CN112661735B - Continuous production system and method for methyltetrahydrophthalic anhydride - Google Patents
Continuous production system and method for methyltetrahydrophthalic anhydride Download PDFInfo
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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 29
- 238000010924 continuous production Methods 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 54
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000003054 catalyst Substances 0.000 claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 24
- 238000003860 storage Methods 0.000 claims abstract description 23
- 239000010409 thin film Substances 0.000 claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims description 21
- 238000006317 isomerization reaction Methods 0.000 claims description 16
- 238000009413 insulation Methods 0.000 claims description 10
- 238000003786 synthesis reaction Methods 0.000 claims description 10
- 230000015572 biosynthetic process Effects 0.000 claims description 7
- 238000012544 monitoring process Methods 0.000 claims description 6
- 238000005086 pumping Methods 0.000 claims description 6
- 238000012806 monitoring device Methods 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims description 2
- 239000010408 film Substances 0.000 claims 3
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 230000008569 process Effects 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 125000004432 carbon atom Chemical group C* 0.000 abstract 1
- 239000000047 product Substances 0.000 description 28
- 239000000463 material Substances 0.000 description 8
- 239000000376 reactant Substances 0.000 description 5
- 238000005457 optimization Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000004821 distillation Methods 0.000 description 3
- 239000003822 epoxy resin Substances 0.000 description 3
- 229920000647 polyepoxide Polymers 0.000 description 3
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 2
- 238000000199 molecular distillation Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- PMJHHCWVYXUKFD-SNAWJCMRSA-N (E)-1,3-pentadiene Chemical group C\C=C\C=C PMJHHCWVYXUKFD-SNAWJCMRSA-N 0.000 description 1
- LWMIDUUVMLBKQF-UHFFFAOYSA-N 4-methyl-3a,4,5,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound CC1CC=CC2C(=O)OC(=O)C12 LWMIDUUVMLBKQF-UHFFFAOYSA-N 0.000 description 1
- JDBDDNFATWXGQZ-UHFFFAOYSA-N 5-methyl-3a,4,5,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1=CC(C)CC2C(=O)OC(=O)C12 JDBDDNFATWXGQZ-UHFFFAOYSA-N 0.000 description 1
- 229920002732 Polyanhydride Polymers 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- SYSQUGFVNFXIIT-UHFFFAOYSA-N n-[4-(1,3-benzoxazol-2-yl)phenyl]-4-nitrobenzenesulfonamide Chemical class C1=CC([N+](=O)[O-])=CC=C1S(=O)(=O)NC1=CC=C(C=2OC3=CC=CC=C3N=2)C=C1 SYSQUGFVNFXIIT-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- PMJHHCWVYXUKFD-UHFFFAOYSA-N piperylene Natural products CC=CC=C PMJHHCWVYXUKFD-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000004382 potting Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000011949 solid catalyst Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a continuous production system and a continuous production method of methyl tetrahydrophthalic anhydride, wherein the production system comprises a tower reactor, a carbon five storage tank, a maleic anhydride storage tank, a thin film evaporator, a carbon five receiving tank, an adiabatic evaporator and a finished product tank, wherein the carbon five storage tank is connected with the tower reactor through a first magnetic pump, the maleic anhydride storage tank is connected with the tower reactor through a second magnetic pump, the tower reactor is connected with the thin film evaporator, the thin film evaporator comprises a steam outlet and a liquid outlet, the steam outlet is connected with the carbon five receiving tank through a first condenser, the liquid outlet is connected with the adiabatic evaporator, a catalyst fixer is arranged between the liquid outlet and the adiabatic evaporator, and the adiabatic evaporator is connected with the second condenser through a third magnetic pump and then is connected with the finished product tank. The continuous production system of the methyl tetrahydrophthalic anhydride truly realizes continuous production of the methyl tetrahydrophthalic anhydride, improves the efficiency by about 200 percent compared with the traditional process, has more thorough reaction, reduces the input of five carbon atoms, reduces the energy consumption and improves the yield and the quality of products.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a continuous production system and method of methyl tetrahydrophthalic anhydride.
Background
The liquid methyl tetrahydrophthalic anhydride has the characteristics of light color, difficult volatilization, low toxicity, stable performance, low solidifying point, long-term airtight storage at room temperature, low viscosity, good compatibility with various epoxy resins and the like, and the condensate thereof has excellent electrical property and heat resistance, and forms insulating potting materials and castable materials with the epoxy resins, fillers and the like, thereby being widely applied to the fields of electronic and electrical appliance industry, aerospace industry and the like. The methyl tetrahydrophthalic anhydride is prepared by the polymerization reaction of maleic anhydride, piperylene in C5 and isoprene, the product has 2 isomers, namely 4-methyl tetrahydrophthalic anhydride and 3-methyl tetrahydrophthalic anhydride, the melting points are 65 ℃ and 63 ℃, the methyl tetrahydrophthalic anhydride is seldom used as a curing agent independently, and the actual commercial product is a liquid mixture of a plurality of isomers.
The existing method for producing methyl tetrahydrophthalic anhydride at home and abroad is mainly an intermittent production process, has low automation degree, simultaneously generates carbon five self-polymers due to long-time stay reaction in a kettle in the previous maleic anhydride and carbon five synthesis process, needs to regularly clean the reaction kettle, and simultaneously generates a large amount of polyanhydride after distillation, thereby causing the problems of poor product quality stability, low efficiency, low yield and the like.
The Chinese patent application with application number 201711220925.7 discloses a device for continuously producing methyl tetrahydrophthalic anhydride, which is only provided with a detector and other testing devices based on the existing intermittent production process, and does not really realize continuous production of methyl tetrahydrophthalic anhydride.
The invention patent application of China with the application number of 201811320465.X discloses a process device for refining methyl tetrahydrophthalic anhydride by chemical synthesis and isomerization molecular distillation, which comprises an ultrasonic synthesis reaction kettle, a magnetic isomerization reaction kettle, a methyl tetrahydrophthalic anhydride cooling kettle, a short-range molecular distiller, a light fraction methyl tetrahydrophthalic anhydride tank, a heavy fraction polymeric resin tank and the like, wherein methyl tetrahydrophthalic anhydride is isomerized by the magnetic isomerization reaction kettle, and the isomerized methyl tetrahydrophthalic anhydride enters the short-range molecular distiller to be refined through the cooling methyl tetrahydrophthalic anhydride, so that the novel process for saving energy and reducing consumption by molecular distillation and cleaning of the methyl tetrahydrophthalic anhydride is achieved. The whole reaction is carried out sequentially in batches after a semi-finished product of one kettle is synthesized by the synthesis reaction kettle, and the like, so that the process belongs to the optimization and upgrading of the intermittent production process, the continuous production of the methyl tetrahydrophthalic anhydride is not really realized, and the problem of low efficiency exists.
Disclosure of Invention
In order to solve the technical problems, the invention adopts the following technical scheme: the continuous production system of the methyl tetrahydrophthalic anhydride comprises a tower reactor, a carbon five storage tank, a maleic anhydride storage tank, a thin film evaporator, a carbon five receiving tank, a heat insulation evaporator and a finished product tank, wherein the carbon five storage tank is connected with the tower reactor through a first magnetic pump, the maleic anhydride storage tank is connected with the tower reactor through a second magnetic pump, the tower reactor is connected with the thin film evaporator, the thin film evaporator comprises a steam outlet and a liquid outlet, the steam outlet is connected with the carbon five receiving tank through a first condenser, the liquid outlet is connected with the heat insulation evaporator, a catalyst fixer is arranged between the liquid outlet and the heat insulation evaporator, and the heat insulation evaporator is connected with the finished product tank through a third magnetic pump after being connected with the second condenser.
As the preferable mode of the technical scheme, a first flowmeter is arranged between the first magnetic pump and the tower reactor, and a second flowmeter is arranged between the second magnetic pump and the tower reactor.
As the optimization of the technical scheme, the production system further comprises a monitoring control system, the monitoring control system comprises a DCS, the DCS is connected with the first flowmeter and the second flowmeter, and the first magnetic pump, the second magnetic pump and the third magnetic pump are respectively connected with the DCS.
As the optimization of the technical scheme, the tower reactor is divided into a plurality of sections from top to bottom, and each section is provided with a heating device and a temperature monitoring device which are respectively connected with the DCS.
As the optimization of the technical scheme, the liquid outlet is connected with the heat insulation evaporator through a heat conduction oil heating jacket pipe, the catalyst fixer is arranged on the heat conduction oil heating jacket pipe, and the temperature of the heat conduction oil heating jacket pipe is controlled by the DCS.
The continuous production method of methyl tetrahydrophthalic anhydride uses the continuous production system, and comprises the following steps: storing carbon five in a carbon five storage tank, storing maleic anhydride in a maleic anhydride storage tank, and conveying specified amounts of carbon five and maleic anhydride to a tower reactor by using a first metering pump and a second metering pump respectively, wherein the molar ratio of maleic anhydride to carbon five is 1:1.03-1.10, controlling the synthesis temperature in a tower reactor to be 70-80 ℃, ensuring that the solution enters a thin film evaporator with the temperature controlled to be 100-120 ℃ after the residence time in the tower reactor is 30-40 seconds, condensing unreacted carbon five by a first condenser under a high vacuum state, pumping and recycling the condensed unreacted carbon five into a carbon five receiving tank, enabling liquid at the bottom of the thin film evaporator to enter a catalyst fixer with a catalyst at the temperature of 160-200 ℃ for isomerization reaction, then entering an adiabatic evaporator with the temperature controlled to be 130-140 ℃, condensing the gasified product by a second condenser, and collecting the condensed product in a finished product tank.
Preferably, the temperature of each section in the tower reactor is equal.
The beneficial effects of the invention are as follows: the continuous production system of the methyltetrahydrophthalic anhydride truly realizes continuous production of the methyltetrahydrophthalic anhydride. Compared with the conventional process (one 10m 3 4 batches of materials are produced at most in 24 hours), the continuous production system can produce about 100 tons of products in one day, and the improvement efficiency is about 200%; according to the accurate measurement of the maleic anhydride and the carbon five content, the reaction is more thorough, the carbon five input is reduced, and the proportion is close to the theoretical value; the occupied area of the device is smaller and the energy consumption is lower under the same output, so that the reconstruction problem of the prior old factory is solved; the residence time of the reactants is shortened, the yield of the catalyst product can reach 98.7 percent, and the yield is improved by about 5 percent; the quality stability of the product is improved, and the product does not change color in one year under the illumination condition; meanwhile, the novel large-particle solid catalyst is adopted, so that the isomerization degree is ensured to be more than 35%, and the influence of catalyst residues in a kettle on the product quality and yield during the later-stage reduced pressure distillation is avoided. Meanwhile, the influence of catalyst residues in a kettle on the quality and yield of products during the later reduced pressure distillation is avoided. The final product is detected, wherein the content of free acid is reduced to 0.04% from 0.1% of the common product, the glass transition temperature of the product and an epoxy resin system is increased to 105 ℃, the impact strength reaches 17-18 KJ/square meter, the tensile strength reaches 72MPa, and the bending strength reaches 130MPa. The smell of the product is greatly reduced, and the product plays a great role in protecting the environment and occupational health caused by downstream production.
Drawings
Fig. 1 is a schematic structural view of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made apparent and fully in view of the accompanying drawings, in which some, but not all embodiments of the invention are shown. 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.
In the description of the present invention, it should be noted that the directions or positional relationships indicated by the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. are based on the directions or positional relationships shown in the drawings, are merely for convenience of describing the present invention and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; 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 will be understood in specific cases by those of ordinary skill in the art.
Example 1
As shown in fig. 1, the continuous production system of methyl tetrahydrophthalic anhydride comprises a tower reactor 7, a carbon five storage tank 1, a maleic anhydride storage tank 2, a thin film evaporator 8, a carbon five receiving tank 10, an adiabatic evaporator 12 and a finished product tank 15, wherein the carbon five storage tank 1 is connected with the tower reactor 7 through a first magnetic pump 3, the maleic anhydride storage tank 2 is connected with the tower reactor 7 through a second magnetic pump 4, the tower reactor 7 is connected with the thin film evaporator 8, the thin film evaporator 8 comprises a steam outlet and a liquid outlet, the steam outlet is connected with the carbon five receiving tank 10 through a first condenser 9, the liquid outlet is connected with the adiabatic evaporator 12, a catalyst fixer 11 is arranged between the liquid outlet and the adiabatic evaporator 12, and the adiabatic evaporator 12 is connected with the finished product tank 15 after being connected with the second condenser 14 through a third magnetic pump 13.
Further, a first flowmeter 5 is arranged between the first magnetic pump 3 and the tower reactor 7, and a second flowmeter 6 is arranged between the second magnetic pump 4 and the tower reactor 7.
Further, the production system further comprises a monitoring control system, the monitoring control system comprises a DCS16, the DCS16 is connected with the first flowmeter 5 and the second flowmeter 6, and the first magnetic pump 3, the second magnetic pump 4 and the third magnetic pump 13 are respectively connected with the DCS16. The first flowmeter 5 and the second flowmeter 6 respectively control the carbon five and the maleic anhydride to enter the tower reactor 7 at a set flow rate, so as to control the proportion of the reacted carbon five and the maleic anhydride in the tower reactor 7 and control the residence time of the materials in the tower reactor 7.
Further, the tower reactor 7 is divided into a plurality of sections from top to bottom, and each section is provided with a heating device and a temperature monitoring device which are respectively connected with the DCS16. The sectional temperature control is adopted, so that the temperature of each section in the tower reactor 7 is similar, and excessive reaction temperature change of maleic anhydride and carbon five in the tower reactor 7 is avoided. Maleic anhydride and carbon five move in the tower reactor 7 from bottom to top, the maleic anhydride at the lower end of the tower reactor 7 reacts faster when the maleic anhydride and the carbon five are contacted at the beginning, the temperature rises by rapid heat release in the reaction process, the more upward reaction is, the less heat release is gradually reduced. The sectional temperature control is adopted, so that side reactions caused by overhigh temperature when maleic anhydride and carbon five are in contact are avoided.
Further, the liquid outlet is connected with the heat insulation evaporator 12 through a heat conduction oil heating jacket pipe, the catalyst fixer 11 is arranged on the heat conduction oil heating jacket pipe, and the temperature of the heat conduction oil heating jacket pipe is controlled by the DCS. The material is heated by heating the jacket tube with the heat transfer oil so that it can reach a set temperature when the isomerization reaction is performed with the catalyst in the catalyst holder 11.
Raw materials of carbon five and maleic anhydride respectively enter a tower reactor 7 through a first flowmeter 5 and a second flowmeter 6 according to a set proportion, an outlet of the tower reactor 7 is connected with an inlet of a thin film evaporator 8, redundant carbon five components are separated and recovered at a certain temperature and vacuum degree, and carbon five enters a carbon five recovery tank through a first condenser for recovery. The material outlet of the thin film evaporator 8 is connected with a heat conduction oil heating jacket pipe, and the heat conduction oil heating jacket pipe is used for heating the material. The material is then subjected to an isomerisation reaction using the catalyst in the catalyst holder 11, vaporised in the adiabatic evaporator 12 and finally condensed by the second condenser 14 before being collected in the re-product tank 15.
Example 2
The mole ratio of maleic anhydride to carbon five was 1:1.05 is respectively delivered to a tower reactor through a first metering pump and a second metering pump at 5T/h, the synthesis temperature in the tower reactor is controlled to be 70-75 ℃, the residence time of reactants in the tower reactor is ensured to be 40 seconds, the reactants enter a thin film evaporator with the temperature controlled to be 116-118 ℃, and unreacted carbon five is recovered by pumping and condensing under the state that the vacuum is more than-0.98 MPa. The bottom liquid enters a heat conducting oil heating jacket pipe with the temperature set to 170-175 ℃, enters a catalyst fixer with a catalyst for isomerization reaction after being heated, and then enters an insulated evaporator with the temperature controlled to 136-140 ℃. The gasified product is condensed and collected by a second condenser. Finally, the yield of the product is 98.92 percent, and the isomerization depth is 36.7 percent.
Example 3
The mole ratio of maleic anhydride to carbon five was 1:1.10 is delivered to a tower reactor by a metering pump at a speed of 4T/h, the synthesis temperature is controlled to be 70-73 ℃, the residence time of reactants in the tower reactor is ensured to be 30 seconds, the reactants enter a thin film evaporator with the temperature controlled to be 112-115 ℃, and unreacted carbon five is recovered by pumping and condensing under the state that the vacuum is more than-0.98 MPa. The bottom liquid enters a heat conducting oil heating jacket pipe with the temperature of 165-170 ℃, isomerization reaction is carried out in a catalyst fixer with a catalyst, then the bottom liquid enters an adiabatic evaporator with the temperature controlled between 132 and 135 ℃, and the gasified product is condensed and collected by a second condenser. Finally, the yield of the product is 98.73 percent and the isomerization depth is 35.8 percent.
Example 4
The mole ratio of maleic anhydride to carbon five was 1:1.03, delivering the raw materials to a tower reactor at 5T/h through a metering pump, controlling the synthesis temperature to be 75-80 ℃, ensuring that the raw materials enter a thin film evaporator with the temperature controlled at 120-123 ℃ after staying in the tower reactor for 40 seconds, and pumping out and condensing to recover unreacted carbon five under the state that the vacuum is more than-0.98 MPa. The bottom liquid enters a heat conducting oil heating jacket pipe through a pipeline at the temperature of 175-180 ℃, isomerization reaction is carried out in a catalyst fixer with a catalyst, then enters an adiabatic evaporator with the temperature controlled between 140 and 145 ℃, and the gasified product is condensed and collected through a condenser. Finally, the product yield is 98.76 percent and the isomerization depth is 38.9 percent.
Example 5
The mole ratio of maleic anhydride to carbon five was 1:1.05 is delivered to a tower reactor by a metering pump at 5T/h, the synthesis temperature is controlled to be 70-75 ℃, the residence time in the tower reactor 7 is ensured to be 40 seconds, the raw materials enter a thin film evaporator 8 with the temperature controlled to be 120-123 ℃, and unreacted carbon five is recovered by pumping and condensing under the state that the vacuum is more than-0.98 MPa. The bottom liquid enters a heat conducting oil heating jacket pipe through a pipeline at the temperature of 220-225 ℃, isomerization reaction is carried out in a catalyst fixer 11 with a catalyst, then enters an adiabatic evaporator with the temperature controlled between 136 and 140 ℃, and the gasified product is condensed and collected through a condenser. Finally, the product yield is 99.03 percent and the isomerization depth is 42.7 percent.
It should be noted that technical features such as a carbon five storage tank, a maleic anhydride storage tank, a magnetic pump, a flowmeter, a tower reactor, a thin film evaporator, a condenser, a carbon five receiving tank, a catalyst fixer, an adiabatic evaporator and the like related to the present application should be regarded as the prior art, and specific structures, working principles, control modes and spatial arrangement of the technical features may be selected conventionally in the art, and should not be regarded as the invention point of the present application, and the present application is not further specifically developed and detailed.
While the preferred embodiments of the present invention have been described in detail, it should be appreciated that numerous modifications and variations may be made in accordance with the principles of the present invention by those skilled in the art without undue burden, and thus, all technical solutions which may be obtained by logic analysis, reasoning or limited experimentation based on the principles of the present invention as defined by the claims are within the scope of protection as defined by the present invention.
Claims (4)
1. The continuous production system of the methyl tetrahydrophthalic anhydride is characterized by comprising a tower reactor, a carbon five storage tank, a maleic anhydride storage tank, a film evaporator, a carbon five receiving tank, a heat insulation evaporator and a finished product tank, wherein the carbon five storage tank is connected with the tower reactor through a first magnetic pump, the maleic anhydride storage tank is connected with the tower reactor through a second magnetic pump, the tower reactor is connected with the film evaporator, the film evaporator comprises a steam outlet and a liquid outlet, the steam outlet is connected with the carbon five receiving tank through a first condenser, the liquid outlet is connected with the heat insulation evaporator, a catalyst fixer is arranged between the liquid outlet and the heat insulation evaporator, the heat insulation evaporator is connected with the second condenser through a third magnetic pump and then is connected with the finished product tank, a first flowmeter is arranged between the first magnetic pump and the tower reactor, a second flowmeter is arranged between the second magnetic pump and the tower reactor, the production system further comprises a monitoring control system, the monitoring control system is connected with the first flowmeter and the second flowmeter, the first magnetic pump, the second magnetic pump and the third magnetic pump are respectively connected with the DCS, the tower reactor is provided with a plurality of heating devices from top to bottom, and a plurality of heating devices are respectively connected with the monitoring devices.
2. The continuous production system of methyltetrahydrophthalic anhydride according to claim 1, wherein the liquid outlet is connected to the adiabatic evaporator through a conduction oil heating jacket tube, the catalyst holder is mounted on the conduction oil heating jacket tube, and the temperature of the conduction oil heating jacket tube is controlled by DCS.
3. Continuous production method of methyltetrahydrophthalic anhydride, characterized in that it uses the continuous production system according to any one of claims 1-2, comprising the following steps: storing carbon five in a carbon five storage tank, storing maleic anhydride in a maleic anhydride storage tank, and conveying specified amounts of carbon five and maleic anhydride to a tower reactor by using a first metering pump and a second metering pump respectively, wherein the molar ratio of maleic anhydride to carbon five is 1:1.03-1.10, controlling the synthesis temperature in a tower reactor to be 70-80 ℃, ensuring that the solution enters a thin film evaporator with the temperature controlled to be 100-120 ℃ after the residence time in the tower reactor is 30-40 seconds, condensing unreacted carbon five by a first condenser under a high vacuum state, pumping and recycling the condensed unreacted carbon five into a carbon five receiving tank, enabling liquid at the bottom of the thin film evaporator to enter a catalyst fixer with a catalyst at the temperature of 160-200 ℃ for isomerization reaction, then entering an adiabatic evaporator with the temperature controlled to be 130-140 ℃, condensing the gasified product by a second condenser, and collecting the condensed product in a finished product tank.
4. The continuous production method of methyltetrahydrophthalic anhydride as in claim 3, wherein the temperature of each section in the tower reactor is equal.
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Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1600836A (en) * | 1967-07-12 | 1970-08-03 | Methyl-1,2,3,6-tetrahydrophthalic acid anhydride | |
| US6225475B1 (en) * | 2000-08-18 | 2001-05-01 | Albemarle Corporation | Enhanced production of hydrocarbyl anhydrides |
| CN1683353A (en) * | 2005-03-11 | 2005-10-19 | 河南省科学院化学研究所 | New process for producing liquid methyl tetrahydro phthalic anhydride |
| CN1772327A (en) * | 2004-11-11 | 2006-05-17 | 中国石化上海石油化工股份有限公司 | Waste liquid separating method for tetrahydro methyl phthalic anhydride production process |
| CN202465566U (en) * | 2011-11-29 | 2012-10-03 | 杭州中泰深冷技术股份有限公司 | Crude methyl tetrahydrophthalic anhydride continuous production device |
| CN102977060A (en) * | 2012-12-11 | 2013-03-20 | 南通市福来特化工有限公司 | Method for producing liquid methyl tetrahydrophthalic anhydride |
| CN203820669U (en) * | 2014-04-29 | 2014-09-10 | 浙江阿尔法化工科技有限公司 | Production system of methyl tetrahydrophthalic anhydride |
| CN204051368U (en) * | 2014-08-05 | 2014-12-31 | 嘉兴市正大化工有限公司 | carbon five tail gas recycling and treating device |
| CN104645922A (en) * | 2013-11-15 | 2015-05-27 | 嘉兴市南洋塑料化工有限公司 | Novel isomerization kettle for producing methyl tetrahydrophthalic anhydride and method therewith for quickly cooling isomerization material |
| CN205774230U (en) * | 2016-05-20 | 2016-12-07 | 浙江正大新材料科技有限公司 | The device of continuous prodution methyl tetrahydro phthalic anhydride |
| CN109158067A (en) * | 2018-11-07 | 2019-01-08 | 郭继波 | A kind of chemical industry synthesis isomery molecular distillation purification methyl tetrahydro phthalic anhydride process unit |
| CN209287315U (en) * | 2018-11-22 | 2019-08-23 | 山东清洋新材料有限公司 | The device of continuous production methyl tetrahydro phthalic anhydride |
| CN211536582U (en) * | 2019-12-26 | 2020-09-22 | 嘉兴南洋万事兴化工有限公司 | A five processing systems of carbon for in maleic anhydride is synthetic |
| CN111732564A (en) * | 2020-06-13 | 2020-10-02 | 嘉兴南洋万事兴化工有限公司 | Method and synthesis system for preparing methyltetrahydrophthalic anhydride |
-
2021
- 2021-01-15 CN CN202110052208.8A patent/CN112661735B/en active Active
Patent Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1600836A (en) * | 1967-07-12 | 1970-08-03 | Methyl-1,2,3,6-tetrahydrophthalic acid anhydride | |
| US6225475B1 (en) * | 2000-08-18 | 2001-05-01 | Albemarle Corporation | Enhanced production of hydrocarbyl anhydrides |
| CN1772327A (en) * | 2004-11-11 | 2006-05-17 | 中国石化上海石油化工股份有限公司 | Waste liquid separating method for tetrahydro methyl phthalic anhydride production process |
| CN1683353A (en) * | 2005-03-11 | 2005-10-19 | 河南省科学院化学研究所 | New process for producing liquid methyl tetrahydro phthalic anhydride |
| CN202465566U (en) * | 2011-11-29 | 2012-10-03 | 杭州中泰深冷技术股份有限公司 | Crude methyl tetrahydrophthalic anhydride continuous production device |
| CN102977060A (en) * | 2012-12-11 | 2013-03-20 | 南通市福来特化工有限公司 | Method for producing liquid methyl tetrahydrophthalic anhydride |
| CN104645922A (en) * | 2013-11-15 | 2015-05-27 | 嘉兴市南洋塑料化工有限公司 | Novel isomerization kettle for producing methyl tetrahydrophthalic anhydride and method therewith for quickly cooling isomerization material |
| CN203820669U (en) * | 2014-04-29 | 2014-09-10 | 浙江阿尔法化工科技有限公司 | Production system of methyl tetrahydrophthalic anhydride |
| CN204051368U (en) * | 2014-08-05 | 2014-12-31 | 嘉兴市正大化工有限公司 | carbon five tail gas recycling and treating device |
| CN205774230U (en) * | 2016-05-20 | 2016-12-07 | 浙江正大新材料科技有限公司 | The device of continuous prodution methyl tetrahydro phthalic anhydride |
| CN109158067A (en) * | 2018-11-07 | 2019-01-08 | 郭继波 | A kind of chemical industry synthesis isomery molecular distillation purification methyl tetrahydro phthalic anhydride process unit |
| CN209287315U (en) * | 2018-11-22 | 2019-08-23 | 山东清洋新材料有限公司 | The device of continuous production methyl tetrahydro phthalic anhydride |
| CN211536582U (en) * | 2019-12-26 | 2020-09-22 | 嘉兴南洋万事兴化工有限公司 | A five processing systems of carbon for in maleic anhydride is synthetic |
| CN111732564A (en) * | 2020-06-13 | 2020-10-02 | 嘉兴南洋万事兴化工有限公司 | Method and synthesis system for preparing methyltetrahydrophthalic anhydride |
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