CN114432993B - Synthesis process and synthesis equipment of methyltetrahydrophthalic anhydride - Google Patents
Synthesis process and synthesis equipment of methyltetrahydrophthalic anhydride Download PDFInfo
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- CN114432993B CN114432993B CN202210085973.4A CN202210085973A CN114432993B CN 114432993 B CN114432993 B CN 114432993B CN 202210085973 A CN202210085973 A CN 202210085973A CN 114432993 B CN114432993 B CN 114432993B
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- MWSKJDNQKGCKPA-UHFFFAOYSA-N 6-methyl-3a,4,5,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1CC(C)=CC2C(=O)OC(=O)C12 MWSKJDNQKGCKPA-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 30
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 19
- 230000008569 process Effects 0.000 title claims abstract description 18
- 238000004821 distillation Methods 0.000 claims abstract description 47
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 14
- 239000003054 catalyst Substances 0.000 claims description 12
- 229910052759 nickel Inorganic materials 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 6
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 5
- 229910052801 chlorine Inorganic materials 0.000 claims description 5
- 239000000460 chlorine Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 4
- 229910000838 Al alloy Inorganic materials 0.000 claims description 3
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 claims description 3
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 claims description 3
- 229940092714 benzenesulfonic acid Drugs 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 239000002638 heterogeneous catalyst Substances 0.000 claims description 3
- 238000005984 hydrogenation reaction Methods 0.000 claims description 3
- 230000009467 reduction Effects 0.000 claims description 3
- 238000007670 refining Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 230000002194 synthesizing effect Effects 0.000 claims description 3
- 230000007306 turnover Effects 0.000 claims description 3
- 235000005074 zinc chloride Nutrition 0.000 claims description 3
- 239000011592 zinc chloride Substances 0.000 claims description 3
- 230000007246 mechanism Effects 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 abstract description 7
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- 239000003822 epoxy resin Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229920000647 polyepoxide Polymers 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
- A61L2/16—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using chemical substances
- A61L2/18—Liquid substances or solutions comprising solids or dissolved gases
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/06—Flash distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto
- B08B9/02—Cleaning pipes or tubes or systems of pipes or tubes
- B08B9/027—Cleaning the internal surfaces; Removal of blockages
- B08B9/04—Cleaning the internal surfaces; Removal of blockages using cleaning devices introduced into and moved along the pipes
- B08B9/053—Cleaning the internal surfaces; Removal of blockages using cleaning devices introduced into and moved along the pipes moved along the pipes by a fluid, e.g. by fluid pressure or by suction
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/77—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D307/87—Benzo [c] furans; Hydrogenated benzo [c] furans
- C07D307/89—Benzo [c] furans; Hydrogenated benzo [c] furans with two oxygen atoms directly attached in positions 1 and 3
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The invention discloses a synthesis process and synthesis equipment of methyl tetrahydrophthalic anhydride, which comprises a reaction kettle, an air inlet pipe, a feed pipe, a distillation pipe and a collecting bottle, wherein the air inlet pipe and the feed pipe are arranged at the top of the reaction kettle, the distillation pipe is connected to the right side of the top of the reaction kettle, a sliding block is slidably connected in an inner cavity of the distillation pipe, annular cone blocks are arranged at the periphery of two ends of the sliding block, an inner pipe is arranged in the inner cavity of the sliding block, a connecting pipe is arranged in an inner cavity at a right bent angle of the distillation pipe, a communicating pipe is arranged at the left side of the bottom of the distillation pipe, an air bag is arranged at the lower part of the communicating pipe, when the distillation pipe is heated and stirred, hot steam can push the sliding block to slide in the inner cavity of the distillation pipe, the inner wall of the distillation pipe can be automatically cleaned, air in the right space of the sliding block is extruded into the air bag, after the heating is stopped, the air pressure in the air bag is reduced, the air is refluxed, the sliding block is pushed to reset, and then the air pressure in the distillation pipe is kept balanced, and the service life of the distillation pipe can be prolonged.
Description
Technical Field
The invention relates to the technical field of preparation of methyl tetrahydrophthalic anhydride, in particular to a synthesis process and synthesis equipment of methyl tetrahydrophthalic anhydride.
Background
The liquid methyl tetrahydrophthalic anhydride is an excellent curing agent for epoxy resin, has the characteristics of low melting point, low toxicity, low volatility and the like, is convenient to use, has high reaction activity with the epoxy resin and good miscibility, and an epoxy resin cured product using the curing agent has excellent electrical insulation performance and mechanical performance, and has good market prospect along with the continuous improvement of the requirements of the motor, electronics and electric appliance industries on the reliability of the insulation performance in recent years.
Most of the existing methyl tetrahydrophthalic anhydride synthesis adopts a distillation mode, gas methyl tetrahydrophthalic anhydride is conveyed into a collecting bottle through a distillation tube in synthesis equipment and is liquefied into liquid methyl tetrahydrophthalic anhydride when being cooled, but stains possibly occur on the inner wall of the distillation tube in the existing equipment when the distillation tube is used, the automatic cleaning cannot be carried out, and in the use process, the internal air pressure is changed when hot steam passes through the distillation tube, the pressure is unbalanced, and the service life of the distillation tube is influenced.
Disclosure of Invention
The invention aims to provide a synthesis process and synthesis equipment of methyl tetrahydrophthalic anhydride, which are used for solving the problems in the background technology.
In order to achieve the above purpose, the present invention provides the following technical solutions: the methyl tetrahydrophthalic anhydride synthesis equipment comprises a reaction kettle, an air inlet pipe, a feed pipe, a distillation pipe and a collecting bottle, wherein the air inlet pipe and the feed pipe are arranged at the top of the reaction kettle;
the inner cavity sliding connection of distillation tube has the sliding block, the periphery at sliding block both ends is provided with annular cone piece, the inner cavity of sliding block is provided with the inner tube, the inner cavity of distillation tube right side bent angle department is provided with the connecting tube, the left side of distillation tube bottom is provided with communicating pipe, the lower part of communicating pipe is provided with the gasbag.
Preferably, the right side of inner tube is connected with the lug, the right side fixedly connected with branch pipe of lug outer lane, the left side of linking pipe is provided with the second lug, the outside of second lug is provided with the dog, the output hole has been seted up to the inboard of dog, the output hole is put through with the inner chamber of linking pipe.
Preferably, the branch pipes and the check blocks are respectively provided with six groups, the six groups are correspondingly arranged, and when the sliding block slides to the right side, the branch pipes are tightly connected with the output holes.
Preferably, a notch is formed in the left end of the outer ring of the inner tube, a rectangular block is connected to the inner wall of the notch, a turning block is connected to the right bearing of the notch, a spring is connected between the turning block and the rectangular block, and the lengths of the inner tube and the sliding block are equal.
Preferably, the inner wall of the sliding block is provided with a groove, the right side of the groove and the outer wall of the inner tube corresponding to the groove are respectively provided with a hook, and a tension spring is connected between the two groups of hooks.
Preferably, the chlorine-containing solution is arranged in the air bag, and the top of the air bag is provided with a threaded rod and is in threaded connection with the communicating pipe through the threaded rod.
Preferably, the synthesis process of the methyltetrahydrophthalic anhydride comprises the following steps:
step one: CS and maleic anhydride are used as raw materials to react to prepare crude methyltetrahydrophthalic anhydride;
step two: adding a nickel-based catalyst and a base catalyst into the reaction kettle to realize hydrogenation reduction
Step three: and distilling to obtain methyl tetrahydrophthalic anhydride.
Preferably, when preparing the crude methyltetrahydrophthalic anhydride in the first step, after CS and maleic anhydride raw materials are added, the temperature of the reaction kettle is controlled between 160 ℃ and 220 ℃, and flash evaporation refining is carried out under the condition that the vacuum degree is negative 0.070-0.095 MPa.
Preferably, the nickel-based catalyst in the second step is a solid heterogeneous catalyst composed of fine grains of nickel-aluminum alloy with a porous structure, and the base catalyst is specifically one of benzenesulfonic acid and zinc chloride.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the synthesis process and the synthesis equipment of the methyl tetrahydrophthalic anhydride, when heating and stirring are carried out, after hot steam enters the distillation tube, internal air is heated and expanded and can push the sliding block to slide in the inner cavity of the distillation tube, in the pushing process, the annular cone block is tangent to the inner wall of the distillation tube, the inner wall of the distillation tube can be automatically cleaned, air in the space on the right part of the sliding block is extruded into the air bag, after heating is stopped, air pressure in the air bag is reduced, air flows back, the sliding block is pushed to reset, and then the air pressure balance in the distillation tube is kept, so that the service life of the distillation tube can be prolonged.
2. According to the synthesis process and synthesis equipment of the methyltetrahydrophthalic anhydride, when the sliding block slides to the right side, the branch pipe is tightly connected with the output hole, at the moment, the space on the right side of the sliding block is blocked by the stop block and is closed, the rest gas can only rotate along the outer surfaces of the convex block and the second convex block to form vortex, and finally scraped inner wall dirt is collected into the air bag along with the air flow.
3. According to the synthesis process and synthesis equipment of the methyltetrahydrophthalic anhydride, the tension spring is connected between the hooks, after heating is stopped, the air pressure in the air bag is reduced, air flows back, the sliding block is pushed to reset, the branch pipe is separated from the thrust of the stop block, the left end of the inner pipe is retracted to the inner cavity of the sliding block again due to rebound of the tension spring, and when the inner pipe is stationary, the notch is in a closed state, so that dirt entering the inner pipe can be avoided.
4. According to the synthesis process and the synthesis equipment of the methyltetrahydrophthalic anhydride, after stains enter the air bag along with the airflow, the airflow is slowed down, the stains drop and are attached to the inner wall of the air bag, chlorine-containing solution can sterilize and disinfect the stains, and then the air bag can be replaced by unscrewing the threaded rod.
Drawings
FIG. 1 is a schematic diagram of the apparatus for synthesizing methyltetrahydrophthalic anhydride according to the present invention;
FIG. 2 is a cross-sectional view of a distillation tube according to the present invention;
FIG. 3 is a schematic view of the structure of the inner tube of the present invention;
FIG. 4 is an enlarged view of a portion of FIG. 3A in accordance with the present invention;
FIG. 5 is a schematic view of the structure of the connecting pipe of the present invention;
FIG. 6 is a cross-sectional view of a slider of the present invention.
In the figure: 1. a reaction kettle; 2. an air inlet pipe; 3. a feed pipe; 4. a distillation tube; 5. a collection bottle; 6. a motor; 7. a sliding block; 71. an annular cone block; 73. an inner tube; 74. a bump; 75. a branch pipe; 76. a groove; 77. a hook; 78. a tension spring; 8. a connecting pipe; 81. a second bump; 82. a stop block; 83. an output aperture; 9. a notch; 91. rectangular blocks; 92. a turnover block; 93. a spring; 10. a communicating pipe; 11. an air bag.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but 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 and 2, the present invention provides a technical solution: the methyl tetrahydrophthalic anhydride synthesis equipment comprises a reaction kettle 1, an air inlet pipe 2, a feed pipe 3, a distillation pipe 4 and a collecting bottle 5, wherein the air inlet pipe 2 and the feed pipe 3 are arranged at the top of the reaction kettle 1, the distillation pipe 4 is connected to the right side of the top of the reaction kettle 1, the right end of the distillation pipe 4 is connected with the collecting bottle 5, a motor 6 is further arranged in the middle of the top of the reaction kettle 1, and an output shaft of the motor 6 is connected with a stirring mechanism; the inner cavity sliding connection of distillation tube 4 has slider 7, the periphery at slider 7 both ends is provided with annular awl piece 71, slider 7's inner chamber is provided with inner tube 73, distillation tube 4 right side bent angle department's inner chamber is provided with connecting pipe 8, distillation tube 4 bottom's left side is provided with communicating pipe 10, the lower part of communicating pipe 10 is provided with gasbag 11, when methyl tetrahydrophthalic anhydride mixes the preparation, add raw materials into reation kettle 1 through inlet pipe 3, heat and stir, the hot steam that the heating produced is collected in collecting bottle 5 through distillation tube 4 can obtain the methyl tetrahydrophthalic anhydride of liquid, after the hot steam gets into distillation tube 4, inside air is heated and is expanded and can promote slider 7 in distillation tube 4's inner chamber slip, in-process annular awl piece 71 is tangent with distillation tube 4's inner wall, can carry out automatic clearance to distillation tube 4's inner wall, and the air in slider 7 right part space is pressed into gasbag 11, stop heating after the internal atmospheric pressure of gasbag 11 diminishes, gaseous backward flow, can promote slider 7 to reset, then keep distillation tube 4 inside atmospheric pressure balance, can increase distillation tube 4's life.
Referring to fig. 2, 3 and 5, the right side of the inner tube 73 is connected with a bump 74, the right side of the outer ring of the bump 74 is fixedly connected with a branch tube 75, the left side of the connecting tube 8 is provided with a second bump 81, the outer part of the second bump 81 is provided with a stop block 82, the inner side of the stop block 82 is provided with an output hole 83, the output hole 83 is communicated with the inner cavity of the connecting tube 8, the branch tube 75 and the stop block 82 are respectively provided with six groups, when the sliding block 7 slides to the right side, the branch tube 75 is tightly connected with the output hole 83, at this time, the space on the right side of the sliding block 7 is blocked by the stop block 82 and is closed, the rest of gas can only rotate along the outer surfaces of the vortex bump 74 and the second bump 81 to form a scraping inner wall dirt which is finally collected into the air bag 11 along with the airflow.
Referring to fig. 3 and 4, a notch 9 is formed at the left end of the outer ring of the inner tube 73, a rectangular block 91 is connected to the inner wall of the notch 9, a turning block 92 is connected to the right bearing of the notch 9, a spring 93 is connected between the turning block 92 and the rectangular block 91, the length of the inner tube 73 is equal to that of the sliding block 7, the branch tube 75 is tightly connected with the output hole 83, when the inner tube is pushed continuously, the pushing force from the right stop 82 can push the left side of the inner tube 73 out of the inner cavity of the sliding block 7, then the turning block 92 is pushed up by the elastic force of the spring 93, the notch 9 is opened, the notch 9, the branch tube 75 and the output hole 83 are connected, and steam enters from the notch 9 to collect methyl tetrahydrophthalic anhydride.
Referring to fig. 6, a groove 76 is formed in the inner wall of the sliding block 7, hooks 77 are respectively arranged on the right side of the groove 76 and the outer wall of the inner tube 73 corresponding to the groove 76, a tension spring 78 is connected between the two groups of hooks 77, after heating is stopped, the air pressure in the air bag 11 becomes small, air flows back, the sliding block 7 is pushed to reset, the branch tube 75 is separated from the thrust of the stop block 82, the tension spring 78 rebounds to enable the left end of the inner tube 73 to be retracted into the inner cavity of the sliding block 7 again, and when the sliding block is stationary, the notch 9 is in a closed state, so that dirt entering into the inner tube 73 can be avoided.
Referring to fig. 2, a chlorine-containing solution is disposed in the air bag 11, a threaded rod is disposed at the top of the air bag 11 and is in threaded connection with the communicating pipe 10, after the dirt enters the air bag 11 along with the air flow, the air flow is slowed down, the dirt falls down and adheres to the inner wall of the air bag 11, the chlorine-containing solution can sterilize the dirt, and then the air bag 11 can be replaced by unscrewing the threaded rod.
Example 2: a synthesis process of methyl tetrahydrophthalic anhydride comprises the following steps:
step one: CS and maleic anhydride are used as raw materials to react to prepare crude methyl tetrahydrophthalic anhydride, wherein after CS and maleic anhydride raw materials are added, the temperature of a reaction kettle 1 is controlled between 160 ℃ and 220 ℃, and flash evaporation refining is carried out under the condition that the vacuum degree is negative 0.070-0.095 MPa;
step two: adding a nickel-based catalyst and a base catalyst into the reaction kettle 1 to realize hydrogenation reduction, wherein the nickel-based catalyst is a solid heterogeneous catalyst consisting of fine grains of nickel-aluminum alloy with a porous structure, and the base catalyst is specifically one of benzenesulfonic acid and zinc chloride.
Step three: and distilling to obtain methyl tetrahydrophthalic anhydride.
In the description of the present invention, it should also be noted that, unless explicitly specified and limited otherwise, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. The utility model provides a methyl tetrahydrophthalic anhydride synthesis equipment, includes reation kettle (1), intake pipe (2), inlet pipe (3), distillation tube (4), collecting bottle (5), its characterized in that: the device is characterized in that an air inlet pipe (2) and a feed pipe (3) are arranged at the top of the reaction kettle (1), the distillation pipe (4) is connected to the right side of the top of the reaction kettle (1), the right end of the distillation pipe (4) is connected with a collecting bottle (5), a motor (6) is further arranged in the middle of the top of the reaction kettle (1), and an output shaft of the motor (6) is connected with a stirring mechanism;
the inner cavity of the distillation tube (4) is slidably connected with a sliding block (7), the peripheries of two ends of the sliding block (7) are provided with annular cone blocks (71), the inner cavity of the sliding block (7) is provided with an inner tube (73), the inner cavity at the right corner of the distillation tube (4) is provided with a connecting tube (8), the left side of the bottom of the distillation tube (4) is provided with a communicating tube (10), and the lower part of the communicating tube (10) is provided with an air bag (11);
the right side of the inner tube (73) is connected with a lug (74), the right side of the outer ring of the lug (74) is fixedly connected with a branch tube (75), the left side of the connecting tube (8) is provided with a second lug (81), the outer part of the second lug (81) is provided with a stop block (82), the inner side of the stop block (82) is provided with an output hole (83), and the output hole (83) is communicated with the inner cavity of the connecting tube (8);
a notch (9) is formed in the left end of the outer ring of the inner tube (73), a rectangular block (91) is connected to the inner wall of the notch (9), a turnover block (92) is connected to the right bearing of the notch (9), and a spring (93) is connected between the turnover block (92) and the rectangular block (91);
the inner wall of the sliding block (7) is provided with a groove (76), the right side of the groove (76) and the outer wall of the inner tube (73) corresponding to the groove (76) are respectively provided with a hook (77), and a tension spring (78) is connected between the two groups of hooks (77).
2. The methyltetrahydrophthalic anhydride synthesis device according to claim 1, wherein: the branch pipes (75) and the stop blocks (82) are respectively provided with six groups, the six groups are correspondingly arranged, and when the sliding block (7) slides to the right side, the branch pipes (75) are tightly connected with the output holes (83).
3. The methyltetrahydrophthalic anhydride synthesis device according to claim 1, wherein: the length of the inner tube (73) is equal to that of the sliding block (7).
4. The methyltetrahydrophthalic anhydride synthesis device according to claim 1, wherein: the air bag (11) is internally provided with chlorine-containing solution, and the top of the air bag (11) is provided with a threaded rod and is in threaded connection with the communicating pipe (10) through the threaded rod.
5. The synthesis process of methyl tetrahydrophthalic anhydride is characterized by comprising the following steps:
step one: CS and maleic anhydride are used as raw materials to react to prepare crude methyltetrahydrophthalic anhydride;
step two: adding a nickel-based catalyst and a base catalyst into the reaction kettle (1) to realize hydrogenation reduction, wherein the reaction kettle (1) is the reaction kettle (1) included in the methyl tetrahydrophthalic anhydride synthesis equipment according to any one of claims 1-4;
step three: and distilling to obtain methyl tetrahydrophthalic anhydride.
6. The process for synthesizing methyltetrahydrophthalic anhydride according to claim 5, wherein the process is characterized by: when the crude methyl tetrahydrophthalic anhydride is prepared in the first step, after CS and maleic anhydride raw materials are added, the temperature of the reaction kettle (1) is controlled between 160 ℃ and 220 ℃, and flash evaporation refining is carried out under the condition that the vacuum degree is negative 0.070-0.095 MPa.
7. The process for synthesizing methyltetrahydrophthalic anhydride according to claim 5, wherein the process is characterized by: the nickel-based catalyst in the second step is a solid heterogeneous catalyst consisting of fine grains of nickel-aluminum alloy with a porous structure, and the nickel-based catalyst is specifically one of benzenesulfonic acid and zinc chloride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210085973.4A CN114432993B (en) | 2022-01-25 | 2022-01-25 | Synthesis process and synthesis equipment of methyltetrahydrophthalic anhydride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210085973.4A CN114432993B (en) | 2022-01-25 | 2022-01-25 | Synthesis process and synthesis equipment of methyltetrahydrophthalic anhydride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114432993A CN114432993A (en) | 2022-05-06 |
| CN114432993B true CN114432993B (en) | 2024-01-30 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202210085973.4A Active CN114432993B (en) | 2022-01-25 | 2022-01-25 | Synthesis process and synthesis equipment of methyltetrahydrophthalic anhydride |
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