CN115558523B - Fischer-Tropsch wax deoiling process - Google Patents
Fischer-Tropsch wax deoiling process Download PDFInfo
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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
- C10G73/36—Recovery of petroleum waxes from other compositions containing oil in minor proportions, from concentrates or from residues; De-oiling, sweating
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Abstract
The invention discloses a Fischer-Tropsch wax deoiling process, which adopts a mixed solvent of cyclohexane, butanone and tertiary butanol as a deoiling solvent, mixes the solvent and Fischer-Tropsch wax into a relatively uniform suspension, and deoils by adopting a solid-liquid extraction process of secondary washing. The solvent system of the invention not only can be used for better selective dissolution of oil in Fischer-Tropsch wax, but also has relatively low boiling point, and is beneficial to solvent recovery; the solvent has low toxicity, safety and environmental protection. The invention has the advantages of simple process equipment investment, low investment cost, simple operation, high safety and easy recovery.
Description
Technical Field
The invention relates to a Fischer-Tropsch wax deoiling process, and belongs to the technical field of petrochemical industry.
Background
Fischer-Tropsch wax is a methylene polymer, an alkane polymer synthesized from hydrocarbon-based synthesis gas or natural gas. At present, fischer-Tropsch wax products generally have the defects of wide boiling range (330-800 ℃), wide carbon distribution (C20-C110), high oil content (about 10%), large odor of low-melting-point products, poor color and the like. Some manufacturers actively explore a product quality improvement method, such as deep processing of Fischer-Tropsch wax by adopting a monomer separation process, so that the rough Fischer-Tropsch wax is subdivided into marks such as 33 ℃ wax, 45 ℃ wax, 60 ℃ wax, 70 ℃ wax, 95 ℃ wax, 100 ℃ wax, 105 ℃ wax and the like, and the product performance is also required by referring to the properties of petroleum wax.
At present, the Fischer-Tropsch wax low-melting-point component with a long straight-chain structure has wide market prospect. For example, the molecular distribution of the wax product at 45 ℃ is concentrated on C20-C30, the oil content is 7-10 percent, mainly isoparaffin, trace oxygen-containing compounds such as alcohol, aldehyde, ketone and the like, and C20-C30 straight-chain alkane with the oil content lower than 2 percent is an excellent production raw material of environment-friendly long-carbon-chain chlorinated paraffin CP-70 (international short-chain chlorinated paraffin products are forbidden); in addition, 45 ℃ waxes are also used in the cosmetic industry, requiring about 3 ten thousand tons per year. The 70 ℃ wax has the molecular distribution concentrated in C30-C40 and the oil content of 3-5%, is mainly normal and high-carbon heterogeneous components lower than C30, and the 70 ℃ wax with the oil content of less than 1% is a lubricant of high-end plastics, has good plasticizing gloss, and can be used for replacing 195# wax of Honival; the water-based paint can also be used as a dispersing agent of water-based paint, and the dispersing effect in the water volatilization process is better than that of 105 ℃ wax commonly used in the traditional ink paint due to the lower melting point, so that the problem of poor paint surface smoothness and glossiness caused by poor wax dispersibility at 105 ℃ can be thoroughly solved. How to reduce the oil content of the finely divided Fischer-Tropsch wax to a low level which is beneficial to subsequent application is a solution which is always sought by the Fischer-Tropsch wax industry: further improvement of the fine separation process still cannot achieve the aim; the existing hydrogenation process cannot thoroughly solve the problem, and the high investment and operation cost can offset the benefits brought by deoiling products. The use of physical separation processes is one solution to the problem.
Solvent deoiling is a main means for improving the quality of petroleum wax products, and a mixed solvent of acetone or methyl ethyl ketone (butanone) and benzene and/or toluene is generally adopted, and oil components in the wax are removed as much as possible through multistage dilution and dissolution. By adjusting the conditions of solvent composition, agent-oil ratio, dilution temperature and the like, the oil content of the petroleum wax can be reduced to less than 0.5 percent, even less than 0.3 percent. The principle is that the insolubility of the strong polar ketone solvent to paraffin linear alkane molecules is utilized to reduce the viscosity of the system at low temperature and improve the fluidity; the solubility of aromatic hydrocarbon to oil substances (including aromatic hydrocarbon, naphthene and long-branched chain heterogeneous molecules) is utilized to carry out dissolution, so as to achieve the aim of reducing the oil content.
However, petroleum wax deoiling processes are not well suited for Fischer-Tropsch wax deoiling. First, solvent systems are unsuitable because the oil component structure in Fischer-Tropsch waxes is relatively single, with shorter branched chain heterogeneous molecules being the dominant, and less polar. Deoiling Fischer-Tropsch wax by using a deoiling solvent system and a multipoint dilution process of petroleum wax, the agent-to-oil ratio is found to be as high as 8:1 or even more than 10:1, but the wax yield is less than 80%, which is not suitable for industrial production. From the technical point of view, the petroleum wax production is often carried out by combining oil dewaxing and wax deoiling, the wax deoiling process is to continuously melt and separate out low-melting-point components in the heating process and dissolve the low-melting-point components in a solvent, and then the target product is obtained and the solvent is recovered through solid-liquid separation, agent-oil separation and other processes; and the Fischer-Tropsch wax is directly sprayed with powder or granulated after the fine separation process. Deoiling requires a separate process to perform.
The prior patent researches the Fischer-Tropsch wax deoiling method, CN113736518A adopts the addition of a wax crystallization modifier for sweating deoiling aiming at the Fischer-Tropsch wax with the melting point of 70 ℃ and above, the production period is 20-40 hours, the yield is 71-83%, the melting point is raised by about 2 ℃, and the oil content can be reduced to below 1.0%; CN106554822a adopts a single solvent (methyl isobutyl ketone) to carry out solvent deoiling through a traditional multi-point dilution process, and fischer-tropsch wax with 96% yield and oil content lower than 1.0% is obtained; CN112574785a is subjected to multistage dilution deoiling under pressurized conditions, and although the solvent is not particularly limited, in the examples, a butanone/toluene mixed solvent is mainly used, the yield is 88-93%, and the oil content can reach 0.2% -0.6%.
The prior Fischer-Tropsch wax deoiling technology is improved under a petroleum wax deoiling process system, wherein the sweating deoiling process is abandoned by the petroleum wax production industry due to long period, high energy consumption and low efficiency; the multipoint dilution process is a dewaxing and deoiling process which has proved to be better, and the deoiling process of the Fischer-Tropsch wax in CN106554822A is equivalent to the traditional solvent dewaxing process, and the key points of the process are solvent selection and dilution temperature control. And crystallizing and separating out the wax in the continuous cooling of the melting system. Because of the large wax content of the melt system, the dissolution and dispersion of the solvent determines the oil content of the final product. Neither the monoketone (methyl isobutyl ketone) nor the ketone-benzene mixed solvent is separated from the petroleum wax deoiling solvent system, but the system has long flow, multiple equipment and complex operation, and the new device is difficult to pass verification and recovery due to the involvement of dangerous chemicals such as toluene, ammonia liquor and the like.
Therefore, aiming at the structural characteristics of Fischer-Tropsch wax and the requirement of final oil content (butanone solubility), it is necessary to develop a new process and solvent system suitable for the deoiling of Fischer-Tropsch wax.
Disclosure of Invention
Aiming at the problems, the invention provides a Fischer-Tropsch wax deoiling process, which adopts a mixed solvent of cyclohexane, butanone and tertiary butanol as a deoiling solvent, mixes the solvent and Fischer-Tropsch wax into a relatively uniform suspension, and deoils by adopting a solid-liquid extraction process of secondary washing. The solvent system of the invention not only can be used for better selective dissolution of oil in Fischer-Tropsch wax, but also has relatively low boiling point, and is beneficial to solvent recovery; the solvent has low toxicity, safety and environmental protection. The invention has the advantages of simple process equipment investment, low investment cost, simple operation, high safety and easy recovery.
The technical scheme of the invention is as follows: a Fischer-Tropsch wax deoiling process is characterized in that a mixed solvent of cyclohexane, butanone and tertiary butanol is used as a deoiling solvent, and the Fischer-Tropsch wax is deoiled by a solid-liquid extraction process of secondary washing; the volume percentage of each solvent in the mixed solvent is as follows: 2-20% of cyclohexane, 80-95% of butanone and 2-15% of tertiary butanol.
The properties of each solvent are shown in Table 1 below.
TABLE 1 Properties of the solvents
| Cyclohexane | Butanone | Tert-butanol | |
| Boiling point/. Degree.C | 80.7 | 79.6 | 82.5 |
| Melting Point/. Degree.C | 6.5 | -86.7 | 25.5 |
| viscosity/mPa.s at 25 DEG C | (25℃)0.888 | (25℃)0.423 | (30℃)3.35 |
| Dipole moment, x 10 -30 C·m | 0 | 9.21 | 1.66 |
| Grade of | Industrial grade | Industrial grade | Industrial grade |
The Fischer-Tropsch wax is the Fischer-Tropsch wax with the solid melting point below 70 ℃ and the oil content of the Fischer-Tropsch wax is more than or equal to 3 percent.
Further, the solid-liquid extraction process of the secondary washing specifically comprises the following steps: grinding and mixing Fischer-Tropsch wax and a mixed solvent (the mass ratio of the Fischer-Tropsch wax to the mixed solvent is 0.2-1:1), so as to obtain a uniform pasty suspension; adding the suspension into a mixed solvent (the mass ratio of the solvent to the wax is 0.2-0.5:1), stirring, vibrating or countercurrent washing pulp at 20-60 ℃, performing solid-liquid separation, and back flushing the obtained filter cake by adopting the mixed solvent (the mass ratio of the solvent to the wax is 0.1-0.5:1) at 20-60 ℃, and evaporating the solvent from the filter cake to obtain deoiled Fischer-Tropsch wax; the used mixed solvent is recycled.
The grinding may be carried out using any available grinding machine such as a grinder, colloid mill or stirrer. The solid-liquid separation adopts a vacuum filter. The mixed solvent is recycled as follows: feeding the solvent for pulp washing and cake washing into a solvent recovery tower, and steaming under normal pressure or reduced pressure to obtain regenerated solvent; the solvent from which the filter cake was distilled off was also recycled.
The innovation points of the invention are as follows:
1. the traditional multi-point dilution process is abandoned, and a solid-liquid extraction process of secondary washing is adopted: mixing a proper amount of solvent with Fischer-Tropsch wax to prepare slurry suspension, washing (countercurrent or oscillating) the suspension with a proper amount of solvent, then carrying out vacuum filtration and solid-liquid separation, carrying out secondary washing and vacuum filtration on the solid part with solvent back flushing, and recovering the solvent of the obtained solid part and the liquid part respectively.
2. According to the molecular structure characteristics of the Fischer-Tropsch wax and the properties of oil components contained in the Fischer-Tropsch wax and the characteristics of solvents required for preparing suspension, through theoretical deduction and a large amount of exploratory tests, the cyclohexane-butanone-tertiary butanol mixed solvent system is found to have the characteristics of excellent selectivity, good oil dissolving effect, low viscosity, good fluidity, moderate boiling point, good safety, easy pulping, easy filtration, easy recovery, no toxicity/low toxicity and the like, and has ideal deoiling effect on the Fischer-Tropsch wax.
The mixed solvent is characterized in that: the Fischer-Tropsch wax is fully mixed with a solvent in a solid state (fine powder) through the processes of grinding, stirring, colloid milling and the like to form a pasty suspension. Because the size of wax particles is not uniform, the formed suspension belongs to a multi-stage dispersion system, wax particles are impacted with a solvent continuously in the process of forming a mixed system, and oil substances are dissolved by the solvent with similar polarity (according to a similar compatibility principle); the weak polar solvent is adsorbed by the nonpolar wax particles to act like a surfactant, so that the wax particles can be temporarily suspended in the system to ensure that the oil substances are fully dissolved. And then the suspension balance is broken by adding the polar solvent, in the polar solvent atmosphere, the nonpolar wax particles are aggregated into larger particles due to being repelled, sedimentation occurs, and the oil-in-wax phenomenon in the traditional deoiling process can not occur in the process, so that the oil dissolved in the solvent is thoroughly carried out. And the oil-wax separation is thoroughly realized by the processes of solid-liquid separation, filter cake re-washing and the like. And (5) recovering and recycling the solvent.
The invention has the technical effects that:
1. the deoiling process is simple: (1) operating at normal pressure; (2) the operation temperature is 10-40 ℃ below the Fischer-Tropsch wax melting point, (3) the mature grinding or stirring pulping process is adopted: 0.2 to 1:1, making the wax ratio into thick paddle-shaped suspension, enabling the solvent to fully contact with wax molecules, enabling oil molecules to enter the solvent through intermolecular force, and keeping the wax molecules in a free state due to the repulsion with the polarity of the solvent; (4) fully washing the slurry in a vibrating or countercurrent mode by using a wax ratio of 0.2-0.5:1; (5) vacuum filtering with vacuum filter, and separating solid from liquid; (6) backwashing the filter cake by using a wax ratio of 0.1-0.5:1; (7) vacuum filter suction filtration, wherein the solid part is deoiling wax containing a small amount of solvent, and the liquid part is solvent containing deoiling oil; (8) wax remover and solvent recovery; the whole process is simple.
2. The deoiling effect is ideal: the oil content can be reduced to less than 1% after the wax is deoiled at 45 ℃ and 50 ℃; the wax at 60 ℃ and 70 ℃ can be reduced to less than 0.5 percent, thereby achieving the ideal use performance requirement.
3. Deoiling conditions are relaxed: the normal pressure operation is carried out, the wax ratio is low (2-0.5), and the deoiling temperature is 20-60 ℃.
4. Lower recovery energy consumption: because the boiling point of the solvent and the azeotropic point of the system are all lower than 100 ℃, the recovery system can be operated at lower temperature.
5. The system has environmental protection: the benzene solvent in the traditional deoiling solvent system is abandoned, and the environment-friendly effect is achieved by adopting a low-toxicity/nontoxic solvent composite system.
6. Low investment and easy recovery: and large-scale refrigeration equipment is not needed, and a water heating or cooling system is safer.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The effects thereof are described below with reference to the drawings and examples of the specification.
Example 1
(1) Preparing solvent
Preheating the mixed solvent (butanone: cyclohexane: tert-butanol=90:2:8) to 55 ℃, and preparing the solvent with the Fischer-Tropsch wax amount of 2 times for later use;
(2) Pulping
70# Fischer-Tropsch wax (oil content 3.61%, melting point 69.6 ℃) and preheated solvent are put into a grinder according to the mass ratio of 1:1 for grinding, so as to prepare thick paste (suspension);
(3) Pulp washing
Driving the paste in the step (2) into a washing kettle with mechanical stirring to heat to 55 ℃, and driving the solvent (solvent with 0.6 times of Fischer-Tropsch wax) preheated to the same temperature in the step (1) into the washing kettle; stirring, and keeping the temperature and stirring for 30-60 min, wherein the materials are in a uniform thin paste (one-step washing); pumping into a vacuum filter for agent-wax separation, and scraping off filter cakes;
(4) Cake washer
And (3) returning the filter cake to the washing kettle, adding the preheated solvent (solvent with the Fischer-Tropsch wax content of 0.4 times) in the step (1), stirring, washing again (secondary washing), and filtering in vacuum after 10-20 min.
(5) Recovery of solvent
The solvent of the first and second washes is mixed and then enters a solvent recovery tower, and the regenerated solvent is obtained by steaming under the condition of normal pressure or reduced pressure, and the solvent yield can reach more than 95%.
(6) Filter cake
And (3) allowing the filter cake after the second washing to enter a solvent evaporation tower, and evaporating the solvent under the condition of normal pressure or reduced pressure to obtain the deoiling wax. The yield of the deoiling wax is 94.5%, the melting point is 70.5 ℃ and the oil content is 0.43%; the total recovery rate of the solvent is more than 98.9 percent.
Example 2
Deoiling 70# Fischer-Tropsch wax (same as in example 1) according to the process of example 1, preheating a solvent (butanone: cyclohexane: tert-butanol=80:5:15) to 35 ℃, and pulping by using a colloid mill with better pulping effect, wherein the solvent ratio (the mass ratio of the solvent to the Fischer-Tropsch wax, the same applies below) is 1.2; and washing by adopting an oscillation kettle, wherein the ratio of the first washing agent to the second washing agent is 0.3. The yield of the deoiling wax is 95.0%, the melting point is 70.3 ℃ and the oil content is 0.45%; the total recovery rate of the solvent is more than 99.5 percent.
Example 3
Deoiling 60# Fischer-Tropsch wax (oil content 5.33%, melting point 60.5 ℃) by the process of example 1, preheating the solvent (butanone: cyclohexane: tert-butanol=85:5:12) to 50 ℃, grinding to slurry, and the solvent ratio is 0.8; and (3) washing the vibrating kettle, wherein the ratio of the first lotion to the second lotion is 0.4, and the ratio of the second lotion to the first lotion is 0.3. The yield of the deoiling wax is 92.8%, the melting point is 61.7 ℃ and the oil content is 0.48%; the total recovery rate of the solvent is more than 98.8 percent.
Example 4
Deoiling 60# Fischer-Tropsch wax (same as in example 3) by the process of example 1, preheating the solvent (butanone: cyclohexane: t-butanol=80:20:5) to 30 ℃, and pulping with a colloid mill at a solvent ratio of 0.5; and (3) washing the vibrating kettle, wherein the ratio of the first lotion to the second lotion is 0.2 and the ratio of the first lotion to the second lotion is 0.3. The yield of the deoiling wax is 92.7%, the melting point is 61.2 ℃ and the oil content is 0.49%; the total recovery rate of the solvent is more than 99.5 percent.
Example 5
Deoiling 50# Fischer-Tropsch wax (oil content 6.27%, melting point 50.4 ℃) by the process of example 1, preheating the solvent (butanone: cyclohexane: tert-butanol=85:12:3 by volume) to 30deg.C (summer normal temperature), stirring to prepare slurry, and the solvent ratio is 1.2; stirred tank washing, one lotion ratio of 0.5 and two lotions ratio of 0.3. The yield of the deoiling wax is 91.8%, the melting point is 51.1 ℃ and the oil content is 0.68%; the total recovery rate of the solvent is more than 99.5 percent.
Example 6
Deoiling 50# Fischer-Tropsch wax (as in example 5) by the process of example 2, preheating the solvent (butanone: cyclohexane: t-butanol=90:10:5 by volume) to 40 ℃, pulping with a colloid mill at a solvent ratio of 0.5; and (3) washing the vibrating kettle, wherein the ratio of the first lotion to the second lotion is 0.3 and the ratio of the second lotion to the first lotion is 0.2. The yield of the deoiling wax is 91.5%, the melting point is 50.8 ℃ and the oil content is 0.61%; the total recovery rate of the solvent is more than 99.5 percent.
Example 7
Deoiling 45# Fischer-Tropsch wax (oil content 8.92% and melting point 46.1 ℃) by the process of example 1, preheating the solvent (butanone: cyclohexane: tert-butanol=80:15:5) to 30 ℃ and pulping with a stirring mechanism, wherein the solvent ratio is 0.5; and (3) washing the vibrating kettle, wherein the ratio of the first lotion to the second lotion is 0.3 and the ratio of the first lotion to the second lotion is 0.2. The yield of the deoiling wax is 89.2%, the melting point is 46.9 ℃ and the oil content is 0.75%; the total recovery rate of the solvent is more than 99.5 percent.
Example 8
Deoiling 45# Fischer-Tropsch wax (same as in example 7) according to the process of example 2, pulping by a colloid mill at a normal temperature of about 25 ℃ with a solvent (butanone: cyclohexane: tert-butanol=85:10:15 by volume ratio), pulping by a colloid mill at a ratio of 0.2, washing by a shaking kettle, and washing by a lotion ratio of 0.2 and a lotion ratio of 0.1. The yield of the deoiling wax is 89.7%, the melting point is 46.2 ℃ and the oil content is 0.80%; the total recovery rate of the solvent is more than 99.8 percent.
Claims (2)
1. A Fischer-Tropsch wax deoiling process is characterized in that a mixed solvent of cyclohexane, butanone and tertiary butanol is used as a deoiling solvent, and the Fischer-Tropsch wax is deoiled by a solid-liquid extraction process of secondary washing; the volume percentage of each solvent in the mixed solvent is as follows: 2-15% of cyclohexane, 80-90% of butanone and 3-15% of tertiary butanol; the Fischer-Tropsch wax is the Fischer-Tropsch wax with the solid melting point below 70 ℃, and the oil content is more than or equal to 3%;
the solid-liquid extraction process of the secondary washing specifically comprises the following steps: grinding and mixing Fischer-Tropsch wax and a mixed solvent to obtain a uniform pasty suspension; adding the suspension into a mixed solvent, stirring, vibrating or countercurrent washing pulp at 20-60 ℃, and performing solid-liquid separation, wherein an obtained filter cake is backwashed by adopting the mixed solvent at 20-60 ℃, and the filter cake is steamed to remove the solvent, so that the deoiled Fischer-Tropsch wax is obtained; the used mixed solvent is recycled;
the grinding and mixing step comprises the steps of mixing a mixed solvent and Fischer-Tropsch wax in a mass ratio of 0.2-1: 1, a step of;
the pulp washing step comprises the steps of mixing a solvent and Fischer-Tropsch wax in a mass ratio of 0.2-0.5: 1, a step of;
the filter cake backwashing step comprises the steps of mixing a solvent and Fischer-Tropsch wax in a mass ratio of 0.1-0.5: 1, a step of;
the equipment adopted for grinding is a grinder, a colloid mill or a stirrer;
the solid-liquid separation adopts a vacuum filter.
2. A fischer-tropsch wax de-oiling process according to claim 1 wherein the mixed solvent is recycled as: feeding the solvent for pulp washing and cake washing into a solvent recovery tower, and steaming under normal pressure or reduced pressure to obtain regenerated solvent; the solvent from which the filter cake was distilled off was also recycled.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106554822A (en) * | 2015-09-28 | 2017-04-05 | 亚申科技研发中心（上海）有限公司 | De-oiling method to Fischer Tropsch waxes |
| CN108865252A (en) * | 2017-05-16 | 2018-11-23 | 神华集团有限责任公司 | Fischer Tropsch waxes and preparation method thereof and preparation system |
| CN110003947A (en) * | 2018-01-04 | 2019-07-12 | 中国石油化工股份有限公司 | The method for producing low gatch and high viscosity index base oil |
| CN112574785A (en) * | 2020-10-23 | 2021-03-30 | 国家能源集团宁夏煤业有限责任公司 | Deoiling method and application of Fischer-Tropsch synthetic wax |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106554822A (en) * | 2015-09-28 | 2017-04-05 | 亚申科技研发中心（上海）有限公司 | De-oiling method to Fischer Tropsch waxes |
| CN108865252A (en) * | 2017-05-16 | 2018-11-23 | 神华集团有限责任公司 | Fischer Tropsch waxes and preparation method thereof and preparation system |
| CN110003947A (en) * | 2018-01-04 | 2019-07-12 | 中国石油化工股份有限公司 | The method for producing low gatch and high viscosity index base oil |
| CN112574785A (en) * | 2020-10-23 | 2021-03-30 | 国家能源集团宁夏煤业有限责任公司 | Deoiling method and application of Fischer-Tropsch synthetic wax |
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