CN109879716B - Device and method for fine desulfurization of isoprene - Google Patents
Device and method for fine desulfurization of isoprene Download PDFInfo
- Publication number
- CN109879716B CN109879716B CN201910210960.3A CN201910210960A CN109879716B CN 109879716 B CN109879716 B CN 109879716B CN 201910210960 A CN201910210960 A CN 201910210960A CN 109879716 B CN109879716 B CN 109879716B
- Authority
- CN
- China
- Prior art keywords
- isoprene
- desulfurization
- sulfur
- outlet
- distillation tower
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Abstract
The invention discloses a device and a method for accurately desulfurizing isoprene, wherein the device for accurately desulfurizing isoprene comprises a desulfurization separation tank, the desulfurization separation tank is connected with the outlet end of a desalting water pipe, the outlet at the bottom of the desulfurization separation tank is connected with the inlet of a distillation tower through an isoprene heat exchanger, the outlet at the top of the distillation tower is connected with the inlet of a low-sulfur isoprene cooler through the isoprene heat exchanger, the outlet of the low-sulfur isoprene cooler is connected with the inlet of a product tank, the outlet at the bottom of the distillation tower is respectively connected with the inlet of a reboiler and the inlet of a sulfur-containing waste liquid cooler through circulating liquid pipes, and the outlet of the reboiler is connected with the lower side port of the distillation tower. The isoprene obtained by the device and the method for accurately desulfurizing the isoprene is a high-quality isoprene product with the total sulfur content of not more than 5 mu g/g, the total nitrogen content of not more than 2 mu g/g and the total water content of less than 200 mu g/g, and the device and the method have the advantages of short process, low device investment and low desulfurization cost.
Description
Technical Field
The invention relates to the technical field of isoprene fine desulfurization, in particular to a device and a method for isoprene fine desulfurization.
Background
The ethylene cracking device by-product carbon five has complex composition, not only contains alkanes, mono-olefins, dienes, alkynes and cyclohydrocarbons, has a plurality of isomers, but also contains a small amount of C4 and C6 components and dicyclopentadiene, wherein the content of isoprene accounts for about 60 percent of the total amount.
At present, domestic cracking carbon five is mainly used as a raw material for producing fine chemical products such as hydrogenated resin, isoprene rubber, styrene-isoprene-styrene block copolymer (SIS), polydicyclopentadiene (PDCPD), cycloolefin copolymer, unsaturated polyester resin, petroleum resin and the like, but a lot of research work is urgently needed to be perfected in the aspects of high-end production and customization of the products so as to further improve the added value of the cracking carbon five and improve the competitiveness of domestic fine chemical products in the international market.
Because the sulfur content of the raw materials is not strictly controlled by the conventional ethylene cracking device, the fluctuation of the content of the byproduct cracking carbon five sulfur is large, the total sulfur content of the byproduct cracking carbon five of some devices is about 30 mug/g, and the total sulfur content of some devices is as high as 200 mug/g. If isoprene is used as a raw material for high-end carbon-five petroleum resin, isoprene rubber or SIS, it is required that the total sulfur of isoprene is not more than 5. mu.g/g.
According to sulfur form detection research, the sulfur form in the cracked carbon five-rectified high-purity isoprene product is mainly carbon disulfide, and the carbon disulfide has almost no removal effect by adopting conventional amine liquid extraction and alkali liquor extraction technologies. The prior mature technologies comprise a hydrodesulfurization method and an adsorbent desulfurization method, but the former method has the advantages of large device investment, high desulfurization cost, wide sulfur form adaptability and high desulfurization precision; the investment of the latter device is relatively small, but the sulfur capacity of the adsorbent is small, the adsorbent needs to be regenerated periodically, the regeneration operation of the adsorbent is complicated, and the desulfurization cost is increased.
Disclosure of Invention
In view of the above technical problems in the related art, the present invention provides an apparatus and a method for fine desulfurization of isoprene, which can overcome the above disadvantages in the prior art.
In order to achieve the technical purpose, the technical scheme of the invention is realized as follows:
the device for accurately desulfurizing the isoprene comprises a desulfurization separation tank, wherein the top of the desulfurization separation tank is connected with the outlet end of a desalting water pipe, the bottom outlet of the desulfurization separation tank is connected with the inlet of a distillation tower through an isoprene heat exchanger, the top outlet of the distillation tower is connected with the inlet of a low-sulfur isoprene cooler through the isoprene heat exchanger, the outlet of the low-sulfur isoprene cooler is connected with the inlet of a product tank, the top outlet of the product tank is connected with a non-condensing gas pipe, and the bottom outlet of the product tank is connected with a product pipe through a product pump; the bottom outlet of the distillation tower is respectively connected with the inlet of a reboiler and the inlet of a sulfur-containing waste liquid cooler through a circulating liquid pipe, the outlet of the reboiler is connected with the lower side port of the distillation tower, and the outlet of the sulfur-containing waste liquid cooler is connected with the sulfur-containing waste liquid pipe;
desulfurization knockout drum both ends are equipped with desulfurization reactor and baffle respectively, desulfurization reactor passes through the flange and is connected with the desulfurization knockout drum, the baffle with the bottom inner wall fixed connection of desulfurization knockout drum, the inside special filler that is equipped with of desulfurization reactor, special filler hangs in desulfurization reactor through the link, desulfurization reactor upper portion is equipped with liquid distributor, liquid distributor's material import passes through the mixture exit linkage of flange and whirl blender, whirl blender's main material access connection contains the sulphur isoprene pipe, whirl blender's vice material access connection fine desulfurization agent pipe.
Furthermore, the height of the partition board is 60-80% of the diameter of the desulphurization separation tank, the outlet end of the desalting water pipe and the desulphurization reactor are respectively positioned at two sides of the partition board, and the outlet at the bottom of the desulphurization separation tank and the outlet end of the desalting water pipe are positioned at the same side of the partition board.
Furthermore, trays are arranged in the distillation tower, and the number of the trays in the distillation tower is 5-10.
Furthermore, the liquid distributor comprises communicated tubes transversely distributed in the desulfurization reactor, and small holes are formed in the tubes and are uniformly distributed on the tubes.
Further, the special filler is a stainless steel micro-filament bundle, the stainless steel micro-filament bundle is composed of stainless steel micro-filaments with the diameter of 0.05-0.15mm, the stainless steel micro-filaments are in a continuous S-shaped corrugated shape, and the length of the stainless steel micro-filament bundle is 3-6 m.
According to another aspect of the present invention, there is provided a method for fine desulfurization of isoprene, the method comprising the steps of:
1) and (3) enabling sulfur-containing isoprene and a fine desulfurizer to enter a liquid cyclone mixer through a sulfur-containing isoprene pipe and a fine desulfurizer pipe respectively to form a mixture, enabling the mixture to be uniformly distributed on the cross section of a special filler in a desulfurization reactor through a liquid distributor for desulfurization, injecting trace demineralized water into a desulfurization separation tank through a demineralized water pipe, dissolving a desulfurization product, and obtaining the desulfurized mixture.
2) Outputting the desulfurized mixture from a bottom outlet of the desulfurization separation tank, exchanging heat through a heat exchanger, then feeding the mixture into a distillation tower, controlling the operating pressure of the distillation tower and the temperatures of the bottom and the top of the distillation tower, evaporating low-sulfur isoprene in the desulfurized mixture from a top outlet of the distillation tower, exchanging heat through the heat exchanger, and then feeding the mixture into a low-sulfur isoprene cooler for cooling to obtain an isoprene product; and (4) forming high-sulfur waste liquid by other components in the desulfurized mixture, and discharging the high-sulfur waste liquid after cooling by a sulfur-containing waste liquid cooler.
Further: in the desulfurization separation tank, the retention time of the mixture in the step 1) on the side of the partition plate provided with the desulfurization reactor is 0.5-2 hours, and the retention time of the mixture in the step 1) on the side of the partition plate provided with the desalting water pipe is 5-15 minutes.
Further, the fine desulfurizer in the step 1) is prepared from 40-70wt% of primary amine, 20-50wt% of secondary amine, 3-7wt% of nonionic surfactant, 2-5wt% of amphoteric surfactant and 1-3wt% of scorch retarder, wherein the primary amine is one or more of monoethanolamine, diglycolamine and ethylenediamine, the secondary amine is one or more of diethanolamine, diisoethanolamine and N-monomethyl ethanolamine, the nonionic surfactant is one or more of alkylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, octanol secondary polyoxyethylene ether and coconut diethanolamide, the amphoteric surfactant is prepared by mixing tetradecyl betaine and tertiary ammonium oxide OB-2 according to the mass ratio of 1: 1-2: 1, and the scorch retarder is N-nitrosodiphenylamine, OB-2, and the fine desulfurizer is prepared from the mixture of N-nitrosodiphenylamine and OB-2, One or more of N-cyclohexyl thiophthalimide, polyisobutylene succinimide and polyisobutylene polyamine.
Further, the preparation method of the fine desulfurizing agent comprises the steps of uniformly stirring tetradecyl betaine and tertiary ammonium oxide OB-2 according to a proportion at normal temperature to obtain an amphoteric surfactant, mixing primary amine, secondary amine, a nonionic surfactant, the amphoteric surfactant and a scorch retarder according to a proportion, stirring at the temperature of 40-50 ℃, stirring in a forward direction for 0.5 hour, then stirring in a reverse direction for 0.5 hour, and alternating for multiple times, wherein the total stirring time is more than or equal to 2 hours, and standing for 0.5-1 hour after stirring to obtain the fine desulfurizing agent.
Further, the addition amount of the fine desulfurizing agent in the step 1) is 0.02-0.1% of the mass of the isoprene, the reaction temperature is 20-50 ℃, the operation pressure is the pressure for ensuring that the isoprene is in a liquid phase and can be pumped to a distillation tower, the mass of the injected desalted water is 0.05-0.2% of the mass of the isoprene material, and the desalted water is one or more of softened water, deionized water and steam condensate water; in the step 2), the operation pressure at the top of the distillation tower is 0.1-0.2MPa, the temperature at the bottom of the distillation tower is 60-80 ℃, and the temperature at the top of the distillation tower is 50-70 ℃.
The invention has the beneficial effects that:
the isoprene obtained by the device and the method for fine desulfurization of isoprene is a high-quality isoprene product with the total sulfur content of not more than 5 mug/g, the total nitrogen content of not more than 2 mug/g and the total water content of less than 200 mug/g;
the organic amine in the fine desulfurizing agent is a direct reactant for removing carbon disulfide in isoprene, the non-ionic surfactant and the amphoteric surfactant can effectively improve the solubility of the organic amine and the isoprene and accelerate the reaction speed, the amphoteric surfactant can obviously improve the intersolubility of a desulfurization product and water, and the anti-coking agent can effectively reduce coking of the desulfurization product and an isoprene self-polymer in a reboiler and at the bottom of a distillation tower;
the process is simple and short, the investment of the device is saved, the desulphurization cost is low, and the desulphurization product, the unreacted desulfurizer and a small amount of heavy components in the raw materials form sulfur-containing waste liquid which can be sent to an incinerator or a boiler for incineration treatment.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a schematic structural diagram of an apparatus for fine desulfurization of isoprene according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of a hydrocyclone;
FIG. 3 is a schematic diagram of a liquid distributor;
FIG. 4 is a schematic structural view of a proprietary filler;
in the figure: 1. the device comprises a desulfurization reactor, 2, a cyclone liquid mixer, 3, a liquid distributor, 4, special packing, 5, a desulfurization separation tank, 6, a partition plate, 7, an isoprene heat exchanger, 8, a distillation tower, 9, a tray, 10, a low-sulfur isoprene cooler, 11, a product tank, 12, a product pump, 13, a reboiler, 14, a sulfur-containing waste liquid cooler, 21, a sulfur-containing isoprene pipe, 22, a fine desulfurizing agent pipe, 23, a desalted water pipe, 24, a mixing material pipe, 25, a low-sulfur isoprene pipe, 26, a noncondensed gas pipe, 27, a product pipe, 28, a circulating liquid pipe, 29, stainless steel microfilaments, 30, a main material inlet, 31, an auxiliary material inlet, 32, a cyclone groove, 33, a mixture outlet, 34, a material inlet, 35, a main pipe, 36, a pipe array, 37, small holes, 38 and a plug.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments that can be derived by one of ordinary skill in the art from the embodiments given herein are intended to be within the scope of the present invention.
As shown in fig. 1 to 4, the apparatus for isoprene fine desulfurization according to the embodiment of the present invention includes a desulfurization separation tank 5, wherein the top of the desulfurization separation tank 5 is connected to the outlet end of a desalted water pipe 23, the bottom outlet of the desulfurization separation tank 5 is connected to the inlet of a distillation column 8 through an isoprene heat exchanger 7, the top outlet of the distillation column 8 is connected to the inlet of a low-sulfur isoprene cooler 10 through the isoprene heat exchanger 7, the outlet of the low-sulfur isoprene cooler 10 is connected to the inlet of a product tank 11, the top outlet of the product tank 11 is connected to a noncondensable gas pipe 26, and the bottom outlet of the product tank 11 is connected to a product pipe 27 through a product pump 12; the bottom outlet of the distillation tower 8 is respectively connected with the inlet of a reboiler 13 and the inlet of a sulfur-containing waste liquid cooler 14 through a circulating liquid pipe 28, the outlet of the reboiler 13 is connected with the lower port of the distillation tower 8, and the outlet of the sulfur-containing waste liquid cooler 14 is connected with a sulfur-containing waste liquid pipe 29;
the desulfurization separation tank 5 both ends are equipped with desulfurization reactor 1 and baffle 6 respectively, desulfurization reactor 1 passes through the flange and is connected with desulfurization separation tank 5, baffle 6 with the bottom inner wall fixed connection of desulfurization separation tank 5, desulfurization reactor 1 includes liquid cyclone 2, liquid distributor 3 and is equipped with the reactor shell of special filler 4, special filler 4 hangs in desulfurization reactor 1 through the link, desulfurization reactor 1 upper portion is equipped with liquid distributor 3, the material import 34 of liquid distributor 3 is connected with liquid cyclone 2's mixture export 33 through the flange, liquid cyclone 2's main material import 30 is connected and is contained sulphur isoprene pipe 21, liquid cyclone 2's auxiliary material import 31 is connected fine desulfurization agent pipe 22, the spiral whirl groove 32 that sets up in liquid cyclone 2 can make the material produce rotatory and shear thereby improve the dissolution rate of fine desulfurization agent and isoprene in the flow process .
The height of the partition plate 6 is 60% of the diameter of the desulfurization separation tank 5, the outlet ends of the desalting water pipes 23 and the desulfurization reactor 1 are respectively positioned at two sides of the partition plate 6, and the bottom outlet of the desulfurization separation tank 5 and the outlet ends of the desalting water pipes 23 are positioned at the same side of the partition plate 6. And a tray 9 is arranged in the distillation tower 8, and the number of the trays in the distillation tower 8 is 5. The liquid distributor 3 comprises row pipes 36 which are transversely distributed in the desulfurization reactor 1 and are communicated with each other through a main pipe 35, small holes 37 with the diameter of 0.2-0.5mm are uniformly distributed in the row pipes 36, the small holes 37 are uniformly distributed in the cross section of the desulfurization reactor 1, the bottom and the side surfaces of the main pipe 35 are also provided with the small holes which are uniformly distributed, and one end of the main pipe and two ends of each row pipe are provided with plugs 38. The special filler is a stainless steel micro-wire bundle (made of 304 and above), the stainless steel micro-wire bundle is composed of stainless steel micro-wires 29 with the diameter of 0.05-0.15mm, the stainless steel micro-wires 29 are in a continuous S-shaped corrugated shape, and the length of the stainless steel micro-wire bundle is 3-6 m.
The fine desulfurizing agent is prepared from 40wt% of primary amine, 50wt% of secondary amine, 3wt% of nonionic surfactant, 5wt% of amphoteric surfactant and 2wt% of scorch retarder, wherein the primary amine is monoethanolamine, the secondary amine is N-monomethyl ethanolamine, the nonionic surfactant is alkylphenol polyoxyethylene ether, the amphoteric surfactant is prepared by mixing tetradecyl betaine and tertiary ammonium oxide OB-2 in a mass ratio of 1:1, the scorch retarder is N-cyclohexyl thiophthalimide, the preparation method of the fine desulfurizing agent comprises the steps of uniformly stirring the tetradecyl betaine and the tertiary ammonium oxide OB-2 in proportion at normal temperature to obtain the amphoteric surfactant, then mixing the primary amine, the secondary amine, the nonionic surfactant, the amphoteric surfactant and the scorch retarder in proportion and stirring at the temperature of 45 ℃, the stirring speed is proper to prevent a large amount of foams from appearing, forward stirring is carried out for 0.5 hour, then reverse stirring is carried out for 0.5 hour, and the stirring is carried out for a plurality of times alternately, the total stirring time is 2 hours, and standing is carried out for 1 hour after the stirring, so that the fine desulfurizing agent is obtained, and air is isolated and the fine desulfurizing agent is prevented from being directly exposed to the sun when being stored.
The method for carrying out the isoprene fine desulfurization by adopting the device comprises the following steps:
1) sulfur-containing isoprene and a fine desulfurizer respectively enter a liquid cyclone mixer 2 through a sulfur-containing isoprene pipe 21 and a fine desulfurizer pipe 22 to form a mixture which flows in a rotating manner and is sheared for multiple times, the mixture is uniformly distributed on the cross section of a special filler in a desulfurization reactor 1 through a liquid distributor 3 to be desulfurized, the isoprene and the fine desulfurizer are dispersed and sheared for countless times through the special filler, a nonionic surfactant and an amphoteric surfactant in the fine desulfurizer can effectively promote the dissolution of organic amine and isoprene, so that carbon disulfide in the isoprene is fully contacted and reacted with organic amine in the fine desulfurizer, the unreacted fine desulfurizer and desulfurization products and the isoprene form suspension in a desulfurization separation tank 5, and a trace demineralized water is injected into the desulfurization separation tank 5 through a demineralized water pipe 23 to dissolve the desulfurization products with strong adhesiveness, the mixture after desulfurization is obtained, the amphoteric surfactant can obviously improve the intersolubility of the desulfurization product and water, so that the desulfurization product is prevented from being adhered to the inner walls of the mixture pipeline after desulfurization and downstream equipment to cause blockage; the addition amount of the fine desulfurizing agent is 0.02-0.1% of the mass of the isoprene, the reaction temperature is 20-50 ℃, the operation pressure is the pressure for ensuring that the isoprene is in a liquid phase and can be pressurized and conveyed to the distillation tower, the sulfur-containing isoprene is fully contacted and reacted with the fine desulfurizing agent in a desulfurization reactor under the conditions of the temperature of 20-50 ℃ and the pressure for liquefying the isoprene, the mass of the injected desalted water is 0.05-0.2% of the mass of the isoprene material, and the desalted water is deionized water; the retention time of the mixture on the side of the partition plate 6 in the desulfurization separation tank 5, which is provided with the desulfurization reactor 1, is 0.5-2 hours, and the retention time of the mixture on the side of the partition plate 6, which is provided with the desalting water pipe 23, is 5-15 minutes;
2) the desulfurized mixture is output from a bottom outlet of the desulfurization separation tank 5, heat exchanged by a heat exchanger 7 and then enters a distillation tower 8, the boiling point of isoprene is not more than 40 ℃, the boiling point of water is 100 ℃, the boiling point of the selected organic amine is more than 110 ℃, the boiling point of other auxiliary agents is more than 150 ℃, the boiling point of a desulfurization product is more than 200 ℃, the operating pressure of the top of the distillation tower is controlled to be 0.1-0.2MPa (G), the temperature of the bottom of the distillation tower is 60-80 ℃, the temperature of the top of the distillation tower is 50-70 ℃, so that low-sulfur isoprene with low boiling point in the desulfurized mixture is evaporated from the top outlet of the distillation tower 8, and enters a low-sulfur isoprene cooler 10 for cooling after heat exchange by the; other high boiling point components in the desulfurized mixture form high-sulfur waste liquid, and the high-sulfur waste liquid is cooled by a sulfur-containing waste liquid cooler 14 and then discharged.
Experimental example 1:
the isoprene is produced after a light and heavy component removal tower of a certain chemical plant, the purity is 98.5-99.8%, the water content is less than 200 mug/g, and the total sulfur content is 25-40 mug/g, the device and the method for isoprene fine desulfurization are adopted to carry out desulfurization treatment, the treatment scale is 5t/h, the addition of a fine desulfurizing agent is 400 mug/g, the addition of desalted water is 800 mug/g, the operating pressure at the top of a distillation tower is 0.1-0.12MPa, the temperature at the bottom of the distillation tower is 60-63 ℃, and the temperature at the top of the distillation tower is 50-52 ℃. The obtained product isoprene has total sulfur content of <2 mu g/g, total nitrogen content of <2 mu g/g and total water content of 120-165 mu g/g.
Experimental example 2:
the isoprene produced by a water elution solvent tower of a certain company has the purity of 80-85 percent, the water content of 400-600 mu g/g and the total sulfur content of 30-60 mu g/g, the device and the method for the isoprene fine desulfurization are adopted for desulfurization treatment, the treatment scale is 8t/h, the addition of a fine desulfurizing agent is 700 mu g/g, the addition of demineralized water is 500 mu g/g, the operating pressure at the top of a distillation tower is 0.09-0.11MPa, the temperature at the bottom of the distillation tower is 60-62 ℃, and the temperature at the top of the distillation tower is 50-52 ℃. The total sulfur content of the obtained isoprene product is less than 2 mug/g, the total nitrogen content is less than 2 mug/g, and the total water content is less than 200 mug/g.
In conclusion, by means of the technical scheme, the isoprene product obtained by desulfurizing the sulfur-containing isoprene is a high-quality isoprene product with the total sulfur content of not more than 5 mu g/g, the total nitrogen content of not more than 2 mu g/g and the total water content of less than 200 mu g/g, the process is short, the device investment is saved, the desulfurization cost is low, the desulfurization product, the unreacted desulfurizing agent and a small amount of heavy components in the raw materials form sulfur-containing waste liquid, and the sulfur-containing waste liquid can be sent to an incinerator or a boiler for incineration treatment.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. An isoprene fine desulfurization device is characterized by comprising a desulfurization separation tank (5), wherein the top of the desulfurization separation tank (5) is connected with the outlet end of a desalting water pipe (23), the bottom outlet of the desulfurization separation tank (5) is connected with the inlet of a distillation tower (8) through an isoprene heat exchanger (7), the top outlet of the distillation tower (8) is connected with the inlet of a low-sulfur isoprene cooler (10) through the isoprene heat exchanger (7), the outlet of the low-sulfur isoprene cooler (10) is connected with the inlet of a product tank (11), the top outlet of the product tank (11) is connected with a non-condensing gas pipe (26), and the bottom outlet of the product tank (11) is connected with a product pipe (27) through a product pump (12); the bottom outlet of the distillation tower (8) is respectively connected with the inlet of a reboiler (13) and the inlet of a sulfur-containing waste liquid cooler (14) through a circulating liquid pipe (28), the outlet of the reboiler (13) is connected with the lower side port of the distillation tower (8), and the outlet of the sulfur-containing waste liquid cooler (14) is connected with a sulfur-containing waste liquid pipe (29);
the desulfurization separation tank (5) is provided with a desulfurization reactor (1) and a partition plate (6) at two ends respectively, the desulfurization reactor (1) is connected with the desulfurization separation tank (5) through a flange, the partition plate (6) is fixedly connected with the inner wall of the bottom of the desulfurization separation tank (5), the height of the partition plate (6) is 60-80% of the diameter of the desulfurization separation tank (5), the outlet end of a desalting water pipe (23) and the desulfurization reactor (1) are respectively positioned at two sides of the partition plate (6), the bottom outlet of the desulfurization separation tank (5) and the outlet end of the desalting water pipe (23) are positioned at the same side of the partition plate (6), a special filler (4) is arranged inside the desulfurization reactor (1), the special filler (4) is suspended in the desulfurization reactor (1) through a suspension ring, and a liquid distributor (3) is arranged at the upper part of the desulfurization reactor (1), the material inlet (34) of the liquid distributor (3) is connected with the mixture outlet (33) of the cyclone liquid mixer (2) through a flange, the main material inlet (30) of the cyclone liquid mixer (2) is connected with the sulfur-containing isoprene pipe (21), and the auxiliary material inlet (31) of the cyclone liquid mixer (2) is connected with the fine desulfurizing agent pipe (22).
2. The apparatus according to claim 1, characterized in that trays (9) are provided in the distillation column (8), and the number of trays in the distillation column (8) is 5-10.
3. The device according to claim 1, characterized in that the liquid distributor (3) comprises interconnected tubes (36) distributed transversely inside the desulfurization reactor (1), said tubes (36) being provided with small holes (37), said small holes (37) being uniformly distributed over said tubes (36).
4. The device according to claim 1, characterized in that the proprietary filler is a stainless steel microfilament bundle consisting of stainless steel microfilaments (29) with a diameter of 0.05-0.15mm, said stainless steel microfilaments (29) being in the form of a continuous S-shaped corrugation, said stainless steel microfilament bundle having a length of 3-6 meters.
5. Method for the fine desulfurization of isoprene using the device according to any one of claims 1 to 4, characterized by comprising the following steps:
1) sulfur-containing isoprene and a fine desulfurizer respectively enter a cyclone liquid mixer (2) through a sulfur-containing isoprene pipe (21) and a fine desulfurizer pipe (22) to form a mixture, the mixture is uniformly distributed on the cross section of a special filler in a desulfurization reactor (1) through a liquid distributor (3) for desulfurization, trace demineralized water is injected into a desulfurization separation tank (5) through a demineralized water pipe (23), and a desulfurization product is dissolved to obtain a desulfurized mixture;
2) outputting the desulfurized mixture from a bottom outlet of the desulfurization separation tank (5), exchanging heat through a heat exchanger (7), then feeding the mixture into a distillation tower (8), controlling the operating pressure of the distillation tower (8) and the temperatures of the tower bottom and the tower top, so that low-sulfur isoprene in the desulfurized mixture is evaporated from a top outlet of the distillation tower (8), exchanges heat through the heat exchanger (7), and then feeding the mixture into a low-sulfur isoprene cooler (10) for cooling, thus obtaining an isoprene product; other components in the desulfurized mixture form high-sulfur waste liquid, and the high-sulfur waste liquid is cooled by a sulfur-containing waste liquid cooler (14) and then discharged.
6. The method of claim 5, wherein: in the desulfurization separation tank (5), the retention time of the mixture in the step 1) on the side of the partition plate (6) provided with the desulfurization reactor (1) is 0.5-2 hours, and the retention time of the mixture in the step 1) on the side of the partition plate (6) provided with the desalting water pipe (23) is 5-15 minutes.
7. The method of claim 5, wherein: the fine desulfurizer prepared by the step 1) is prepared from 40-70wt% of primary amine, 20-50wt% of secondary amine, 3-7wt% of nonionic surfactant, 2-5wt% of amphoteric surfactant and 1-3wt% of scorch retarder, wherein the primary amine is one or more of monoethanolamine, diglycolamine and ethylenediamine, the secondary amine is one or more of diethanolamine, diisoethanolamine and N-monomethylethanolamine, the nonionic surfactant is one or more of alkylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, sec-octanol polyoxyethylene ether and cocofatty acid diethanolamide, the amphoteric surfactant is prepared by mixing tetradecyl betaine and tertiary ammonium oxide OB-2 according to the mass ratio of 1: 1-2: 1, and the scorch retarder is N-nitrosodiphenylamine, N-cyclohexyl thiophthalamide, One or more of polyisobutenyl succinimide and polyisobutylene polyamine.
8. The method of claim 7, wherein: the preparation method of the fine desulfurizing agent comprises the steps of uniformly stirring tetradecyl betaine and tertiary ammonium oxide OB-2 in proportion at normal temperature to obtain an amphoteric surfactant, mixing primary amine, secondary amine, a nonionic surfactant, the amphoteric surfactant and a scorch retarder in proportion, stirring at the temperature of 40-50 ℃, stirring in a forward direction for 0.5 hour, then in a reverse direction for 0.5 hour, and alternately stirring for multiple times, wherein the total stirring time is more than or equal to 2 hours, and standing for 0.5-1 hour after stirring to obtain the fine desulfurizing agent.
9. The method of claim 5, wherein: the adding amount of the fine desulfurizer in the step 1) is 0.02-0.1% of the mass of the isoprene, the reaction temperature is 20-50 ℃, the operation pressure is the pressure which ensures that the isoprene is in a liquid phase and can be pressurized and conveyed to a distillation tower, the mass of the injected desalted water is 0.05-0.2% of the mass of the isoprene material, and the desalted water is one or more of softened water, deionized water and steam condensate water; in the step 2), the operation pressure at the top of the distillation tower is 0.1-0.2MPa, the temperature at the bottom of the distillation tower is 60-80 ℃, and the temperature at the top of the distillation tower is 50-70 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910210960.3A CN109879716B (en) | 2019-03-20 | 2019-03-20 | Device and method for fine desulfurization of isoprene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910210960.3A CN109879716B (en) | 2019-03-20 | 2019-03-20 | Device and method for fine desulfurization of isoprene |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109879716A CN109879716A (en) | 2019-06-14 |
| CN109879716B true CN109879716B (en) | 2021-08-13 |
Family
ID=66933093
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910210960.3A Active CN109879716B (en) | 2019-03-20 | 2019-03-20 | Device and method for fine desulfurization of isoprene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109879716B (en) |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03151334A (en) * | 1989-11-08 | 1991-06-27 | Nippon Steel Chem Co Ltd | Desulfurizing purification of naphthalene |
| WO2011034989A2 (en) * | 2009-09-16 | 2011-03-24 | Envion, Inc. | Decomposition of waste plastics |
| CN202297419U (en) * | 2012-02-21 | 2012-07-04 | 淄博鲁华同方化工有限公司 | Device for removing sulfur components in isoprene |
| CN103320157A (en) * | 2013-06-13 | 2013-09-25 | 宁波中一石化科技有限公司 | Cracking C5 desulfurization agent composition |
| CN103571524A (en) * | 2013-12-06 | 2014-02-12 | 宁波中一石化科技有限公司 | Device and method for removing cracking C5 total sulfur |
| CN104083990A (en) * | 2014-07-25 | 2014-10-08 | 中节能六合天融环保科技有限公司 | Efficient composite renewable desulfurizing agent |
| CN205109606U (en) * | 2015-08-29 | 2016-03-30 | 宁波章甫能源科技有限公司 | Novel fibre liquid film reactor |
| CN105451861A (en) * | 2013-08-22 | 2016-03-30 | 通用电气公司 | Use of polyamines as a cs2 scavenger in isoprene production |
| CN105837408A (en) * | 2015-01-16 | 2016-08-10 | 宁波章甫能源科技有限公司 | Desulfurizer composition for removal of sulfides in MTBE |
| CN205676426U (en) * | 2016-06-21 | 2016-11-09 | 宁波章甫能源科技有限公司 | A kind of device of liquid hydrocarbon fine de-sulfur |
| WO2017188847A1 (en) * | 2016-04-25 | 2017-11-02 | Start-Catalyst Llc | A device, process, and catalyst intended for desulfurization/demercaptanization/dehydration of gaseous hydrocarbons |
-
2019
- 2019-03-20 CN CN201910210960.3A patent/CN109879716B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03151334A (en) * | 1989-11-08 | 1991-06-27 | Nippon Steel Chem Co Ltd | Desulfurizing purification of naphthalene |
| WO2011034989A2 (en) * | 2009-09-16 | 2011-03-24 | Envion, Inc. | Decomposition of waste plastics |
| CN202297419U (en) * | 2012-02-21 | 2012-07-04 | 淄博鲁华同方化工有限公司 | Device for removing sulfur components in isoprene |
| CN103320157A (en) * | 2013-06-13 | 2013-09-25 | 宁波中一石化科技有限公司 | Cracking C5 desulfurization agent composition |
| CN105451861A (en) * | 2013-08-22 | 2016-03-30 | 通用电气公司 | Use of polyamines as a cs2 scavenger in isoprene production |
| CN103571524A (en) * | 2013-12-06 | 2014-02-12 | 宁波中一石化科技有限公司 | Device and method for removing cracking C5 total sulfur |
| CN104083990A (en) * | 2014-07-25 | 2014-10-08 | 中节能六合天融环保科技有限公司 | Efficient composite renewable desulfurizing agent |
| CN105837408A (en) * | 2015-01-16 | 2016-08-10 | 宁波章甫能源科技有限公司 | Desulfurizer composition for removal of sulfides in MTBE |
| CN205109606U (en) * | 2015-08-29 | 2016-03-30 | 宁波章甫能源科技有限公司 | Novel fibre liquid film reactor |
| WO2017188847A1 (en) * | 2016-04-25 | 2017-11-02 | Start-Catalyst Llc | A device, process, and catalyst intended for desulfurization/demercaptanization/dehydration of gaseous hydrocarbons |
| CN205676426U (en) * | 2016-06-21 | 2016-11-09 | 宁波章甫能源科技有限公司 | A kind of device of liquid hydrocarbon fine de-sulfur |
Non-Patent Citations (2)
| Title |
|---|
| "催化液化气脱硫醇装置技术改造";涂联等;《河南化工》;20161231;第33卷(第10期);第45-46页 * |
| "液化气深度脱硫技术在MTBE装置上的应用";秦素平等;《石油石化节能与减排》;20131231;第3卷(第4期);第29-32页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109879716A (en) | 2019-06-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101348409A (en) | Method for producing low carbon alkene | |
| CN101423482B (en) | Integrated method of sulphonation and neutralization reaction | |
| CN102320910B (en) | Crude benzene hydrogenation method | |
| CN108862440A (en) | The energy-efficient transformation condensate liquid stripping deamination apparatus of one kind and deamination method | |
| CN111847478B (en) | Comprehensive treatment process for conversion condensate | |
| CN109879716B (en) | Device and method for fine desulfurization of isoprene | |
| EA003222B1 (en) | Process for the preparation of urea | |
| CN210560278U (en) | Hydrocracking and hydrodesulfurization integrated unit | |
| CN102311347B (en) | Device and method for continuously producing mixed dinitrobenzene by using coking benzene | |
| CN102963944B (en) | Stripping tower for CO conversion condensate | |
| CN109385313A (en) | A kind of raw gas washing process | |
| CN109529573B (en) | Process device and process method for liquid-phase desulfurization of hydrogen sulfide and sulfur dioxide | |
| CN109420417A (en) | A kind of hydration method separation sour gas technique and device | |
| CN210261603U (en) | N-methyldiethanolamine production device | |
| CN210885331U (en) | Device for producing synthetic ammonia by utilizing sodium cyanide tail gas | |
| CN202199241U (en) | Recovery device of exhausted gas of synthesis ammonia and cuprammonia regenerative system comprising same | |
| CN108722138B (en) | Acid gas treatment process and system containing hydrogen sulfide and carbon dioxide | |
| CN1919732A (en) | Primary separation tower for carbon disulphide preparation process | |
| CN219907011U (en) | Device for preparing ammonia water | |
| CN210057822U (en) | Transform condensate purification system | |
| CN106345254B (en) | Handle the method and device of H 2 S-containing gas | |
| CN214881200U (en) | System for synthesizing xanthinol nicotinate continuously through micro-channel | |
| CN207793109U (en) | A kind of propylene refining device | |
| US20230405543A1 (en) | Preparation system of ethylene by ethanol dehydration and device thereof | |
| CN202786166U (en) | Device for removing hydrogen sulfide from liquefied petroleum gas |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |