CN109321274B - Process for recovering paraffin from Fischer-Tropsch wax residue by one-step method and simultaneously passivating and inactivating catalyst - Google Patents
Process for recovering paraffin from Fischer-Tropsch wax residue by one-step method and simultaneously passivating and inactivating catalyst Download PDFInfo
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- CN109321274B CN109321274B CN201811294428.6A CN201811294428A CN109321274B CN 109321274 B CN109321274 B CN 109321274B CN 201811294428 A CN201811294428 A CN 201811294428A CN 109321274 B CN109321274 B CN 109321274B
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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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- 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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1022—Fischer-Tropsch products
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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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/70—Catalyst aspects
- C10G2300/705—Passivation
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Processing Of Solid Wastes (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
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Abstract
The invention relates to a process for recovering paraffin from Fischer-Tropsch wax residue and simultaneously passivating and inactivating a catalyst by a one-step method, and belongs to the technical field of Fischer-Tropsch wax residue treatment. The invention aims to provide a process for recovering paraffin from Fischer-Tropsch wax residue and passivating and inactivating a catalyst by a one-step method. Mixing Fischer-Tropsch wax residue with a compound solvent, heating to 100-250 ℃, preserving heat for 30-240 min, and then carrying out solid-liquid separation to obtain solid residue and a mixed solution; the obtained solid residue is a catalyst for deactivation, and the obtained mixed solution is a paraffin solution. The method can complete the separation of paraffin and the passivation and inactivation of the catalyst in one step, reduce the technical process and equipment investment and reduce the cost. The method of the invention is adopted to separate and recover Fischer-Tropsch wax residue, the recovery efficiency of paraffin wax is high and can reach more than 99%, and the temperature of the combustible point of the catalyst after passivation and inactivation treatment is raised to more than 600 ℃, so that the potential risk of combustion is completely avoided, and the catalyst can be safely buried.
Description
Technical Field
The invention relates to a process for recovering paraffin from Fischer-Tropsch wax residue and simultaneously passivating and inactivating a catalyst by a one-step method, and belongs to the technical field of Fischer-Tropsch wax residue treatment.
Background
The coal-to-liquid technology in China is related to national energy safety. Besides obtaining clean gasoline and diesel oil, the coal-based oil also is an important product. The 'wax residue' is generated in the separation process of the Fischer-Tropsch paraffin and the Fischer-Tropsch catalyst. The paraffin wax synthesized from the fischer-tropsch reactor is a mixed wax with various melting point specifications. The light wax with a lower melting point is easily separated from the catalyst, while the heavy wax with a higher melting point is easily wrapped on the surface of the catalyst, forms a filter cake along with the catalyst and finally forms so-called wax residue. It can be seen that the wax residue mainly contains paraffin and a catalyst, and because the wax residue contains the reduced metal catalyst, the wax residue is easy to spontaneously combust and smoke and ignite when exposed to air, and if the wax residue is not treated, the wax residue can be ignited to cause safety accidents, thereby bringing serious troubles to enterprises. The wax residue belongs to dangerous waste and needs to be treated by a company with the treatment qualification of the dangerous waste, which causes high treatment cost and brings economic burden to enterprises.
The conventional technology adopts a high-temperature cracking process for the oil (wax) -containing solid waste residues, the wax component in the wax residues is subjected to high-temperature cracking, and the solid residues of the catalyst can be used as common wastes for landfill treatment after high-temperature treatment, such as patents CN105542854A and CN 103173238A. This technique presents a certain safety risk and waste of resources because it is not economically cost effective to convert the wax to lower gaseous hydrocarbons.
In contrast, the inventor has studied a process for recovering wax residue by an extraction separation method, i.e., an invention patent with application number 201810619832X, in which fischer-tropsch wax residue is mixed with an extractant, and an extraction separation method is adopted to separate solid from liquid, recover paraffin from the liquid, and passivate the solid (i.e., a catalyst). By adopting the method, high-grade solid paraffin can be recovered, and the aim of catalyst deactivation is fulfilled. However, it was found in the research that this method also has certain drawbacks: the extraction process is complex and comprises two steps of solid paraffin recovery and catalyst deactivation, and the process route is long and the equipment investment is large. In addition, the method has the advantages that the extracting agent contains the pore canal penetrating agent, and the recovery rate of the paraffin can be improved to more than 95%. However, when the amount of wax residue to be treated is large (tens of thousands of tons per year), the absolute loss amount of paraffin is still large.
Disclosure of Invention
Aiming at the defects, the technical problem solved by the invention is to provide a process for recovering paraffin from Fischer-Tropsch wax residue and simultaneously passivating and inactivating a catalyst by a one-step method.
The invention relates to a process for recovering paraffin from Fischer-Tropsch wax residue and simultaneously passivating and inactivating a catalyst by a one-step method, which comprises the steps of mixing Fischer-Tropsch wax residue with a compound solvent, heating to 100-250 ℃, keeping the temperature for 30-240 min, and then carrying out solid-liquid separation to obtain solid residue and a mixed solution; the obtained solid slag is a deactivated and inactivated catalyst, and the obtained mixed solution is a paraffin solution; wherein the compound solvent consists of a hydrocarbon solvent, water and a pore breaking agent, and the weight ratio of the hydrocarbon solvent to the water to the pore breaking agent is 1 (1.0-4.0) to 0.2-1.0.
Preferably, the hydrocarbon solvent is at least one of aromatic hydrocarbon, petroleum ether, naphtha and solvent oil.
Preferably, the hole breaking agent is at least one of alkali metal oxide, alkaline earth metal oxide, alkali metal hydroxide and alkaline earth metal hydroxide.
Preferably, the hole breaking agent is at least one of calcium oxide, magnesium oxide, potassium oxide, sodium oxide, caustic soda, potassium hydroxide, calcium hydroxide and magnesium hydroxide.
Further preferably, the weight ratio of the Fischer-Tropsch wax residue to the compound solvent is 1: 1-5.
Preferably, stirring is performed while the temperature is raised and maintained.
Preferably, the paraffin solution is treated by the following method: and standing and separating the paraffin solution to obtain an organic solvent phase and a water phase, and distilling and separating the organic solvent phase to obtain the paraffin.
Preferably, the organic solvent phase is separated from the paraffin wax, and the resulting solvent is used to prepare a complex solvent, while the aqueous phase is subjected to desalting treatment and then used to prepare a complex solvent.
Compared with the prior art, the invention has the following beneficial effects:
1) the method can complete the separation of paraffin and the passivation and inactivation of the catalyst in one step, reduce the technical process and equipment investment and reduce the cost.
2) The method of the invention is adopted to separate and recycle Fischer-Tropsch wax residue, and the recovery efficiency of paraffin is high and can reach more than 99%.
3) By adopting the method, the temperature of the combustible point of the catalyst after passivation and inactivation treatment is raised to be over 600 ℃, the potential risk of combustion is completely avoided, and the catalyst can be safely buried.
Detailed Description
The invention relates to a process for recovering paraffin from Fischer-Tropsch wax residue and simultaneously passivating and inactivating a catalyst by a one-step method, which comprises the steps of mixing Fischer-Tropsch wax residue with a compound solvent, heating to 100-250 ℃, keeping the temperature for 30-240 min, and then carrying out solid-liquid separation to obtain solid residue and a mixed solution; the obtained solid slag is a deactivated and inactivated catalyst, and the obtained mixed solution is a paraffin solution; wherein the compound solvent consists of a hydrocarbon solvent, water and a pore breaking agent, and the weight ratio of the hydrocarbon solvent to the water to the pore breaking agent is 1 (1.0-4.0) to 0.2-1.0.
According to the method, the specific compound solvent is adopted, paraffin separation and catalyst passivation and inactivation are completed in one step under the heating condition, the technological process and equipment investment are reduced, the temperature of a combustible point of the catalyst subjected to passivation and inactivation is increased to be more than 600 ℃, and the potential risk of combustion is completely avoided.
The compound solvent mainly comprises a hydrocarbon solvent and a water two-phase component, wherein a pore breaking agent is dissolved in the water phase. Preferably, in the compound solvent, the weight ratio of the hydrocarbon solvent, the water and the pore breaking agent is 1 (1.0-4.0) to 0.2-1.0.
Hydrocarbon solvents commonly used in the art are suitable for the present invention, and preferably, the hydrocarbon solvent is at least one of aromatic hydrocarbon, petroleum ether, naphtha and mineral spirit.
The Fischer-Tropsch catalyst is a porous substance, the surface of the Fischer-Tropsch catalyst is coated by paraffin, and the pore channels also contain a large amount of paraffin, so that if the paraffin in the pore channels is not separated, the recovery rate of the wax residue is low. Experimental tests show that if the pore canal penetrating agent is not added, under the optimized condition, the paraffin recovery rate of the extracting agent to the Fischer-Tropsch wax residue is not more than 85%. The inventor researches the permeation effect of the pore canal penetrating agent using fatty alcohol-polyoxyethylene ether and lauryl alcohol-polyoxyethylene ether in the early period, and after the pore canal penetrating agent is added, the recovery rate of the extracting agent to paraffin can be improved to more than 95%. However, when the amount of wax residue to be treated is large (tens of thousands of tons per year), the absolute loss amount of paraffin is still large. Therefore, the pore canal penetrant is used to replace pore canal destroying agent, and this can destroy the catalyst structure completely, so that paraffin is separated from deep pores of the catalyst and the paraffin recovering rate may reach at least 99%. Preferably, the hole breaking agent is at least one of alkali metal oxide, alkaline earth metal oxide, alkali metal hydroxide and alkaline earth metal hydroxide.
Preferably, the hole-breaking agent is at least one of calcium oxide, magnesium oxide, potassium oxide, sodium oxide, caustic soda, potassium hydroxide, calcium hydroxide and magnesium hydroxide.
Preferably, the water is distilled water or deionized water.
Preferably, the weight ratio of the Fischer-Tropsch wax residue to the compound solvent is 1 (1-5).
In the method of the present invention, stirring may or may not be performed at the time of temperature rise and heat preservation, and in order to enhance mass transfer, stirring at the time of temperature rise and heat preservation is preferable.
By adopting the method, the mixed solution after solid-liquid separation is the paraffin solution, the paraffin can be recovered from the mixed solution by adopting the existing method, and preferably, the following method is adopted for recovery treatment: and standing and separating the paraffin solution to obtain an organic solvent phase and a water phase, and distilling and separating the organic solvent phase to obtain the paraffin.
For resource recycling and cost saving, preferably, after the paraffin is separated from the organic solvent phase, the obtained solvent is used for preparing the compound solvent, and the water phase is used for preparing the compound solvent after desalting treatment.
The following examples are provided to further illustrate the embodiments of the present invention and are not intended to limit the scope of the present invention.
Example 1
(1) Placing the Fischer-Tropsch wax residue and a compound solvent in a hydrothermal reaction kettle according to the mass ratio of 1:1, heating to 100 ℃, and preserving heat for 240min, wherein the compound solvent consists of a hydrocarbon solvent, deionized water and a pore breaking agent, and the weight ratio of the hydrocarbon solvent to the deionized water to the pore breaking agent is 1:1.0: 0.2; the hydrocarbon solvent is petroleum ether, and the hole breaking agent is calcium oxide.
(2) And (2) sending the mixture obtained in the step (1) into liquid-solid separation equipment for separation to obtain a mixed solution and solid slag.
(3) And (3) sending the mixed solution obtained after the separation in the step (2) into a static separation device, separating the organic solvent from the upper part, and separating saturated liquid water from the lower part. The organic solvent enters a solvent recovery device, the solvent is distilled out and reused, and the crude paraffin product at the bottom of the distillation kettle is sent to a product storage tank or a subsequent deep processing device; the liquid water is subjected to desalting treatment and then returned for use.
The recovery efficiency of paraffin was determined by gravimetric method to be 99.2%.
The combustible temperature of the catalyst after surface passivation treatment is measured to be more than 800 ℃, and the catalyst can be sent to a landfill site for safe landfill.
Example 2
(1) Placing the Fischer-Tropsch wax residue and a compound solvent in a hydrothermal reaction kettle according to the mass ratio of 1:5, heating to 250 ℃, and keeping the temperature for 30min, wherein the compound solvent consists of a hydrocarbon solvent, deionized water and a pore breaking agent, and the weight ratio of the hydrocarbon solvent to the deionized water to the pore breaking agent is 1:4.0: 1.0; the hydrocarbon solvent is 120# solvent oil, and the hole breaking agent is potassium oxide.
(2) And (2) sending the mixture obtained in the step (1) into liquid-solid separation equipment for separation to obtain a mixed solution and solid slag.
(3) And (3) sending the mixed solution obtained after the separation in the step (2) into a static separation device, separating the organic solvent from the upper part, and separating saturated liquid water from the lower part. The organic solvent enters a solvent recovery device, the solvent is distilled out and reused, and the crude paraffin product at the bottom of the distillation kettle is sent to a product storage tank or a subsequent deep processing device; the liquid water is subjected to desalting treatment and then returned for use.
The recovery efficiency of paraffin was determined by gravimetric method to be 99.1%.
The combustible temperature of the catalyst after surface passivation treatment is measured to be more than 650 ℃, and the catalyst can be sent to a landfill site for safe landfill.
Example 3
(1) Placing the Fischer-Tropsch wax residue and a compound solvent in a hydrothermal reaction kettle according to the mass ratio of 1:2, heating to 150 ℃, and keeping the temperature for 200min, wherein the compound solvent consists of a hydrocarbon solvent, deionized water and a pore breaking agent, and the weight ratio of the hydrocarbon solvent to the deionized water to the pore breaking agent is 1:2: 0.5; the hydrocarbon solvent is toluene, and the hole breaking agent is sodium hydroxide.
(2) And (2) sending the mixture obtained in the step (1) into liquid-solid separation equipment for separation to obtain a mixed solution and solid slag.
(3) And (3) sending the mixed solution obtained after the separation in the step (2) into a static separation device, separating the organic solvent from the upper part, and separating saturated liquid water from the lower part. The organic solvent enters a solvent recovery device, the solvent is distilled out and reused, and the crude paraffin product at the bottom of the distillation kettle is sent to a product storage tank or a subsequent deep processing device; the liquid water is subjected to desalting treatment and then returned for use.
The recovery efficiency of paraffin was determined by gravimetric method to be 99.2%.
The combustible point temperature of the catalyst after surface passivation treatment is measured to be more than 700 ℃, and the catalyst can be sent to a landfill site for safe landfill.
Example 4
(1) Placing the Fischer-Tropsch wax residue and a compound solvent in a hydrothermal reaction kettle according to the mass ratio of 1:3, heating to 200 ℃, and keeping the temperature for 150min, wherein the compound solvent consists of a hydrocarbon solvent, deionized water and a pore breaking agent, and the weight ratio of the hydrocarbon solvent to the deionized water to the pore breaking agent is 1:3: 0.8; the hydrocarbon solvent is petroleum ether, and the hole breaking agent is calcium hydroxide.
(2) And (2) sending the mixture obtained in the step (1) into liquid-solid separation equipment for separation to obtain a mixed solution and solid slag.
(3) And (3) sending the mixed solution obtained after the separation in the step (2) into a static separation device, separating the organic solvent from the upper part, and separating saturated liquid water from the lower part. The organic solvent enters a solvent recovery device, the solvent is distilled out and reused, and the crude paraffin product at the bottom of the distillation kettle is sent to a product storage tank or a subsequent deep processing device; the liquid water is subjected to desalting treatment and then returned for use.
The recovery efficiency of paraffin was determined by gravimetric method to be 99.1%.
The combustible temperature of the catalyst after surface passivation treatment is measured to be more than 750 ℃, and the catalyst can be sent to a landfill site for safe landfill.
Example 5
(1) Placing the Fischer-Tropsch wax residue and a compound solvent in a hydrothermal reaction kettle according to the mass ratio of 1:4, heating to 200 ℃, and keeping the temperature for 180min, wherein the compound solvent consists of a hydrocarbon solvent, deionized water and a pore breaking agent, and the weight ratio of the hydrocarbon solvent to the deionized water to the pore breaking agent is 1:2.5: 0.4; the hydrocarbon solvent is petroleum ether, and the hole breaking agent is magnesium hydroxide.
(2) And (2) sending the mixture obtained in the step (1) into liquid-solid separation equipment for separation to obtain a mixed solution and solid slag.
(3) And (3) sending the mixed solution obtained after the separation in the step (2) into a static separation device, separating the organic solvent from the upper part, and separating saturated liquid water from the lower part. The organic solvent enters a solvent recovery device, the solvent is distilled out and reused, and the crude paraffin product at the bottom of the distillation kettle is sent to a product storage tank or a subsequent deep processing device; the liquid water is subjected to desalting treatment and then returned for use.
The recovery efficiency of paraffin was determined by gravimetric method to be 99.0%.
The combustible temperature of the catalyst after surface passivation treatment is measured to be more than 600 ℃, and the catalyst can be sent to a landfill site for safe landfill.
Claims (5)
1. The process for recovering paraffin from Fischer-Tropsch wax residue and simultaneously passivating and inactivating the catalyst by one-step method is characterized by comprising the following steps: mixing Fischer-Tropsch wax residue with a compound solvent, heating to 100-250 ℃, preserving heat for 30-240 min, and then carrying out solid-liquid separation to obtain solid residue and a mixed solution; the obtained solid slag is a deactivated and inactivated catalyst, and the obtained mixed solution is a paraffin solution; the composite solvent consists of a hydrocarbon solvent, water and a pore breaking agent, the weight ratio of the hydrocarbon solvent to the water to the pore breaking agent is 1 (1.0-4.0) to 0.2-1.0, and the weight ratio of the Fischer-Tropsch wax residue to the composite solvent is 1: 1-5; the hydrocarbon solvent is at least one of aromatic hydrocarbon, petroleum ether, naphtha and solvent oil; the hole breaking agent is at least one of alkali metal oxide, alkaline earth metal oxide, alkali metal hydroxide and alkaline earth metal hydroxide.
2. The one-step process for recovering paraffin wax from Fischer-Tropsch wax residue while deactivating a catalyst, as recited in claim 1, wherein: the hole breaking agent is at least one of calcium oxide, magnesium oxide, potassium oxide, sodium oxide, caustic soda, potassium hydroxide, calcium hydroxide and magnesium hydroxide.
3. The one-step process for recovering paraffin wax from Fischer-Tropsch wax residue while deactivating a catalyst, as recited in claim 1, wherein: heating and stirring while keeping the temperature.
4. The one-step process for recovering paraffin wax from Fischer-Tropsch wax residue while deactivating a catalyst, as recited in claim 1, wherein: the paraffin solution was treated as follows: and standing and separating the paraffin solution to obtain an organic solvent phase and a water phase, and distilling and separating the organic solvent phase to obtain the paraffin.
5. The one-step process for recovering paraffin wax from Fischer-Tropsch wax residue while deactivating a catalyst according to claim 4, wherein: after the organic solvent phase is separated to obtain paraffin, the obtained solvent is used for preparing a compound solvent, and the water phase is subjected to desalting treatment and then is used for preparing the compound solvent.
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| CN110355180A (en) * | 2019-07-02 | 2019-10-22 | 国家能源集团宁夏煤业有限责任公司 | Slag Lasaxing Oilfield method and system |
| CN112694914A (en) * | 2020-12-30 | 2021-04-23 | 国家能源集团宁夏煤业有限责任公司 | Recovery method and device for recovering wax from catalyst-containing wax residue |
Citations (4)
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| CN101380597A (en) * | 2008-10-23 | 2009-03-11 | 广州有色金属研究院 | Method for removing landification dead catalyst oiliness material |
| CN105498860A (en) * | 2016-01-30 | 2016-04-20 | 清华大学 | Method for deoiling oil-bearing waste catalyst |
| CN106902896A (en) * | 2017-01-18 | 2017-06-30 | 昆明理工大学 | A kind of method for removing aluminium scrap base hydrogenation catalyst surface oily substance |
| CN108704673A (en) * | 2018-05-31 | 2018-10-26 | 上海华畅环保设备发展有限公司 | Ebullated bed wood tar adds the de-oiling method and device of the outer waste discharge catalyst of hydrogen |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101380597A (en) * | 2008-10-23 | 2009-03-11 | 广州有色金属研究院 | Method for removing landification dead catalyst oiliness material |
| CN105498860A (en) * | 2016-01-30 | 2016-04-20 | 清华大学 | Method for deoiling oil-bearing waste catalyst |
| CN106902896A (en) * | 2017-01-18 | 2017-06-30 | 昆明理工大学 | A kind of method for removing aluminium scrap base hydrogenation catalyst surface oily substance |
| CN108704673A (en) * | 2018-05-31 | 2018-10-26 | 上海华畅环保设备发展有限公司 | Ebullated bed wood tar adds the de-oiling method and device of the outer waste discharge catalyst of hydrogen |
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