CN112707545A - Oil-water separation device and method for polymer resin liquid in C5 petroleum resin production - Google Patents
Oil-water separation device and method for polymer resin liquid in C5 petroleum resin production Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 120
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- VTIIJXUACCWYHX-UHFFFAOYSA-L disodium;carboxylatooxy carbonate Chemical compound [Na+].[Na+].[O-]C(=O)OOC([O-])=O VTIIJXUACCWYHX-UHFFFAOYSA-L 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/38—Treatment of water, waste water, or sewage by centrifugal separation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
- C02F2103/38—Polymers
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Cyclones (AREA)
Abstract
The utility model relates to a polymerization resin liquid oil-water separator and method in C5 petroleum resin production, provides a polymerization resin liquid oil-water separator in C5 petroleum resin production, and the device includes: the device comprises a pressure-bearing shell (2-5), and a cyclone separation device (2-3) and a fiber heterojunction device (2-2) which are arranged in the pressure-bearing shell (2-5), wherein the cyclone separation device (2-3) is arranged on a fixed frame, the fiber heterojunction device (2-2) is arranged in an overflow pipe of the cyclone separation device, or the fiber heterojunction forms an annular device and is arranged at the upper part of an outlet of the overflow pipe of the cyclone separation device. Also provides a method for separating oil from water in the polymerized resin liquid in the production of C5 petroleum resin.
Description
Technical Field
The utility model belongs to the technical field of polymerized resin liquid degree of depth oil-water separation in the chemical industry resin production process, a device that carries out whirl fibre heterojunction separation to polymerized resin liquid in the production of C5 petroleum resin is applicable to the colourity that reduces the petroleum resin product, improves the quality of petroleum resin product. Specifically, the invention provides a device and a method for deeply separating oil and water from polymerized resin liquid in C5 petroleum resin production.
Background
In the petrochemical industry, a low-molecular polymer prepared from ethylene by-products such as C5 and C9 fractions is usually prepared by a petroleum resin cracking method, and the average molecular weight of the low-molecular polymer is 300-3000. At present, petroleum resin products have been developed into a plurality of varieties, brands and widely applied functional synthetic resins with the production capacity of more than 90 million tons per year all over the world. The aliphatic C5 petroleum resin can be prepared by using an alkene mixture containing more piperylene in C5 fraction as a raw material, wherein the preparation process mainly comprises cationic catalysis and polymerization reaction. Aliphatic C5 petroleum resin can be prepared by using a mixture of dicyclopentadiene mainly contained in C5 fraction as a raw material, and the preparation process mainly adopts a thermal polymerization technology. The C5 petroleum resin takes an aliphatic hydrocarbon structure as a chain link, has the advantages of chemical resistance, ethanol corrosion resistance, water resistance, better miscibility, lower acidity and the like, has the characteristics of good viscosity regulation and thermal stability, low production cost and the like, and is widely applied to the industries of traffic paint, high-solid-content coating, tackifier, printing ink, papermaking, waterproof material preparation and the like. Among them, aliphatic C5 petroleum resin is drawing attention because of its excellent properties such as light color, good fluidity and adhesion, and good aging resistance.
China C5 petroleum resin is mainly applied to the industries of adhesives, paper sizing presses, coating additives and the like. The C5 petroleum resin technology in China is relatively laggard, the scale of a production device is smaller, the color of a product is darker, the thermal stability is poorer, the variety is single, and the application is greatly limited, so that the improvement of the quality and the quantity of the C5 petroleum resin product is very necessary. Various efforts have been made by researchers to address the problems involved.
The invention patent CN103772610B provides an oxidation decoloration refining method of C5/C9 petroleum resin, which adopts dark petroleum resin as raw material, hydrogen peroxide and sodium percarbonate as oxidant, the hydrogen peroxide reacts with melted petroleum resin, and substances which are easy to oxidize and contain unsaturated bonds such as double bonds and the like and affect the chroma in the petroleum resin are removed firstly; and then, adding excessive sodium carbonate to enhance the oxidative bleaching performance of hydrogen peroxide and further remove impurities which influence chromaticity in the resin to achieve the decolorizing effect, but the process has large medicine dosage and high cost.
The invention patent CN102453217B provides a petroleum resin hydrogenation and decoloration method, which comprises the steps of dissolving petroleum resin in an organic solvent to prepare a petroleum resin feed, mixing the petroleum resin feed with hydrogen, feeding the mixture into a fixed bed hydrogenation reactor for hydrogenation reaction, and separating the organic solvent from the obtained hydrogenation reaction product to obtain the hydrogenated petroleum resin. The method can effectively contain double bonds in sulfide and saturated petroleum resin in the petroleum resin through catalyst grading, so as to achieve the aim of decoloring the petroleum resin, but the catalyst required in the process is large in dosage and is easy to react insufficiently, so that the petroleum resin is not decolored completely.
The invention patent application CN201820721041.3 provides a petroleum resin polymer dehydration storage tank, wherein a water outlet is arranged at the bottom of the storage tank, a petroleum resin polymer outlet is arranged at the top of the storage tank, a three-section structure is arranged on an inlet pipeline of a raw material inlet along the flow direction, in order to reduce the turbulence and the flow speed of the raw material flow, the liquid level of the raw material in a granular dehydrating agent is gradually raised, and the dehydration is realized by controlling the flow speed of the raw material inlet and the petroleum resin polymer outlet. However, the granular dehydrating agents in the device are frequently replaced, and the dosage of the dehydrating agents is too large, so that the device is not suitable for long-term stable production work of large enterprises.
The patent application CN201921120052.7 provides a coalescence oil-water separation device, which comprises a separation cylinder, a lifting mechanism and a coalescence mechanism, wherein the coalescence mechanism is lifted up and down in a solution, so that an oil layer of liquid can be coalesced under the action of gravity through the coalescence action of the coalescence mechanism, when the coalescence mechanism rises above the liquid level, air floatation is formed under the action of three phases of water, oil and gas, the oil layer is separated to the upper layer, and an aqueous solution sinks to the lower layer, so that the separation structure can be effectively improved. But the device structure is comparatively complicated, dismantles the difficulty, and the difficult maintenance of fragile increases later stage running cost.
In summary, the problem of deep oil-water separation treatment of polymer resin liquid is urgently to be solved, and particularly, obtaining a low-chroma petroleum resin product is important. In order to solve the problem, a large number of patents adopt a hydrogenation and decoloration method, hydrogen is introduced when resin and a solvent are mixed, and hydrogenated petroleum resin is formed after cooling. Therefore, it is necessary to develop an efficient, economical and simple separation process to deeply separate oil from water in the polymerized resin liquid, reduce the amount of catalyst used in the process, further reduce the discharge of high-concentration wastewater, and achieve the purposes of reducing the content of catalyst, no chemical agent addition, and reducing the discharge of wastewater, thereby improving the quality of petroleum resin products.
Disclosure of Invention
The invention provides a novel device and a method for separating oil from water in polymerized resin liquid in C5 petroleum resin production, which realize the purposes of reducing the chroma of a resin product and improving the quality of the resin product by deeply separating the oil from the water in the polymerized resin liquid.
In one aspect, the present disclosure provides a polymerized resin liquid oil-water separator in the production of C5 petroleum resin, the apparatus comprising:
the device comprises a pressure-bearing shell, a cyclone separation device and a fiber heterojunction device, wherein the cyclone separation device and the fiber heterojunction device are arranged in the pressure-bearing shell;
the cyclone separation device is provided with an oil-water mixed phase inlet, a separated oil phase outlet, a separated water phase outlet, an oil-water mixed phase separation main body and a fixing frame for mounting the cyclone separation device;
the fiber heterojunction device is formed by blending hydrophilic and hydrophobic materials formed by combining a plurality of materials.
In a preferred embodiment, the pressure-containing housing is a cylindrical vessel.
In another preferred embodiment, the cyclone tube of the cyclone separation device and the fiber heterojunction device is made of corrosion-resistant material, and the heterojunction filter element is made of a combination of multiple materials including stainless steel and glass fiber.
In another preferred embodiment, the size of the cyclone separation device and the fiber heterojunction device is designed according to the treatment capacity, and a connection mode of combining a cyclone tube and a fiber heterojunction filter element is adopted.
In another preferred embodiment, the single throughput of the cyclone tube is 0.8m3/h-2.5m3H, connected together in parallel, and set according to throughputThe number of the cyclone tubes connected in parallel.
In another preferred embodiment, the polymeric resin liquid enters the cyclone separation device and the fiber heterojunction device through a conduit in a tangential direction, wherein due to the action of the cyclone field, a downward outer cyclone and an upward inner cyclone are formed in the cyclone cavity, so that the oil phase with low density enters the inner cyclone, oil drops collected enter the purified oil pipeline from the overflow cavity after being treated by the fiber heterojunction filter element from the overflow port of the cyclone pipe and then are conveyed to a subsequent unit, and oil-water separation is realized.
In another aspect, the present disclosure provides a method for separating oil from water in a polymer resin liquid in the production of C5 petroleum resin, the method comprising:
the polymerized resin liquid enters a cyclone separation device arranged in the pressure-bearing shell from an inlet of the pressure-bearing shell to primarily separate oil and water, a separated water phase flows out from a bottom flow port of the cyclone separation device and flows out from a bottom outlet of the pressure-bearing shell, a separated oil phase flows to a fiber heterojunction device from an overflow port of the cyclone separation device and then flows out from an upper outlet of the pressure-bearing shell, micro water drops in the oil-water mixture are intercepted by the fiber heterojunction and coalesced into larger water drops, and the coalesced water drops sink to a water accumulation groove on the side face of the pressure-bearing shell under the action of gravity and are discharged from a water outlet.
In a preferred embodiment, the water content in the oligomer mixed solution at the inlet of the fiber heterojunction device is less than or equal to 2000ppm, and the viscosity of the mixed solution is less than or equal to 15 cp.
In another preferred embodiment, the polymeric resin fluid has an outlet moisture content of 15ppm or less and a pressure drop loss of 0.1MPa or less after being processed through the fiber heterojunction device.
Has the advantages that:
1) the cyclone fiber heterojunction device is utilized to realize cyclone coalescence integration, no component is arranged in the cyclone, the structure is simple, the pressure drop loss is less than or equal to 0.1MPa, the dehydration efficiency reaches more than 95 percent, and the deep and efficient separation of oil and water is realized.
2) The invention utilizes the rotational flow fiber heterojunction device to realize oil-water separation on the basis of not adding other chemical agents, reduces the consumption of the catalyst by more than 85 percent and saves the cost.
3) The equipment provided by the invention has the advantages of simple structure, easiness in operation, modular structure and easiness in maintenance, wherein the adopted cyclone separation device is in a parallel connection mode, the number of parallel pipes can be changed according to the treatment capacity, and the change of the treatment capacity can be flexibly coped with.
4) The invention utilizes the rotational flow fiber heterojunction device to realize that the water content in the petroleum resin product is less than or equal to 20ppm, and the low-chroma and high-purity petroleum resin product is obtained.
Drawings
The accompanying drawings are included to provide a further understanding of the disclosure, and are incorporated in and constitute a part of this specification to further illustrate the disclosure and not limit the disclosure.
FIG. 1 is a schematic view of the overall process flow of the method for deep oil-water separation of polymerized resin liquid in the production process of C5 petroleum resin according to one preferred embodiment of the present disclosure.
FIG. 2 is a schematic diagram of a C5 feedstock cyclone integrated oil-water separation plant according to a preferred embodiment of the present disclosure.
Fig. 3 is a schematic diagram of the separation principle of a cyclonic fiber heterojunction device according to a preferred embodiment of the present disclosure.
Detailed Description
After extensive and intensive research, the inventor of the application finds that for the problems of product quality reduction and the like caused by high water content of polymerized resin liquid in the production process of C5 petroleum resin, the adoption of the cyclone fiber heterojunction device can realize high-efficiency and low-consumption oil-water separation, and solves the problems of large using amount of the existing catalyst, poor dehydration and decoloration effects, large discharge amount of high-concentration wastewater, high cost, complex operation and the like, thereby developing the oil-water separation equipment with high efficiency, low consumption, stable operation and easy management.
The technical concept of the invention is as follows:
raw material C5, circulating polymerization liquid and catalyst (AlCl)3) Conveying the mixture to a polymerization kettle through a pipeline for reaction to obtain a polymerization solution after the reaction, wherein one part of the polymerization solution is used as a circulating polymerization solution, the other part of the polymerization solution is used as a mixed solution and flows into a neutralization kettle to perform a neutralization reaction with injected dilute alkali solution, and the polymerization solution after the neutralization reactionAfter heat exchange, carrying out preliminary oil-water separation in a standing layering tank, treating the separated sewage in a plant sewage treatment system, separating the dewatered polymeric resin liquid in a cyclone cavity by cyclone, trapping a small amount of oil in a water phase through an oleophylic hydrophobic fiber heterojunction formed by combining multiple materials, and allowing the water separated from the oil phase to flow out from a bottom flow port of a cyclone pipe to obtain a crude petroleum resin liquid with low water content;
and (3) allowing the crude resin liquid to enter a stripping tower, stripping and extracting oligomers in the material through superheated steam, allowing the oligomers to enter a cyclone fiber heterojunction device, and separating the free dispersed oil, the suspended oil and the emulsified oil quickly and efficiently by adopting a cyclone combined fiber heterojunction technology to obtain a high-purity petroleum resin product.
In a first aspect of the present disclosure, there is provided a polymeric resin liquid oil-water separation device in C5 petroleum resin production, the device comprising:
the device comprises a pressure-bearing shell, a cyclone separation device and a fiber heterojunction device, wherein the cyclone separation device and the fiber heterojunction device are arranged in the shell;
the cyclone separation device is provided with an oil-water mixed phase inlet, a separated oil phase outlet, a separated water phase outlet, an oil-water mixed phase separation main body and a fixing frame for mounting the cyclone separation device;
the fiber heterojunction device is formed by mixing and weaving hydrophilic and hydrophobic materials formed by combining a plurality of materials, and is arranged in the overflow pipe of the cyclone separation device.
In the present disclosure, the pressure-bearing housing is a cylindrical vessel.
In the disclosure, the cyclone tube of the cyclone separation device and the fiber heterojunction device is made of corrosion-resistant material, and the heterojunction filter element is made of stainless steel, glass fiber and other materials.
In the present disclosure, the size of the cyclone separation device and the fiber heterojunction device is designed according to the treatment capacity, and a connection mode of combining the cyclone tube with the fiber heterojunction filter element is adopted.
In the present disclosure, the single throughput of swirl tubes is 0.8m3/h-2.5m3And h, connecting the cyclone tubes together in a parallel mode, and setting the parallel number of the cyclone tubes according to the treatment capacity.
In this disclosure, polymeric resin liquid gets into hydrocyclone separation device and fibre heterojunction device through the pipe tangential of special construction, because the effect in whirl field forms decurrent outer whirl and ascending interior whirl in the whirl intracavity for oil phase that density is little gets into interior whirl, assembles oil and drips and gets into by the overflow chamber after the fiber heterojunction filter core is handled from whirl pipe overflow mouth and purify the oil pipeline and carry to follow-up unit, realizes the oil-water deep separation.
In the present disclosure, the cyclone separator and the fiber heterojunction device separate the water phase in the polymerized resin liquid by using the rotation and revolution cyclone, so that the oil and water are deeply separated to obtain the crude petroleum resin with low water content.
In the disclosure, the cyclone separator and the fiber heterojunction device separate the dispersed oil, the suspended oil and the emulsified oil in a free state rapidly and efficiently by using the self-revolution and revolution cyclone separation oligomer mixed liquid.
In the present disclosure, the fiber heterojunction device may be installed inside the overflow pipe of the cyclone separation device to save the cavity space; or the fiber heterojunction can be combined into an annular device which is arranged at the upper part of the outlet of the overflow pipe of the cyclone separation device.
In a second aspect of the present disclosure, there is provided a method for separating oil from water in a polymeric resin liquid in the production of C5 petroleum resin, the method comprising:
the water-containing resin enters the cyclone separation device from the inlet at a certain tangential speed, the water-containing resin primarily separates oil and water in a cavity of the cyclone separation device under the self-revolution and revolution coupling effects of a cyclone field and the cyclone separation device, the separated water phase flows out from a bottom flow port of the cyclone separation device and flows out from an outlet of the cavity, the separated oil phase flows to the fiber heterojunction device from an overflow port of the cyclone separation device, due to the hydrophilicity and hydrophobicity of the material of the fiber heterojunction, the oil phase flows out from an outlet at the upper part of the cavity through the fiber heterojunction, micro water drops in the oil-water mixture are intercepted by the fiber heterojunction and coalesced into larger water drops, and the coalesced water drops sink to a water accumulation groove at the side under the action of gravity and are discharged from a water outlet.
In the disclosure, the water content in the oligomer mixed liquor at the inlet of the cyclone separator is less than or equal to 2000ppm, and the viscosity of the mixed liquor is less than or equal to 15 cp.
In the present disclosure, after the polymeric resin liquid is subjected to cyclone separation by the cyclone separator and the fiber heterojunction device, the outlet water content is less than or equal to 15ppm, the pressure drop loss is less than or equal to 0.1MPa, and the polymeric resin liquid can stably operate for a long time.
Reference is made to the accompanying drawings.
FIG. 1 is a schematic view of the overall process flow of the method for deep oil-water separation of polymerized resin liquid in the production process of C5 petroleum resin according to one preferred embodiment of the present disclosure. As shown in FIG. 1, a raw material C5, a recycled polymerization liquid (polymer), and a catalyst (AlCl)3) Conveying the mixture into a polymerization kettle 1-1 through a pipeline for reaction, circulating the mixed liquor after the reaction to a heat exchanger 1-2 for heat exchange and recycling through a pump respectively, or flowing into a neutralization kettle 1-3 for neutralization reaction with injected dilute alkali liquor, allowing the polymer solution after the neutralization reaction to enter a standing layering tank 1-5 for primary oil-water separation after heat exchange in the heat exchanger 1-4, allowing the separated sewage to enter a plant sewage treatment system for treatment, adding condensate into the dewatered polymer resin solution, allowing the dewatered polymer resin solution to enter a cyclone fiber heterojunction device 1-6 for cyclone separation, allowing the separated water to enter the plant sewage treatment system for treatment, allowing the dewatered polymer resin solution to enter a settling tank 1-7 for settling to obtain crude petroleum resin solution with low water content, allowing the crude resin solution to enter a stripping tower 1-8, and stripping oligomers in the materials through superheated steam to extract oligomers, and then the oligomer mixture enters a cyclone fiber heterojunction device 1-10 after heat exchange in a heat exchanger 1-9, and free dispersed oil, suspended oil and emulsified oil are quickly and efficiently separated through the cyclone fiber heterojunction device to obtain a high-purity petroleum resin product.
FIG. 2 is a schematic diagram of a C5 feedstock cyclone integrated oil-water separation plant according to a preferred embodiment of the present disclosure. As shown in a in figure 2, a polymerized resin liquid enters a middle feeding cavity of a cyclone separation device 2-3 from an inlet 2-1 of a pressure-bearing shell 2-5 and then tangentially enters a cyclone tube through a conduit with a special structure, pre-dehydration is completed under the action of a cyclone field, the obtained oil phase is subjected to deep dehydration through a fiber heterojunction filter element of a fiber heterojunction device 2-2, the obtained crude petroleum resin liquid flows out from an upper outlet 2-6, the dehydrated water flows out from a bottom outlet 2-4 and then enters a plant sewage treatment system for treatment, micro water drops in the oil-water mixture are intercepted by the fiber heterojunction and coalesced into larger water drops, and the coalesced water drops sink to a water collecting tank on the side surface of the pressure-bearing shell under the action of gravity and are discharged from a water outlet 2-7. As shown in b in fig. 2, the oligomer mixture enters the cyclone tube from the inlet 2-8, the pre-dehydration is completed under the action of the cyclone field, the oil phase is deeply dehydrated through the fiber heterojunction filter element 2-9, the obtained oligomer flows out from the overflow port 2-10, and the dehydrated water flows out from the underflow port 2-11 and then enters the plant sewage treatment system for treatment.
Fig. 3 is a schematic diagram of the separation principle of a cyclonic fiber heterojunction device according to a preferred embodiment of the present disclosure. As shown in figure 3, the polymer resin liquid is pumped into the cyclone separator through an inlet 3-1, under the action of the cyclone field, the water phase with high density moves downwards along the axial direction, moves outwards along the radial direction, moves downwards along the wall when reaching the cone section and is discharged from a bottom flow port 3-2 to form an outer cyclone; the oil with low density moves towards the direction of the central axis, forms an upward internal rotational flow at the center of the axis and is discharged from the middle part 3-3 of the overflow port; as shown in an enlarged fiber heterojunction filter element, the water-containing oil phase flows through the fiber heterojunction filter element formed by weaving the oleophilic hydrophobic material and the hydrophilic oleophobic material through the inlet 3-4, the oil in the water-containing oil phase is agglomerated and enlarged through the fiber heterojunction filter element and is discharged from the top 3-5 of an overflow port, and the water in the water-containing oil phase is agglomerated into large drops by small drops and is finally discharged from the outlet 3-6 of the deeply dehydrated water phase.
Examples
The invention is further illustrated below with reference to specific examples. It is to be understood, however, that these examples are illustrative only and are not to be construed as limiting the scope of the present invention. Test methods in which specific conditions are not specified in the following examples are generally carried out under conventional conditions or under conditions recommended by the manufacturer. All percentages and parts are by weight unless otherwise indicated.
Example 1:
in the production process of the C5 petroleum resin of 11 ten thousand tons/year, according to the method of the invention, a rotational flow fiber heterojunction device is adopted to carry out deep oil-water separation treatment on the polymerized petroleum resin liquid, and the specific operation process and effect are described as follows:
1. material Properties and associated parameters
The polymer liquid to be treated in the production of petroleum resin is a liquid-liquid two-phase mixture, wherein the impurities are free dispersion water, suspension water and emulsion water, the viscosity of the polymer liquid is 5cp, the temperature is 85 ℃, the pressure is 0.6MPa, and the density is 920kg/m3The weight of the water phase accounts for 10 percent, the viscosity is 1cp, and the treatment capacity is 8-25 t/h.
2. Polymeric resin liquid cyclone fiber heterojunction device
The device adopts a cyclone tube combined fiber heterojunction filter element mode, selects 10 cyclone tubes for parallel treatment and is in a vertical state, wherein the size of the cyclone tube is DN35 (the diameter is 35mm), the specification is HL/L (liquid-liquid) 35, and the treatment capacity of a single cyclone tube is 0.8-2.5m3/h。
The coalescence separation adopts the specification of
The 10 fiber heterojunction filter element is made of phenolic resin modified superfine glass fiber cotton felt.
3. Carrying out the process
Raw material C5, circulating polymerization liquid and catalyst (AlCl)3) Conveying the mixture into a polymerization kettle through a pipeline for reaction to obtain a polymerization solution after reaction, wherein one part of the polymerization solution is used as a circulating polymerization solution, the other part of the polymerization solution is used as a mixed solution and is circulated to a heat exchanger for heat exchange and recycling through a pump or flows into a neutralization kettle to perform neutralization reaction with injected dilute alkali liquor, the polymerization solution after the neutralization reaction enters a standing layering tank for preliminary oil-water separation after heat exchange through the heat exchanger, the separated sewage enters a plant sewage treatment system for treatment, the dehydrated polymerization resin solution enters a cyclone fiber heterojunction device, pre-dehydration is firstly completed under the action of a cyclone field, and an oil phase is obtained and then subjected to multiple kinds of oil-water separationThe oleophylic hydrophobic fiber heterojunction filter element formed by combining the materials is subjected to deep oil-water separation, then is settled in a settling tank to obtain crude petroleum resin with low water content, and enters a purified oil pipeline to be conveyed to a subsequent unit.
4. Analysis of results
After deep oil-water separation by the cyclone fiber heterojunction device, dispersed water, suspended water and emulsified water in the oil phase are discharged as sewage through a bottom flow port of the cyclone separator, and the rest high-purity oil phase is conveyed to a subsequent unit. The water content of the petroleum resin product after deep water-oil separation treatment of the cyclone fiber heterojunction device is lower than 20 ppm; the catalyst consumption is reduced by more than 85%, the generation amount of alkaline wastewater is reduced by more than 85%, and the pressure drop loss of the cyclone separator is less than 0.1MPa, so that the low-energy-consumption long-period continuous operation is realized, and the dehydration efficiency reaches more than 90%.
Example 2:
in the production process of the C5 petroleum resin of 11 ten thousand tons/year, according to the method of the invention, a rotational flow fiber heterojunction device is adopted to carry out deep oil-water separation treatment on oligomer mixed liquor, and the specific operation process and effect are described as follows:
1. material Properties and associated parameters
The polymer liquid to be treated in the production of petroleum resin is a liquid-liquid two-phase mixture, wherein the impurities are free dispersion water, suspension water and emulsion water, the viscosity of the polymer liquid is 2cp, the temperature is 60 ℃, the pressure is 0.4MPa, and the density is 960kg/m3The weight ratio of the water phase is 70%, the viscosity is 1cp, and the treatment capacity is 2 t/h.
2. Oligomer rotational flow fiber heterojunction device
The device adopts a cyclone tube combined fiber heterojunction filter element mode, 1 cyclone tube is selected for treatment, wherein the size of the cyclone tube is DN35, and the treatment capacity of a single cyclone tube is 0.8-2.5m3/h。
The coalescence separation adopts the specification of
The 1 fiber heterojunction filter element is made of phenolic resin modified superfine glass fiber cotton felt.
3. Carrying out the process
And the crude resin liquid enters a stripping tower, the oligomer in the material is extracted through superheated steam stripping, then the oligomer mixture enters a rotational flow fiber heterojunction device after heat exchange of a heat exchanger, and the mixed liquid is treated by using a rotational flow combined fiber heterojunction technology. The oligomer tangentially enters the cyclone tube, pre-dehydration is completed under the action of the cyclone field, the oil phase is deeply dehydrated through the fiber heterojunction filter element, the oil phase flows out of the overflow port, and the water phase flows out of the underflow port and then enters a factory sewage treatment system for treatment, so that deep oil-water separation is realized, and a high-purity petroleum resin product is obtained.
4. Analysis of results
After deep oil-water separation by the cyclone fiber heterojunction device, the dispersed water, the suspended water and the emulsified water in the oil phase are discharged as sewage through a bottom flow port of the cyclone separator, and the water content of the oligomer after deep oil-water separation treatment by the cyclone fiber heterojunction device is lower than 20 ppm; the catalyst consumption is reduced by more than 85 percent; the pressure drop loss of the cyclone separator is less than 0.1MPa, so that the low-energy-consumption long-period continuous operation is realized, and the dehydration efficiency reaches more than 95%.
The above-listed embodiments are merely preferred embodiments of the present disclosure, and are not intended to limit the scope of the present disclosure. That is, all equivalent changes and modifications made according to the contents of the claims of the present application should be considered to be within the technical scope of the present disclosure.
All documents referred to in this disclosure are incorporated by reference into this application as if each were individually incorporated by reference. Furthermore, it should be understood that various changes or modifications to the disclosure may be made by those skilled in the art after reading the above teachings of the disclosure, and such equivalents may fall within the scope of the disclosure as defined by the appended claims.
Claims (9)
1. A polymerized resin liquid oil-water separation device in C5 petroleum resin production, which comprises:
the device comprises a pressure-bearing shell (2-5), and a cyclone separation device (2-3) and a fiber heterojunction device (2-2) which are arranged in the pressure-bearing shell (2-5), wherein the cyclone separation device (2-3) is arranged on a fixed frame, the fiber heterojunction device (2-2) is arranged in an overflow pipe of the cyclone separation device, or the fiber heterojunction forms an annular device and is arranged at the upper part of an outlet of the overflow pipe of the cyclone separation device;
the cyclone separation device (2-3) is provided with an oil-water mixed phase inlet, a separated oil phase outlet, a separated water phase outlet, an oil-water mixed phase separation main body and a fixing frame for mounting the cyclone separation device;
the fiber heterojunction device (2-2) is formed by blending hydrophilic and hydrophobic materials formed by combining a plurality of materials.
2. The apparatus according to claim 1, characterized in that said pressurized casing (2-5) is a cylindrical container.
3. The apparatus of claim 1, wherein the cyclone tube of the cyclone separation device and the fiber heterojunction device is made of corrosion resistant material, and the heterojunction filter element is made of a combination of materials including stainless steel and glass fiber.
4. The apparatus of claim 1, wherein the cyclonic separation apparatus and the fiber heterojunction device are sized for throughput and are connected by a cyclone tube in combination with a fiber heterojunction filter element.
5. The apparatus of claim 4, wherein the swirl tube has a single throughput of 0.8m3/h-2.5m3And h, the cyclone tubes are connected together in a parallel mode, and the parallel number of the cyclone tubes can be set according to the treatment capacity.
6. The apparatus of claim 1, wherein the polymeric resin liquid enters the cyclone separator tangentially through the conduit, wherein due to the action of the cyclone field, a downward outer cyclone and an upward inner cyclone are formed in the cyclone chamber, so that the oil phase with low density enters the inner cyclone, and the oil droplets collected enter the purified oil pipeline from the overflow port of the cyclone pipe after being treated by the fiber heterojunction filter element and then are conveyed to the subsequent unit through the overflow chamber, thereby realizing oil-water separation.
7. A method for separating oil from water in polymerized resin liquid in the production of C5 petroleum resin comprises the following steps:
the polymerized resin liquid enters a cyclone separation device (2-3) arranged in the pressure-bearing shell (2-5) from an inlet (2-1) of the pressure-bearing shell (2-5) to carry out primary separation on oil and water, a separated water phase flows out from a bottom flow port of the cyclone separation device (2-3), and the oil phase after separation flows to a fiber heterojunction device (2-2) from an overflow port of a cyclone separation device (2-3) and flows out from an upper outlet (2-6) of the pressure-bearing shell (2-5) after being treated by the fiber heterojunction device (2-2), tiny water drops in the oil-water mixture are intercepted by the fiber heterojunction and are coalesced into larger water drops, and the coalesced water drops sink to a water accumulation groove on the side surface of the pressure-bearing shell (2-5) under the action of gravity and are discharged from a water discharge port (2-7).
8. The method of claim 7, wherein the water content of the oligomer mixture at the inlet of the fiber heterojunction device (2-2) is less than or equal to 2000ppm and the viscosity of the mixture is less than or equal to 15 cp.
9. The method of claim 8, wherein said polymeric resin liquid after being treated by said fiber heterojunction device (2-2) has an outlet moisture content of 15ppm or less and a pressure drop loss of 0.1MPa or less.
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| CN115557631A (en) * | 2022-09-15 | 2023-01-03 | 华东理工大学 | Oil-water separation device and method integrating cyclone, air flotation and medium coalescence |
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