 ℃) is analyzed by a Differential Scanning Calorimeter (DSC), and the larger the heat of fusion is, the more concentrated the carbon number is, and the test conditions are: the sample is weighed to be 5mg, the temperature rising rate is 5 ℃/min, and the detection result is 232J/g.
Comparative example 1
The Fischer-Tropsch refined wax is used as a raw material to separate fraction wax with the melting point of 60.3 ℃ in a short-distance way, the temperature is reduced to 30 ℃ for crystallization in a sweating device, and the temperature is kept for more than 4 hours for full crystallization. Slowly heating to 52 ℃ for 8 hours, and discharging light components (sweat); continuously heating to 56 ℃ and keeping the temperature for 8 hours, and discharging light components (sweat); continuously heating to 60 ℃ and keeping the temperature for 8-12h, stopping sweating when no sweat is discharged, and heating to melt and collect the product. The yield of the product is 65%, the melting point is 63.1 ℃, the oil content (solubility in butanone) is 0.5%, the penetration is 6.1 (1/10) mm@25deg.C, and the viscosity is 4.0mm 2 /s@100℃。
The heat of fusion in the temperature measurement zone (55-75 ℃) is analyzed by a Differential Scanning Calorimeter (DSC), and the larger the heat of fusion is, the more concentrated the carbon number is, and the test conditions are: the sample is weighed to be 5mg, the temperature rising rate is 5 ℃/min, and the detection result is 235J/g.
Comparative example 2
The method comprises the steps of short-range separation of Fischer-Tropsch refined wax to obtain fraction wax with a melting point of 60.3 ℃ as a raw material, deoiling by a solvent deoiling device, mixing the raw material with MIBK solvent in a mixing tank at a temperature of 1:4, feeding the mixture into a sleeve crystallization, cooling, performing primary solvent dilution (wax ratio of 1:4) in the sleeve crystallization, performing secondary solvent dilution (wax ratio of 1:4) at an outlet of a sleeve crystallizer, feeding the sleeve crystallization into a suction filtration device at an outlet temperature of 0 ℃, washing a filter cake by the solvent (wax ratio of 1:2), and suction filtering, wherein a final filter cake is subjected to solvent recovery by a solvent recovery device, thereby obtaining a product.
The yield of the product is 90 percent, the melting point of the product is 61.1 ℃, the oil content (solubility in butanone) is 0.8 percent, and the penetration is 7.2 (1/10) mm@25deg.C, viscosity 3.7mm 2 /s@100℃。
The heat of fusion in the temperature measurement zone (55-75 ℃) is analyzed by a Differential Scanning Calorimeter (DSC), and the larger the heat of fusion is, the more concentrated the carbon number is, and the test conditions are: the sample is weighed to be 5mg, the temperature rising rate is 5 ℃/min, and the detection result is 211J/g.
| Example 1 | Example 2 | Comparative example 1 | Comparative example 2 | |
| The oil content of the product is% | Less than 0.1 | Less than 0.1 | 0.5 | 0.8 |
| Heat of fusion (55-75 ℃) J/g | 228 | 232 | 235 | 211 |
| Product yield% | 82 | 80 | 65 | 90 |
The experimental comparison result shows that: the three-stage deoiling product provided by the embodiment of the invention can realize the melting heat similar to that of sweating deoiling under the condition of obviously high product yield, and the oil content of the product is obviously reduced. Compared with the conventional solvent deoiling mode, the method realizes the remarkable improvement of the oil content and carbon number concentration of the product under the condition of slightly reducing the product yield.
The foregoing description of the embodiments has been provided for the purpose of illustrating the general principles of the invention, and is not meant to limit the invention thereto, but to limit the invention thereto, and any modifications, equivalents, improvements and equivalents thereof may be made without departing from the spirit and principles of the invention.
Claims (9)
1. The production device is used for preparing the wax for the printing ink by taking Fischer-Tropsch synthetic wax as a raw material and is characterized by comprising a hydrogenation device, a separation device and a crystallization filtering device which are sequentially connected, wherein the crystallization filtering device comprises N stages of crystallization filtering units which are connected in series, N > =2, each stage of crystallization filtering unit comprises a mixing tank, a crystallizer and a filter, the crystallizer is connected with the mixing tank, the filter is connected with the crystallizer, the filter of the Nth stage of crystallization filtering unit is connected with a second solvent recovery device, the outlet temperature of the crystallizer in each stage of crystallization filtering unit is sequentially reduced, and the crystallizer of each stage comprises at least two heat exchangers which are connected in series;
in the crystallization filtering device, after the cold energy is recovered through heat exchange between N-level filtrate from an N-level filter and an N-level crystallizer, the N-1 level filtrate is used as N-1 level solvent to be sent to an N-1 level mixing tank, N-2 level filter cakes are dissolved after the N-1 level solvent is heated, wherein N > =2 and N < = N, the first level filtrate from the first level filter is sent to a first solvent recovery device for solvent regeneration after heat exchange between the first level filtrate and the first level crystallizer, the regenerated solvent is sent to an N level mixing tank of an N level crystallization filtering unit, the regenerated solvent is used as cold solvent in the N level filtering device to wash the residual filtrate on the surface of the filter cakes, and the filter cakes obtained in the N level filter are evaporated in a second solvent recovery device to recover the solvent in the filter cakes and obtain product wax;
wherein the solvent in the multistage crystallization filtration treatment is one or more of ketone solvents, ester solvents and isoparaffin solvents.
2. Use according to claim 1, wherein the heat exchanger is a double-pipe heat exchanger or a shell-and-tube heat exchanger.
3. Use according to claim 1, characterized in that the heat exchanger is a shell-and-tube crystallizer, the crystallised material being conveyed by means of a high-pressure pump.
4. Use according to claim 1, characterized in that the filter uses nitrogen as safety gas and is used for back-flushing the filter cloth.
5. Use according to claim 1, characterized in that the separation device is a thin film evaporator, a short path evaporator or a reduced pressure rectification column.
6. A process for the production of a fischer-tropsch wax product using a production plant according to any one of claims 1 to 5, characterized in that the process comprises:
carrying out multistage crystallization and filtration treatment on the narrow-fraction wax of the Fischer-Tropsch wax, wherein the narrow-fraction wax of the Fischer-Tropsch wax is obtained by separating the Fischer-Tropsch wax after hydrofining;
in each stage of crystallization and filtration treatment, the narrow fraction wax is dissolved and then sequentially crystallized and filtered, and the outlet temperatures of crystallization and filtration are gradually reduced;
the method comprises the steps of carrying out heat exchange on filtrate and a crystallizer in each stage of crystallization filtration treatment, then using the filtrate and the crystallizer as solvents in the previous stage of crystallization filtration treatment, carrying out solvent regeneration on the filtrate and the crystallizer after heat exchange in the first stage of crystallization filtration treatment, using the regenerated solvents as solvents in the last stage of crystallization filtration treatment, and evaporating and recovering the solvents in the filter cake in a second solvent recovery device to obtain a product, wherein the Fischer-Tropsch wax product is wax for printing ink;
wherein the solvent in the multistage crystallization filtration treatment is one or more of ketone solvents, ester solvents and isoparaffin solvents.
7. The method of claim 6, further comprising evaporating the solvent from the final stage filter cake.
8. The method according to claim 6, wherein the separation is thin film evaporation, short path evaporation or vacuum distillation.
9. The process of claim 6 wherein the narrow-cut wax has a primary boiling point greater than 350 ℃ and a final boiling point less than 550 ℃.
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