CN116532052A - Reaction equipment and process for synthesizing tertiary dodecyl mercaptan by using dodecene catalysis - Google Patents

Reaction equipment and process for synthesizing tertiary dodecyl mercaptan by using dodecene catalysis Download PDF

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Publication number
CN116532052A
CN116532052A CN202310656801.2A CN202310656801A CN116532052A CN 116532052 A CN116532052 A CN 116532052A CN 202310656801 A CN202310656801 A CN 202310656801A CN 116532052 A CN116532052 A CN 116532052A
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reaction tank
reaction
dodecyl mercaptan
dodecene
shell
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CN202310656801.2A
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CN116532052B (en
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戴正亮
黄明
余大东
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Anhui Taihunte Technology Co ltd
Anqing Changhong Technology Co ltd
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Anqing Changhong Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D21/00Separation of suspended solid particles from liquids by sedimentation
    • B01D21/26Separation of sediment aided by centrifugal force or centripetal force
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/005Separating solid material from the gas/liquid stream
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/085Feeding reactive fluids
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/10Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C319/00Preparation of thiols, sulfides, hydropolysulfides or polysulfides
    • C07C319/02Preparation of thiols, sulfides, hydropolysulfides or polysulfides of thiols
    • C07C319/04Preparation of thiols, sulfides, hydropolysulfides or polysulfides of thiols by addition of hydrogen sulfide or its salts to unsaturated compounds
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00Purification; Separation; Use of additives
    • C07C7/04Purification; Separation; Use of additives by distillation
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/584Recycling of catalysts

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The invention discloses reaction equipment and a process for synthesizing tertiary dodecyl mercaptan by using dodecene catalysis, and belongs to the technical field of tertiary dodecyl mercaptan processing. The invention is used for solving the technical problems of low reaction rate of synthesizing tertiary dodecyl mercaptan in the prior art, hydrogen sulfide leakage and high production cost in the synthesis process, and the reaction equipment for synthesizing tertiary dodecyl mercaptan by using dodecene catalysis comprises a shell, wherein a compression storage tank is arranged outside one side of the shell, an air duct communicated with the shell is arranged on the compression storage tank, a reaction tank is rotatably arranged on the inner side of the shell, and a stirring piece is arranged on the inner side of the reaction tank. The invention can not only effectively mix a plurality of heterogeneous materials of the tertiary dodecyl mercaptan synthesis reaction uniformly and improve the synthesis reaction rate, but also simplify the post-treatment procedure of the synthesis reaction, recover the hydrogen sulfide and reduce the threat of hydrogen sulfide leakage and the production cost of the tertiary dodecyl mercaptan.

Description

Reaction equipment and process for synthesizing tertiary dodecyl mercaptan by using dodecene catalysis
Technical Field
The invention relates to the technical field of tertiary dodecyl mercaptan processing, in particular to reaction equipment and a process for synthesizing tertiary dodecyl mercaptan by using dodecene catalysis.
Background
The tertiary dodecyl mercaptan is colorless oily liquid and is mainly used for ABS resin, styrene-butadiene rubber, nitrile rubber and high-impact polystyrene products, and is used as a molecular weight regulator in the polymerization reaction process. Can also be used as stabilizing agent and antioxidant of polyolefin such as polyvinyl chloride, polyethylene, etc., and can also be used for synthesizing raw materials of certain medicines, pesticides, bactericides and perfume.
In the prior art, when tert-dodecyl mercaptan is synthesized, the tert-dodecyl mercaptan is usually prepared by reacting dodecene, catalyst aluminum trichloride and hydrogen sulfide, but dodecene is a liquid compound, the catalyst aluminum trichloride is a solid compound, hydrogen sulfide usually can be a gaseous compound, three heterogeneous materials are mixed and reacted in the same reaction system, the driven synthesis reaction equipment is usually mixed by simple stirring, the hydrogen sulfide phase material floats on the top of the solid-liquid phase mixed material and is difficult to fully mix with the solid-liquid phase mixed material, the synthesis reaction time of tert-dodecyl mercaptan is long, the proper rate of tert-dodecyl mercaptan is low, the solid material and the liquid material are required to be separated by filtering, centrifuging and other modes after the reaction is finished, hydrogen sulfide in the reaction system is a highly toxic compound, the traditional synthesis reaction equipment treats the residual hydrogen sulfide in the reaction as waste gas, on the one hand, the threat of hydrogen sulfide leakage exists, on the other hand, the hydrogen sulfide cannot be compressed and the serious raw material is also wasted, and the tert-dodecyl mercaptan synthesis reaction cost is high.
In view of the technical drawbacks of this aspect, a solution is now proposed.
Disclosure of Invention
The invention aims to provide reaction equipment and a process for synthesizing tertiary dodecyl mercaptan by using dodecene catalysis, which are used for solving the technical problems that in the prior art, when heterogeneous materials are stirred by the equipment for synthesizing tertiary dodecyl mercaptan, heterogeneous materials are difficult to mix uniformly, so that the synthesis reaction rate of tertiary dodecyl mercaptan is low, and in the synthesis reaction process of tertiary dodecyl mercaptan, unreacted hydrogen sulfide raw materials are treated as waste gas, serious raw material waste is caused while the leakage of hydrogen sulfide threatens, and the synthesis reaction cost of tertiary dodecyl mercaptan is high.
The aim of the invention can be achieved by the following technical scheme:
the reaction equipment for synthesizing tertiary dodecyl mercaptan by using dodecene catalysis comprises a shell, wherein a compression storage tank is arranged outside one side of the shell, an air duct communicated with the shell is arranged on the compression storage tank, a reaction tank is rotatably arranged inside the shell, a stirring piece is arranged inside the reaction tank, an auxiliary mechanism which is matched with the stirring piece and used for assisting gas materials to enter the reaction tank and circulate on the inner wall of the reaction tank is arranged at the bottom of the reaction tank, a driving assembly for driving the reaction tank or the stirring piece to rotate is arranged at the bottom of the inner side of the shell, a plurality of communication holes are formed in the outer wall of the reaction tank, and an airtight assembly for sealing the communication holes is arranged outside the reaction tank;
the airtight assembly comprises a bushing arranged outside the reaction tank, wherein a plurality of side plates and a transmission mechanism used for driving the side plates to move along the horizontal direction are arranged on the inner side of the bushing, a sealing plate is arranged on one side, close to the reaction tank, of each side plate, and a sealing column matched with the communication hole is arranged on each sealing plate.
Further, the installation cavity has been seted up at the inboard top of casing, the top of retort extends to the inboard of installation cavity and passes through the sealing washer rotation with the inner wall of installation cavity and be connected, the inboard rotation of installation cavity is installed and is connect the material ring, the bottom rigid coupling that connects the material ring has the connecting pipe, the bottom of connecting pipe extends to the inboard of retort, the bottom rigid coupling of casing has the feed hopper, the bottom of feed hopper extends to the inboard that connects the material ring.
Further, the stirring piece comprises a stirring shaft and a plurality of cross bars fixedly connected to the outer portion of the stirring shaft, and the upper end and the lower end of the stirring shaft are respectively connected with the bottom and the top center of the reaction tank in a rotating mode through sealing pieces.
Further, the auxiliary mechanism comprises a box body arranged at the bottom center of the reaction tank, the air pump is arranged at the inner side of the box body, the bottom of the stirring shaft extends to the inner side of the box body, a vertical groove is formed in the bottom center of the stirring shaft, an air inlet hole communicated with the vertical groove is formed in the outer wall of the stirring shaft, a plurality of air guide pipes communicated with the inner bottom of the reaction tank are fixedly connected to the outer wall of the box body, an air inlet pipe is sleeved outside the box body, and one end of the air inlet pipe extends to the inner side of the box body and is rotationally connected with the inner bottom of the box body.
Further, the drive assembly is including installing the output shaft at the inboard top of installation cavity, be used for driving output shaft pivoted driving motor is installed at the top of casing, the outside cover of output shaft is equipped with the lifter plate, a plurality of electric telescopic links that are used for driving the lifter plate to go up and down are installed at the reaction tank top, the top fixed mounting of output shaft has the driving ring, the driving ring is all fixed mounting in one side that is close to each other with the lifter plate has a plurality of spacing pinion rack I, the drive assembly still includes the movable sleeve and establishes at the outside annular cover of lifter plate and install the annular plate at the inboard top of annular cover, the bottom of annular cover is connected with the bottom of retort through the connection monomer, and the spacing pinion rack II is all installed to one side that annular plate and lifter plate are close to each other.
Further, the connecting unit comprises a plurality of containing holes formed in the bottom of the annular sleeve, a tension spring is mounted at the bottom of the inner side of the containing holes, a limiting column is fixedly connected to the bottom of the tension spring, and the bottoms of the limiting columns extend to the bottom of the containing holes and are fixedly connected with the top of the reaction tank.
Further, the transmission rod corresponding to the side plates is installed on the inner side of the bushing, a plurality of connecting shafts are hinged to the outer wall of one side of the transmission rod, and one ends, far away from the transmission rod, of the connecting shafts are respectively hinged to the outer wall of one side, far away from the reaction tank, of the side plates.
Further, the transmission mechanism comprises a connecting ring which is respectively arranged on the inner side of the shell and the mounting cavity, the two connecting rings are fixedly connected through a plurality of connecting shafts, the two connecting rings are respectively provided with a plurality of connecting blocks in a sliding manner, the top of the transmission rod is respectively extended to the inner side of the connecting rings and fixedly connected with the connecting blocks, the bottom of the outer side of the annular sleeve is fixedly connected with a plurality of connecting plates, and the other ends of the connecting plates are respectively extended to the inner side of the connecting rings in the mounting cavity and fixedly connected with the top of the connecting blocks.
A reaction process for synthesizing tertiary dodecyl mercaptan by using dodecene catalysis, which is applicable to the reaction equipment for synthesizing tertiary dodecyl mercaptan by using dodecene catalysis according to any one of claims 1 to 8, and comprises the following steps:
s1, adding a dodecene crude product into a rectifying tower for rectification, and collecting a fraction at 195-200 ℃ as a raw material dodecene;
s2, adding 200kg of raw materials of dodecene and 500kg of aluminum trichloride powder into a reaction tank of reaction equipment for synthesizing tertiary dodecyl mercaptan by using dodecene catalysis, introducing 40kg of dry hydrogen sulfide gas into the reaction tank from an air inlet pipe, increasing the temperature of the reaction tank to 40 ℃, and increasing the pressure of the reaction tank to 2.0-2.5Mpa;
s3, driving the stirring piece to rotate by the driving motor, promoting the mixing of reaction components in the reaction tank, and enabling the air pump to work, so that the hydrogen sulfide gas circulates at the inner side of the reaction tank and reacts for 6 hours;
s4, after the reaction is completed, the side plates move in the direction away from the reaction tank, air compression equipment on the compression storage tank is started to collect hydrogen sulfide gas leaked from the reaction tank, and the reaction tank is driven to rotate by the driving motor to separate liquid from solid in the reaction tank, so that reaction liquid in the reaction system enters the inner side of the shell;
s5, opening a valve on a discharge pipe under the protection of nitrogen, transferring the liquid in the shell into a washing kettle, adding 200kg of 0.2M sodium hydroxide aqueous solution into the washing kettle, stirring for 30-50min, standing for separating liquid, and washing the organic phase with 90kg of purified water for 3 times to obtain a tertiary dodecyl mercaptan crude product;
s6, adding the crude product of the tertiary dodecyl mercaptan into a feeding tower for rectification, and collecting fractions at 170-180 ℃ to obtain a tertiary dodecyl mercaptan finished product.
The invention has the following beneficial effects:
1. according to the reaction equipment for synthesizing the tertiary dodecyl mercaptan by using the dodecene catalysis, the shell, the reaction tank, the stirring piece, the air inlet pipe and the driving component are matched with each other, so that the tertiary dodecyl mercaptan synthesis reaction raw material is conveniently added into the reaction device, the driving component drives the stirring piece to rotate, the catalyst aluminum trichloride and dodecene in the reaction tank can be promoted to be fully mixed together, the box body arranged at the bottom of the reaction tank, the air pump, the air pipe and the stirring piece are matched with each other, hydrogen sulfide gas in the reaction tank can be pumped from the bottom of the reaction tank after being pumped out from the top of the inner side of the reaction tank, the gas circulation from bottom to top is formed, the sedimentation of the catalyst in the reaction tank is avoided, the mixing uniformity of the hydrogen sulfide gas, the catalyst and the dodecene is improved, the reaction rate of the tertiary dodecyl mercaptan is further improved, and the reaction time of the tertiary dodecyl mercaptan is reduced.
2. According to the reaction equipment for synthesizing the tertiary dodecyl mercaptan by utilizing the dodecene catalysis, the bushing, the side plates, the transmission rod, the connecting shaft, the connecting plate and the transmission assembly are mutually matched, the side plates are pushed to be far away from the reaction tank before the reaction tank is driven to rotate by the driving assembly, so that a plurality of communication holes on the reaction tank are opened, hydrogen sulfide gas and some liquid reactants in the reaction tank flow out of the reaction tank and are separated from a catalyst under the action of gravity and the pressure in the reaction tank, the reaction tank is positioned at the inner side of a shell, the compression equipment on the compression storage tank works, the gas in the shell can be sucked into the compression storage tank for compression storage, the leakage of the hydrogen sulfide gas is avoided, the loss of the hydrogen sulfide can be reduced, the production cost is reduced, the reaction tank is driven by the driving assembly to rotate, the generated centrifugal force can promote the separation of a solid catalyst from the aluminum oxide, the raw materials dodecene and the hydrogen sulfide can be directly added into the reaction tank for the synthesis reaction in the later production process, the operation process is simplified, and the tertiary dodecyl mercaptan synthesis rate is improved.
3. According to the reaction process for synthesizing the tertiary dodecyl mercaptan by using the dodecene catalysis, the dodecene is rectified, the hydrogen sulfide is dried, the moisture content in the raw materials can be effectively reduced, the side reaction is reduced, the tertiary dodecyl mercaptan reacts in the reaction equipment for synthesizing the tertiary dodecyl mercaptan by using the dodecene catalysis, the solid material aluminum trichloride, the liquid material dodecene and the gas material hydrogen sulfide can be promoted to be fully and uniformly mixed in the reaction tank by stirring and gas circulation, the mixing uniformity degree among heterogeneous materials is improved, the full mixing among materials is promoted, the reaction time of the tertiary dodecyl mercaptan is reduced, the solid phase, the liquid phase and the gas phase in the reaction system can be rapidly separated by mutually matching the communication hole arranged on the reaction tank with the sealing component, the shell arranged outside the reaction tank is mutually matched with the compression storage tank, the hydrogen sulfide gas can be compressed and collected, the leakage of the hydrogen sulfide is avoided, the water absorption and inactivation of the catalyst can be avoided in the subsequent synthesis process by nitrogen protection, the treatment process of the catalyst can be recycled, the post-reaction treatment process is simplified, the reaction cost is reduced, the post-treatment time of the tertiary dodecyl mercaptan is improved, and the post-treatment time is shortened.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of the overall structure of a reaction apparatus for synthesizing tertiary dodecyl mercaptan by using dodecene catalysis in the invention;
FIG. 2 is a schematic diagram showing a schematic cross-sectional front view of a reaction apparatus for synthesizing tertiary dodecyl mercaptan by using dodecene catalysis in the present invention;
FIG. 3 is an enlarged schematic view of the structure of FIG. 2A according to the present invention;
FIG. 4 is an enlarged schematic view of the structure of FIG. 2B according to the present invention;
FIG. 5 is an enlarged schematic view of the structure of FIG. 2 at C according to the present invention;
FIG. 6 is a schematic view showing the overall structure of the reaction tank and the liner according to the present invention;
FIG. 7 is a schematic view of the overall structure of the receiving ring according to the present invention;
FIG. 8 is a schematic view of the overall structure of the stirring element in the present invention;
fig. 9 is a schematic structural diagram of an output shaft, a lifting plate, a first limiting toothed plate and a second limiting toothed plate in the present invention.
In the figure: 100. a housing; 101. a receiving ring; 102. a feed hopper; 103. an air duct; 104. a compression tank; 200. a reaction tank; 201. a stirring member; 300. a bushing; 301. a side plate; 302. a sealing plate; 303. a communication hole; 304. a sealing column; 305. a filter screen; 306. a horizontal axis; 400. a transmission rod; 401. a connecting shaft; 500. a driving motor; 501. an output shaft; 502. a lifting plate; 503. a drive ring; 504. a first limiting toothed plate; 505. an electric telescopic rod; 600. an annular sleeve; 601. a tension spring; 602. a limit column; 603. an annular plate; 604. a limiting toothed plate II; 605. a splice plate; 700. a linking ring; 701. a joint block; 702. a connecting shaft; 800. a case; 801. an air inlet hole; 802. an air duct; 803. and an air inlet pipe.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in connection with the embodiments, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Referring to fig. 1, 2 and 7, the reaction apparatus for synthesizing tertiary dodecyl mercaptan by using dodecene catalysis provided in this embodiment includes a housing 100, a compression storage tank 104 is installed outside one side of the housing 100, an air duct 103 communicated with the housing 100 is installed on the compression storage tank 104, a reaction tank 200 is rotatably installed inside the housing 100, a stirring member 201 is installed inside the reaction tank 200, an installation cavity is provided at the top of the inner side of the housing 100, and the top of the reaction tank 200 extends to the inner side of the installation cavity and is rotatably connected with the inner wall of the installation cavity through a sealing ring;
the bottom of the installation cavity is sealed by the outer wall of the top of the reaction tank 200, and a sealing ring for sealing the reaction tank 200 and the installation cavity is made of fluororubber material, so that the installation cavity forms a sealed cavity, hydrogen sulfide gas is prevented from entering the inner side of the installation cavity, the compression storage tank 104 arranged outside the shell 100 can collect and compress the hydrogen sulfide gas inside the shell 100 after the reaction is completed, the leakage of the hydrogen sulfide gas is prevented, and the hydrogen sulfide gas which does not participate in the reaction is recycled;
the inner side of the installation cavity is rotatably provided with a receiving ring 101, the bottom of the receiving ring 101 is fixedly connected with a connecting pipe, the bottom of the connecting pipe extends to the inner side of the reaction tank 200, a sealing valve (not shown) for preventing gas leakage is arranged on the connecting pipe, the bottom of the shell 100 is fixedly connected with a feeding funnel 102, and the bottom of the feeding funnel 102 extends to the inner side of the receiving ring 101;
the bottom of the shell 100 is provided with a discharging pipe (not shown) with a valve, the bottom of the receiving ring 101 is provided with an inclined plane which is obliquely downwards arranged towards the direction of the connecting pipe, the top of the receiving ring 101 is provided with a groove for conveying reaction raw materials such as catalyst, dodecene and the like, after the reaction raw materials enter the inner side of the shell 100 from the feeding funnel 102, the materials are conveyed towards the direction of the connecting pipe along the bottom of the groove on the receiving ring 101 so as to enter the inner side of the reaction tank 200, the receiving ring 101 is rotationally connected with the inner wall of the mounting cavity, the receiving ring 101 can synchronously rotate along with the reaction tank 200, and the receiving ring 101 with an annular structure can enable the materials to enter the inner side of the mounting cavity from the feeding funnel 102 and then to be conveyed towards the direction of the connecting pipe along the inclined plane of the bottom of the receiving ring 101, so that the materials enter the inner side of the reaction tank 200, and the top of the receiving ring 101 is abutted with the bottom of the mounting cavity, and the materials are prevented from overflowing from the groove on the receiving ring 101.
Example 2
Referring to fig. 2 and 8, in the reaction apparatus for synthesizing tert-dodecyl mercaptan by dodecene catalysis provided in the present embodiment, a stirring member 201 includes a stirring shaft and a plurality of cross bars fixedly connected to the outside of the stirring shaft, and the upper and lower ends of the stirring shaft are respectively connected with the bottom and the top center of a reaction tank 200 in a rotating manner through sealing members, wherein the sealing members are made of corrosion-resistant materials.
An auxiliary mechanism which is matched with the stirring piece 201 mutually to assist the hydrogen sulfide gas to enter the reaction tank 200 and circulate at the inner wall of the reaction tank 200 is arranged at the bottom of the reaction tank 200;
the auxiliary mechanism comprises a box 800 arranged at the bottom center of the reaction tank 200, an air pump is arranged at the inner side of the box 800, the bottom of a stirring shaft extends to the inner side of the box 800, a vertical groove is formed at the bottom center of the stirring shaft, an air inlet hole 801 communicated with the vertical groove is formed in the outer wall of the stirring shaft, a plurality of air guide pipes 802 communicated with the inner bottom of the reaction tank 200 are fixedly connected to the outer wall of the box 800, an air inlet pipe 803 is sleeved on the outer side of the shell 100, and one end of the air inlet pipe 803 extends to the inner side of the shell 100 and is rotationally connected with the inner bottom of the box 800.
A valve (not shown) is arranged on the air inlet pipe 803, the valve on the air inlet pipe 803 is opened, hydrogen sulfide gas enters the inner side of the box body 800 through the air inlet pipe 803, then enters the inner side of the reaction tank from the plurality of air guide pipes 802, the hydrogen sulfide gas is conveniently conveyed to the inner side of the reaction tank 200, after the materials are added, the valve on the air inlet pipe 803 is closed, in the reaction process, an air pump (not shown) sucks the hydrogen sulfide gas at the top of the inner side of the reaction tank 200 from the plurality of air inlet holes 801 to the inner side of the box body 800 through a vertical groove, then the hydrogen sulfide gas is conveyed to the bottom of the inner side of the reaction tank 200 from the plurality of air guide pipes 802, the hydrogen sulfide gas is formed to circulate inside the reaction tank 200, the hydrogen sulfide gas is promoted to fully contact with a reaction system, and the reaction rate is improved.
Example 3
Referring to fig. 2, 3 and 9, the reaction apparatus for synthesizing tertiary dodecyl mercaptan by using dodecene catalysis provided in the present embodiment includes a driving component installed at the bottom of the inner side of the casing 100 for driving the reaction tank 200 or the stirring member 201 to rotate;
the drive assembly is including installing the output shaft 501 at the inboard top of installation cavity, the top of casing 100 is installed and is used for driving output shaft 501 pivoted driving motor 500, the outside cover of output shaft 501 is equipped with lifter plate 502, a plurality of electric telescopic handle 505 that are used for driving lifter plate 502 to go up and down are installed at retort 200 top, the top fixed mounting of output shaft has driving ring 503, driving ring 503 and lifter plate 502 are all fixed mounting in one side that is close to each other have a plurality of spacing pinion rack one 504, drive assembly still includes movable sleeve and establishes at the outside annular cover 600 of lifter plate 502 and install the annular plate 603 at annular cover 600 inboard top, spacing pinion rack two 604 are all installed to the one side that annular plate 603 and lifter plate 502 are close to each other, the bottom of annular cover 600 is connected with the top of retort 200 through the connecting unit.
The bottom section of the output shaft 501 is of a regular polygon structure, a hole matched with the output shaft 501 is formed in the center of the lifting plate 502, the lifting plate 502 can synchronously rotate along with the rotation of the output shaft 501, the electric telescopic rod 505 contracts, the lifting plate 502 descends, the bottom of the lifting plate 502 is meshed with a first limiting toothed plate 504 at the top of the transmission ring 503, the top of the lifting plate 502 is separated from a second limiting toothed plate 604 at the bottom of the annular plate 603, the driving motor 500 drives the output shaft 501 to rotate, the lifting plate 502 and the transmission ring 503 are driven to synchronously rotate, then the stirring piece is driven to rotate, the reaction system in the reaction tank 200 is promoted to be mixed, the electric telescopic rod 505 stretches, the lifting plate 502 is pushed to ascend, the bottom of the lifting plate 502 is meshed with a second limiting toothed plate 604 at the top of the transmission ring 503, the driving motor 500 drives the output shaft 501 to rotate, and the lifting plate 502 and the annular plate 603 are driven to synchronously rotate, and the reaction tank 200 can be driven to rotate.
Example 4
Referring to fig. 2-6, a reaction apparatus for synthesizing tertiary dodecyl mercaptan by using dodecene catalysis provided in this embodiment includes a plurality of communication holes 303 formed on an outer wall of a reaction tank 200 and an airtight assembly installed outside the reaction tank 200 and matched with the reaction tank 200;
the airtight assembly comprises a bushing 300 installed outside the reaction tank 200, wherein a plurality of side plates 301 and a transmission mechanism for driving the side plates 301 to move in the horizontal direction are installed on the inner side of the bushing 300, a sealing plate 302 is arranged on one side, close to the reaction tank 200, of each side plate 301, and a sealing column 304 matched with a communication hole 303 is installed on each sealing plate 302;
the transmission rod 400 corresponding to the side plates 301 is installed on the inner side of the bushing 300, a plurality of connecting shafts 401 are hinged to the outer wall of one side of the transmission rod 400, and the other ends of the connecting shafts 401 are hinged to the outer wall of one side, away from the sealing plate 302, of the side plates 301.
The upper and lower both ends at curb plate 301 all are movable sleeve and are equipped with the cross axle 306 of level setting, the both ends of a plurality of cross axles 306 respectively with the outer wall of retort 200 and the inner wall rigid coupling of bush 300, the sealed post 304 is located the inboard one end of intercommunicating pore 303 and the identical with intercommunicating pore 303, all be equipped with filter screen 305 on a plurality of intercommunicating pore 303, cross axle 306 plays the guide effect, the motion trail direction of curb plate 301 is guided, when making curb plate 301 to retort 200 orientation motion, a plurality of sealed posts 304 can enter into the inboard of intercommunicating pore 303 smoothly, seal retort 200, a plurality of transfer lines 400 all slide with the inner wall of bush 300 in one side outer wall that keeps away from retort 200, transfer lines 400 rise, make a plurality of transmission connecting shafts 401 take its pin joint on the retort 200 as the axle upwards deflection, thereby drive a plurality of curb plate 301 synchronous to be away from retort 200's direction motion, make a plurality of intercommunicating pore 303 open, transfer lines 400 descend, make a plurality of transmission connecting shafts 401 trend horizontal by the inclination state, thereby promote the synchronous direction motion to retort 200 of a plurality of curb plate 301, a plurality of sealed posts 304 insert respectively to the inner wall of the sealed post, can seal up the outer wall of a plurality of intercommunicating pore 200, thereby prevent the sealing plate 303 from leaking outside the sealed up, further sealing plate 303, and sealing plate 200.
The transmission mechanism comprises a connecting ring 700 which is respectively arranged on the inner side of the shell 100 and the mounting cavity, the two connecting rings 700 are fixedly connected through a plurality of connecting shafts 702, a plurality of connecting blocks 701 are respectively and slidably arranged on the two connecting rings 700, the tops of the plurality of transmission rods 400 respectively extend to the inner side of the connecting rings 700 and are fixedly connected with the connecting blocks 701, a plurality of connecting plates 605 are fixedly connected to the bottom of the outer side of the annular sleeve 600, and the other ends of the plurality of connecting plates 605 respectively extend to the inner side of the connecting rings 700 positioned in the mounting cavity and are fixedly connected with the tops of the connecting blocks 701.
The connecting unit comprises a plurality of containing holes formed in the bottom of the annular sleeve 600, a tension spring 601 is mounted at the bottom of the inner side of the containing holes, a limiting column 602 is fixedly connected to the bottom of the tension spring 601, and the bottoms of the limiting columns 602 extend to the bottom of the containing holes and are fixedly connected with the top of the reaction tank 200.
A plurality of protrusions (not shown) are arranged at the bottom of the connecting plate 605, a plurality of grooves (not shown) with the protrusions matched with each other are formed in the top of the reaction tank 200, the annular sleeve 600 moves downwards under the action of a plurality of tension springs 601 and gravity, the protrusions at the bottom of the connecting plate 605 extend to the inner sides of the grooves, so that the driving assembly is prevented from driving the reaction tank 200 to synchronously rotate when the stirring piece 201 is driven to rotate, the lifting plate 502 is lifted to drive the annular plate 603 to synchronously lift with the annular sleeve 600, the tension springs 601 are stretched, the connecting plate 605 is driven to synchronously lift while the annular sleeve 600 is lifted, the protrusions at the bottom of the connecting plate 605 are separated from the grooves at the top of the reaction tank 200, and the two connecting rings 700 are driven to synchronously lift, so that the transmission rods 400 are driven to synchronously lift.
Example 5
Referring to fig. 1-9, the reaction process for synthesizing tertiary dodecyl mercaptan by using dodecene catalysis provided in the embodiment includes the following steps:
s1, adding a dodecene crude product into a rectifying tower, increasing the temperature of the rectifying tower to 195 ℃ at a speed of 5 ℃/min, rectifying under reduced pressure until no fraction is produced, obtaining a first front fraction, increasing the temperature of a feeding tower to 200 ℃ at a speed of 0.2 ℃/min, rectifying under reduced pressure until no fraction is produced, obtaining raw materials of dodecene and kettle residue, transferring the kettle residue into a heat accumulating type thermal incinerator for incineration, and heating the rectifying tower by hot flue gas generated by the incinerator through waste heat recovery;
s2, adding 200kg of raw materials of dodecene and 500kg of aluminum trichloride powder into the reaction tank 200 from a feed hopper 102 on a reaction device for synthesizing tertiary dodecyl mercaptan by using dodecene catalysis, closing a sealing valve on a connecting pipe, opening a valve on an air inlet pipe 803, introducing 40kg of dried hydrogen sulfide gas into the reaction tank 200 from the air inlet pipe 803, closing the valve on the air inlet pipe 803, increasing the temperature of the reaction tank 200 to 40 ℃, and increasing the pressure of the reaction tank 200 to 2.0-2.5Mpa;
s3, the electric telescopic rod 505 is contracted, the bottom of the lifting plate 502 is meshed with the second limiting toothed plate 604 at the top of the transmission ring 503, the driving motor 500 drives the stirring piece 201 to rotate, the mixing of reaction components in the reaction tank 200 is promoted, the air pump works, hydrogen sulfide gas at the top of the inner side of the reaction tank 200 is sucked into the inner side of the box 800 from the plurality of air inlets 801, and then is conveyed to the bottom of the inner side of the reaction tank 200 from the plurality of air ducts 802, hydrogen sulfide gas circulation is formed at the inner side of the reaction tank 200, and the reaction is carried out for 6 hours;
s4, an electric telescopic rod 505 pushes a lifting plate 502 to slowly ascend, the top of the lifting plate 502 is meshed with a limiting toothed plate II 604 at the bottom of an annular plate 603, a plurality of side plates 301 move towards a direction away from the reaction tank 200, air compression equipment on a compression storage tank 104 is started to absorb, compress and store hydrogen sulfide gas leaked from the reaction tank 200, a driving motor 500 drives the reaction tank 200 to rotate, the generated force center acts, separation of liquid and solid in the reaction tank 200 is promoted, reaction liquid in a reaction system enters the inner side of a shell 100, and a solid catalyst in the reaction system remains in the reaction tank 200;
s5, opening a valve on a discharge pipe under the protection of nitrogen, transferring the liquid in the shell 100 into a washing kettle, adding 200kg of 0.2M sodium hydroxide aqueous solution into the washing kettle, stirring for 30-50min, standing for separating liquid, and washing the organic phase with 90kg of purified water for 3 times to obtain a tertiary dodecyl mercaptan crude product;
s6, adding the tertiary dodecyl mercaptan crude product into a feeding tower, increasing the temperature of the feeding tower to 170 ℃ at a speed of 5 ℃/min, rectifying under reduced pressure until no liquid flows out, obtaining a first fraction II, increasing the temperature of the rectifying tower to 180 ℃ at a speed of 0.3 ℃/min, rectifying under reduced pressure until no liquid flows out, obtaining a tertiary dodecyl mercaptan finished product and a second kettle residue, transferring the second kettle residue into a thermal storage type thermal incinerator for incineration treatment, and heating the rectifying tower by hot flue gas generated by the incinerator through waste heat recovery.
The foregoing is merely illustrative and explanatory of the invention, as it is well within the scope of the invention as claimed, as it relates to various modifications, additions and substitutions for those skilled in the art, without departing from the inventive concept and without departing from the scope of the invention as defined in the accompanying claims.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.

Claims (9)

1. The reaction equipment for synthesizing tertiary dodecyl mercaptan by using dodecene catalysis comprises a shell (100), and is characterized in that a compression storage tank (104) is arranged outside one side of the shell (100), an air duct (103) communicated with the shell (100) is arranged on the compression storage tank (104), a reaction tank (200) is rotatably arranged on the inner side of the shell (100), a stirring piece (201) is arranged on the inner side of the reaction tank (200), an auxiliary mechanism which is matched with the stirring piece (201) and used for assisting gas materials to enter the reaction tank (200) and circulate on the inner wall of the reaction tank (200) is arranged at the bottom of the inner side of the shell (100), a driving component for driving the reaction tank (200) or the stirring piece (201) to rotate is arranged at the bottom of the inner side of the shell (100), a plurality of communication holes (303) are formed in the outer wall of the reaction tank (200), and an airtight component for sealing the communication holes (303) is arranged outside the reaction tank (200);
the airtight assembly comprises a bushing (300) arranged outside the reaction tank (200), a plurality of side plates (301) and a transmission mechanism used for driving the side plates (301) to move in the horizontal direction are arranged on the inner side of the bushing (300), sealing plates (302) are arranged on one sides, close to the reaction tank (200), of the side plates (301), and sealing columns (304) matched with the communication holes (303) are arranged on the sealing plates (302).
2. The reaction device for synthesizing tertiary dodecyl mercaptan by using dodecene catalysis according to claim 1, wherein an installation cavity is formed in the top of the inner side of the shell (100), the top of the reaction tank (200) extends to the inner side of the installation cavity and is rotationally connected with the inner wall of the installation cavity through a sealing ring, a receiving ring (101) is rotationally installed on the inner side of the installation cavity, a connecting pipe is fixedly connected to the bottom of the receiving ring (101), the bottom of the connecting pipe extends to the inner side of the reaction tank (200), a feeding funnel (102) is fixedly connected to the bottom of the shell (100), and the bottom of the feeding funnel (102) extends to the inner side of the receiving ring (101).
3. The reaction apparatus for synthesizing tert-dodecyl mercaptan by dodecene catalysis according to claim 1, wherein the stirring member (201) comprises a stirring shaft and a plurality of cross bars fixedly connected to the outside of the stirring shaft, and the upper and lower ends of the stirring shaft are respectively and rotatably connected with the bottom and top centers of the reaction tank (200) through sealing members.
4. The reaction device for synthesizing tertiary dodecyl mercaptan by utilizing dodecene catalysis according to claim 3, wherein the auxiliary mechanism comprises a box body (800) arranged at the bottom center of the reaction tank (200), an air pump is arranged at the inner side of the box body (800), the bottom of the stirring shaft extends to the inner side of the box body (800), a vertical groove is formed in the bottom center of the stirring shaft, an air inlet hole (801) communicated with the vertical groove is formed in the outer wall of the stirring shaft, a plurality of air guide pipes (802) communicated with the inner bottom of the reaction tank (200) are fixedly connected to the outer wall of the box body (800), an air inlet pipe (803) is sleeved outside the box body (100), and one end of the air inlet pipe (803) extends to the inner side of the box body (100) and is rotationally connected with the inner bottom of the box body (800).
5. The reaction device for synthesizing tertiary dodecyl mercaptan by using dodecene catalysis according to claim 2, wherein the driving assembly comprises an output shaft (501) installed at the inner top of the installation cavity, a driving motor (500) for driving the output shaft (501) to rotate is installed at the top of the shell (100), a lifting plate (502) is sleeved outside the output shaft (501), a plurality of electric telescopic rods (505) for driving the lifting plate (502) to lift are installed at the top of the reaction tank (200), a driving ring (503) is fixedly installed at the top of the output shaft, a plurality of limiting toothed plates I (504) are fixedly installed at one sides, close to each other, of the driving ring (503) and the lifting plate (502), the driving assembly further comprises an annular sleeve (600) movably sleeved outside the lifting plate (502) and an annular plate (603) installed at the inner top of the annular sleeve (600), the bottom of the annular sleeve (600) is connected with the bottom of the reaction tank (200) through a connecting monomer, and limiting plates II (604) are installed at one sides, close to each other, of the limiting plates II (603) and the lifting plate (502).
6. The reaction device for synthesizing tertiary dodecyl mercaptan by using dodecene catalysis according to claim 5, wherein the connecting unit comprises a plurality of containing holes formed at the bottom of the annular sleeve (600), a tension spring (601) is installed at the bottom of the inner side of the containing holes, a limiting column (602) is fixedly connected to the bottom of the tension spring (601), and the bottoms of the limiting columns (602) extend to the bottom of the containing holes and are fixedly connected with the top of the reaction tank (200).
7. The reaction apparatus for synthesizing tert-dodecyl mercaptan by dodecene catalysis according to claim 6, wherein a transmission rod (400) is installed at the inner side of the bushing (300) and is arranged corresponding to the plurality of side plates (301), a plurality of connecting shafts (401) are hinged to one side outer wall of the transmission rod (400), and one ends of the plurality of connecting shafts (401) far away from the transmission rod (400) are respectively hinged to one side outer wall of the plurality of side plates (301) far away from the reaction tank (200).
8. The reaction apparatus for synthesizing tert-dodecyl mercaptan by dodecene catalysis according to claim 7, wherein the transmission mechanism comprises a plurality of engagement plates (605) respectively installed on the inner sides of the shell (100) and the installation chamber, the two engagement plates (700) are fixedly connected through a plurality of engagement shafts (702), a plurality of engagement blocks (701) are slidably installed on the two engagement plates (700), the tops of the plurality of transmission rods (400) respectively extend to the inner sides of the engagement plates (700) and are fixedly connected with the engagement blocks (701), a plurality of engagement plates (605) are fixedly connected to the outer bottoms of the annular sleeve (600), and the other ends of the plurality of engagement plates (605) respectively extend to the inner sides of the engagement plates (700) in the installation chamber and are fixedly connected with the tops of the engagement blocks (701).
9. A reaction process for synthesizing tertiary dodecyl mercaptan by using dodecene catalysis, which is suitable for the reaction equipment for synthesizing tertiary dodecyl mercaptan by using dodecene catalysis according to any one of claims 1 to 8, and is characterized by comprising the following steps:
s1, adding a dodecene crude product into a rectifying tower for rectification, and collecting a fraction at 195-200 ℃ as a raw material dodecene;
s2, adding 200kg of raw materials of dodecene and 500kg of aluminum trichloride powder into a reaction tank (200) of a reaction device for synthesizing tertiary dodecyl mercaptan by using dodecene catalysis, introducing 40kg of dry hydrogen sulfide gas into the reaction tank (200) from an air inlet pipe (803), and raising the temperature of the reaction tank (200) to 40 ℃, wherein the pressure of the reaction tank (200) is raised to 2.0-2.5Mpa;
s3, a driving motor (500) drives a stirring piece (201) to rotate, so that the mixing of reaction components in the reaction tank (200) is promoted, and an air pump works, so that hydrogen sulfide gas circulates inside the reaction tank (200) and reacts for 6 hours;
s4, after the reaction is completed, the side plates (301) move in the direction away from the reaction tank (200), air compression equipment on the compression storage tank (104) is started to collect hydrogen sulfide gas leaked from the reaction tank (200), the reaction tank (200) is driven by the driving motor (500) to rotate, and liquid and solid in the reaction tank (200) are separated, so that reaction liquid in a reaction system enters the inner side of the shell (100);
s5, opening a valve on a discharge pipe under the protection of nitrogen, transferring the liquid in the shell (100) into a washing kettle, adding 200kg of 0.2M sodium hydroxide aqueous solution into the washing kettle, stirring for 30-50min, standing for separating liquid, and washing the organic phase with 90kg of purified water for 3 times to obtain a tertiary dodecyl mercaptan crude product;
s6, adding the crude product of the tertiary dodecyl mercaptan into a feeding tower for rectification, and collecting fractions at 170-180 ℃ to obtain a tertiary dodecyl mercaptan finished product.
CN202310656801.2A 2023-06-05 2023-06-05 Reaction equipment and process for synthesizing tertiary dodecyl mercaptan by using dodecene catalysis Active CN116532052B (en)

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