CN205774230U - The device of continuous prodution methyl tetrahydro phthalic anhydride - Google Patents
The device of continuous prodution methyl tetrahydro phthalic anhydride Download PDFInfo
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- CN205774230U CN205774230U CN201620469855.3U CN201620469855U CN205774230U CN 205774230 U CN205774230 U CN 205774230U CN 201620469855 U CN201620469855 U CN 201620469855U CN 205774230 U CN205774230 U CN 205774230U
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Abstract
The device of a kind of continuous prodution methyl tetrahydro phthalic anhydride, including four diene synthesis reactors, five pipe bundle condensers, two falling film evaporators, a membrane evaporator, five dosing pumps, three material pumps and nine various storage tanks.With the second dosing pump (502), cis-butenedioic anhydride is inputted in the first diene still (101), react with excess carbon five active component reclaimed in carbon five come from the 4th diene still (104), sequentially enter the second diene still (102), the 3rd diene still (103) and the 4th diene still the most again, with carbon five reaction being newly added, then it is isolated to methyl tetrahydro phthalic anhydride product.Can realize making full use of of carbon five resource, reduce the formation of oligomer in building-up process, operating process auto-control degree is high, and reacting balance can improve properties of product, reduces production cost, improves production efficiency.
Description
Technical field
This utility model relates to the industrial production device of a kind of methyl tetrahydro phthalic anhydride, belongs to fine chemistry industry and produces equipment and technology
Field, the device of a kind of continuous prodution methyl tetrahydro phthalic anhydride.
Background technology
Methyl tetrahydro phthalic anhydride is a very important kind of anhydrides among epoxy curing agent, is also methyl hexahydro
The raw materials for production of phthalic anhydride.It compares with other acid anhydride type curing agents, has purity height, lighter color, the most volatile, toxicity
Little, stable performance, length working life, freezing point are low, can the most airtight deposit under room temperature, viscosity low and with all kinds of asphalt mixtures modified by epoxy resin
Fat has the features such as good intermiscibility, and its solidfied material has excellent electrical property and thermostability, with epoxy resin, filler etc.
Composition insulation filling material, castable, be widely used in the fields such as electronic apparatus industry, aerospace industries.Methyl tetrahydrochysene
Phthalic anhydride is carried out polyreaction by cis-butenedioic anhydride with the pentadiene in carbon five, isoprene and prepares.Produce methyl both at home and abroad at present
The method of THPA is mainly batch process production technology.Though batch process production technology have little interracial switching convenient,
Quickly advantage, but automaticity is low, and constant product quality is poor, fluctuation is big, and during synthesis, technique is unstable, causes
Oligomer is formed and is difficult in subsequent technique remove, and finally affects product color, viscosity, fugitive constituent, and active component mistake
Amount, frequent input and output material, operation complexity, exhaust emissions are unstable, cause raw material, energy resource consumption big, and yield is relatively small.
Summary of the invention
This utility model is directed to the device of a kind of continuous prodution methyl tetrahydro phthalic anhydride, can realize the abundant of carbon five resource
Utilize, reduce the formation of oligomer in building-up process, improve properties of product, reduce production cost, improve and produce
Efficiency.
The device of this continuous prodution methyl tetrahydro phthalic anhydride include four diene synthesis reactors, five pipe bundle condensers,
Two falling film evaporators, a membrane evaporator, five dosing pumps, three material pumps and nine various storage tanks, wherein dienes
Synthesis reaction vessel includes the first diene still, the second diene still, the 3rd diene still and the 4th diene still；Entering of second dosing pump
Mouth is the input port of cis-butenedioic anhydride, and the first charging aperture of the second metering delivery side of pump and the first diene still is connected, the first diene still top
The gaseous phase outlet in portion with refluxing opening respectively inlet and outlet with the first pipe bundle condenser be connected；The liquid phase of the first diene still is overflow
Head piece is connected by the import of the 3rd dosing pump and the first falling film evaporator, and the liquid-phase outlet of the first falling film evaporator is with middle
The import of groove is connected, and the gaseous phase outlet of the first falling film evaporator and the import of the second pipe bundle condenser are connected, and the second tubulation is cold
The outlet of condenser is connected with by-product carbon five receiving slit；The outlet of medial launder is by the 4th dosing pump and the first of the second diene still
Charging aperture is connected, and the liquid phase overfall of the second diene still and the first charging aperture of the 3rd diene still are connected, the 3rd diene still
First charging aperture of liquid phase overfall and the 4th diene still is connected, the liquid phase overfall of the 4th diene still and the import of dashpot
It is connected；The input port that import is carbon five of the 5th dosing pump, the 5th metering delivery side of pump respectively with the second of the second diene still
Charging aperture, the second charging aperture of the 3rd diene still, the second charging aperture of the 4th diene still are connected, the second diene still, the 3rd
Diene still, the 4th diene still have the import of gas phase pipeline and the 3rd pipe bundle condenser to be connected with the top of dashpot respectively,
The liquid-phase outlet of the 3rd pipe bundle condenser and the second diene still are connected；The liquid-phase outlet of dashpot passes through the first material pump and second
The import of falling film evaporator is connected, and the gaseous phase outlet of the second falling film evaporator is counted with reclaiming carbon five by the 4th pipe bundle condenser
The import of measuring tank is connected, and the outlet reclaiming carbon five measuring tank is connected with the import reclaiming carbon five storage tank, reclaims carbon five storage tank
Outlet be connected with the import of the first dosing pump, first metering delivery side of pump and the first diene still the second charging aperture be connected；
The liquid-phase outlet of the second falling film evaporator is connected with the import of crude product groove, and the outlet of crude product groove is by the second material pump and thin film
The import of vaporizer is connected, and the gaseous phase outlet of membrane evaporator and the import of the 5th pipe bundle condenser are connected, membrane evaporator
Liquid-phase outlet be connected with the import of methyl tetrahydro phthalic anhydride groove, the liquid-phase outlet of the 5th pipe bundle condenser and Light ends groove
Import be connected, the gaseous phase outlet of the 5th pipe bundle condenser is connected with the import of vacuum buffer tank；Methyl tetrahydro phthalic anhydride is subject to
Trench bottom outlet is connected with the import of the 3rd material pump, and the 3rd material delivery side of pump is the outlet of methyl tetrahydro phthalic anhydride product.
Cis-butenedioic anhydride is inputted in the first diene still with the second dosing pump by the device of this continuous prodution methyl tetrahydro phthalic anhydride, with from
Excess carbon five active component reclaimed in carbon five reaction that 4th diene still comes, sequentially enter the most again the second diene still, the
Three diene stills and the 4th diene still, and carbon five reaction being newly added, then it is isolated to methyl tetrahydro phthalic anhydride product.Can be real
Making full use of of existing carbon five resource, reduces the formation of oligomer in building-up process, and operating process auto-control degree is high,
Reacting balance, can improve properties of product, reduces production cost, improves production efficiency.
Accompanying drawing explanation
Fig. 1 is the first structure principle chart of the device of continuous prodution methyl tetrahydro phthalic anhydride；
Fig. 2 is the second structure principle chart of the device of continuous prodution methyl tetrahydro phthalic anhydride.
Detailed description of the invention
As it is shown in figure 1, the device of this continuous prodution methyl tetrahydro phthalic anhydride includes four diene synthesis reactors: first
Diene still the 101, second diene still the 102, the 3rd diene still the 103, the 4th diene still 104, five pipe bundle condensers: the
One pipe bundle condenser the 201, second pipe bundle condenser the 203, the 3rd pipe bundle condenser the 204, the 4th pipe bundle condenser 206,
5th pipe bundle condenser 208, two falling film evaporators: first falling film evaporator the 202, second falling film evaporator 205, one
Individual membrane evaporator 207, five dosing pumps: first dosing pump the 501, second dosing pump the 502, the 3rd dosing pump 503,
4th dosing pump the 504, the 5th dosing pump 505, three material pumps: first material pump the 506, second material pump the 507, the 3rd material pump
508, nine various storage tanks: reclaim carbon five storage tank 303, reclaim carbon five measuring tank 304, by-product carbon five receiving slit 305, in
Between groove 306, dashpot 307, crude product groove 308, methyl tetrahydro phthalic anhydride groove 309, light component groove 310, vacuum buffer
Groove 311.
As it is shown in figure 1, the input port that import is cis-butenedioic anhydride of the second dosing pump 502, the outlet of the second dosing pump 502 and the
First charging aperture of one diene still 101 is connected, and the gaseous phase outlet at the first diene still 101 top and refluxing opening are respectively with first
The inlet and outlet of pipe bundle condenser 201 is connected；The liquid phase overfall of the first diene still 101 passes through the 3rd dosing pump 503
Import with the first falling film evaporator 202 is connected, the liquid-phase outlet of the first falling film evaporator and the import of medial launder 306
Being connected, the gaseous phase outlet of the first falling film evaporator and the import of the second pipe bundle condenser 203 are connected, the second pipe bundle condenser
The outlet of 203 is connected with by-product carbon five receiving slit 305.The outlet of medial launder 306 is by the 4th dosing pump 504 and second pair
First charging aperture of alkene still 102 is connected, the liquid phase overfall of the second diene still and the first charging aperture of the 3rd diene still 103
Being connected, the liquid phase overfall of the 3rd diene still and the first charging aperture of the 4th diene still 104 are connected, the liquid of the 4th diene still
Phase overfall is connected with the import of dashpot 307；The input port that import is carbon five of the 5th dosing pump 505, the 5th metering
The outlet of pump 505 respectively with the second charging aperture of the second diene still 102, the second charging aperture of the 3rd diene still 103,
Second charging aperture of four diene stills 104 is connected, the second diene still the 102, the 3rd diene still the 103, the 4th diene still 104 and
The top of dashpot 307 is respectively provided with the import of gas phase pipeline and the 3rd pipe bundle condenser 204 and is connected, and the 3rd tubulation is cold
Liquid-phase outlet and the second diene still 102 of condenser 204 are connected.The liquid-phase outlet of dashpot 307 passes through the first material pump 506
Import with the second falling film evaporator 205 is connected, and the gaseous phase outlet of the second falling film evaporator 205 is condensed by the 4th tubulation
Device 206 is connected with the import reclaiming carbon five measuring tank 304, and the outlet reclaiming carbon five measuring tank 304 is stored up with reclaiming carbon five
The import of groove 303 is connected, and the outlet reclaiming carbon five storage tank 303 is connected with the import of the first dosing pump 501, the first metering
The outlet of pump 501 is connected with the second charging aperture of the first diene still 101.The liquid-phase outlet of the second falling film evaporator 205 with
The import of crude product groove 308 is connected, outlet the entering by the second material pump 507 and membrane evaporator 207 of crude product groove 308
Mouth is connected, and the gaseous phase outlet of membrane evaporator 207 and the import of the 5th pipe bundle condenser 208 are connected, membrane evaporator 207
Liquid-phase outlet be connected with the import of methyl tetrahydro phthalic anhydride groove 309, the liquid-phase outlet of the 5th pipe bundle condenser 208 is with light
The import of component groove 310 is connected, the gaseous phase outlet of the 5th pipe bundle condenser 208 and the import phase of vacuum buffer tank 311
Connect.The import of methyl tetrahydro phthalic anhydride groove 309 outlet at bottom and the 3rd material pump 508 is connected, going out of the 3rd material pump 508
Mouth is the outlet of methyl tetrahydro phthalic anhydride product.
The production process of the device of this continuous prodution methyl tetrahydro phthalic anhydride is as follows:
(1) diene synthesis and by-product carbon five: containing the recovery carbon five of 3-5% active component and the liquid from tank field storage tank
Cis-butenedioic anhydride, polymerization inhibitor etc. are squeezed into the first diene still 101 by first dosing pump the 501, second dosing pump 502 to set flow respectively
Carrying out Diene synthesis, reaction is carried out under temperature 60-80 DEG C, 0.10～0.30Mpa pressure, reaction heat by still chuck or
Inner coil pipe and the first pipe bundle condenser 201 carry out heat exchange, and the mixture diene overflowed from the first diene still top closes
Product (methyl tetrahydro phthalic anhydride, excess cis-butenedioic anhydride, carbon non-activated five etc.) is become to control speed and stream by the 3rd dosing pump 503
Entering the first falling film evaporator 202 after amount and carry out flash distillation, extreme portions carbon five takes entrance the second tubulation out of with the form of gas phase
Condenser 203, enters by-product carbon five receiving slit 305, then sends to tank field storage tank after condensation.New carbon five from tank field storage tank
By the 5th dosing pump 505 be divided into three strands with set flow respectively enter the second diene still 102, the 3rd diene still 103, the
Four diene stills 104, methyl tetrahydro phthalic anhydride, cis-butenedioic anhydride mixture from the first falling film evaporator 202 enter medial launder 306
After, the 5th dosing pump 504 input the second diene still 102, and overflow enters the 3rd diene still the 103, the 4th diene successively
Still 104 reacts, in the 4th diene still 104, excess carbon five and a small amount of unreacted cis-butenedioic anhydride fully react after overflow
Entering dashpot 307, the reaction heat of the second diene still the 102, the 3rd diene still the 103, the 4th diene still 104 passes through top gas
Manage the 3rd connected pipe bundle condenser 204 and reactor inner coil pipe or chuck heat exchange mutually.
(2) carbon five recycles and separates with methyl tetrahydro phthalic anhydride: after Diene synthesis finally terminates, methyl tetrahydro phthalic anhydride and mistake
Amount C5 mixture overflow is squeezed into the second falling film evaporator 205 flash distillation by the first material pump 506 after entering dashpot 307 and is steamed
Carbon five, gas phase enters the 4th pipe bundle condenser 206, is recycled carbon five and enters recovery carbon five measuring tank 304 after condensation, then
Enter and reclaim carbon five storage tank 303, then squeezed into the first diene still 101 by the first dosing pump 501 and carry out Diene synthesis, it is achieved follow
Ring set is used.Second falling film evaporator 205 bottom liquid phases component is that thick methyl tetrahydro phthalic anhydride enters crude product groove 308.
(3) decompression distillation: the thick methyl tetrahydro phthalic anhydride in crude product groove 308, is inputted membrane evaporator by the second material pump 507
207 carry out decompression separation, and gaseous component enters the 5th pipe bundle condenser 208, and condensed fluid is that light component is stored in light component groove
310 as by-product；Bottom membrane evaporator 207, methyl tetrahydro phthalic anhydride out enters methyl tetrahydro phthalic anhydride groove 309,
And it is transported to methyl tetrahydro phthalic anhydride finished product storage tank by the 3rd material pump 508, can be former directly as the hydrogenation of methyl hexahydrophthalic anhydride
Expect or prepare isomerized methyltetrahydro phthalic anhydride.
As in figure 2 it is shown, various automatically controlling can be installed on the pipeline of the device of this continuous prodution methyl tetrahydro phthalic anhydride
Instrument, it is achieved automatically controlling of production process.
The device of this continuous prodution methyl tetrahydro phthalic anhydride compared with prior art, has a following advantage:
(1) by using the completely identical in structure diene synthesis still of 4 series connection to carry out diene synthesis reaction, at first
Diene still ensure the cis-butenedioic anhydride of high concentration and second, third, the 4th diene still has neither part nor lot in excess carbon in the recovery carbon five of reaction
Five active components all participate in reaction, and excess carbon five recycles, synthetical recovery, overcomes conventional single diene synthesis still
For keeping cis-butenedioic anhydride fully to react, carbon five excess 3-5% and the carbon five that causes consumes height, production cost is high, resource utilization is low
Etc. problem；And by introducing new carbon five respectively at second and third, in four diene stills, improve carbon five active component concentration,
Can ensure that cis-butenedioic anhydride fully reacts, therefore, whole system maintains carbon five active component, cis-butenedioic anhydride has reached high conversion ratio,
Conversion ratio is more than 99.5%.
(2) enter second, third by five points three strands of new carbon, in the 4th diene still, shorten the carbon five in reaction system
The time of staying of active component, reducing the concentration of carbon five active component, response speed is controlled, and exothermic heat of reaction is more
Steadily, reduce alkadienes high temperature polymerization probability, it is to avoid the accumulation of oligomer in methyl tetrahydro phthalic anhydride, be conducive to improving
Properties of product.
(3) by continuous feed and Automated condtrol on-line monitoring temperature of reaction system, the pressure trend of carbon five, control
Carbon five amount and response speed, thermal discharge in device are made.
(4) in one-level crude product methyl tetrahydro phthalic anhydride, residual carbon five is removed by falling film evaporator flash distillation, light component passes through thin film
Vaporizer decompression is removed, and continuous feed, disengagement area is big, vapo(u)rizing temperature is low, efficiency is high, it also avoid the poly-of single hydrocarbon alkene
Close.
(5) continuous feeding and discharging, the whole closed-loop operation of pilot process, operating process is steady, overcomes gap operating and frequently puts
Empty, reclaim by-product carbon five and concentrate that distillation unit interval evaporation capacity is big, coolant needs big, exhaust emissions density unevenness weighing apparatus etc. to ask
Topic, greatly reduces waste gas discharge, alleviates vent gas treatment load.
Claims (1)
1. a device for continuous prodution methyl tetrahydro phthalic anhydride, including four diene synthesis reactors, five tubulation condensations
Device, two falling film evaporators, a membrane evaporator, five dosing pumps, three material pumps and nine various storage tanks, it is special
Levy the diene synthesis reactor being described and include the first diene still (101), the second diene still (102), the 3rd diene still (103)
With the 4th diene still (104), the input port that import is cis-butenedioic anhydride of the second dosing pump (502), the second dosing pump (502)
Outlet be connected with the first charging aperture of the first diene still (101), the gaseous phase outlet at the first diene still (101) top and
Refluxing opening inlet and outlet with the first pipe bundle condenser (201) respectively is connected；The liquid phase of the first diene still (101) is overflow
Head piece is connected with the first falling film evaporator (202) by the 3rd dosing pump (503), and the liquid phase of the first falling film evaporator goes out
Mouth is connected with the import of medial launder (306), the gaseous phase outlet of the first falling film evaporator and the second pipe bundle condenser (203)
Import be connected, the outlet of the second pipe bundle condenser (203) is connected with the import of by-product carbon five receiving slit (305)；In
Between the outlet of groove (306) be connected by the first charging aperture of the 4th dosing pump (504) with the second diene still (102),
The liquid phase overfall of two diene stills and the first charging aperture of the 3rd diene still (103) are connected, the liquid phase overflow of the 3rd diene still
Mouth is connected with the first charging aperture of the 4th diene still (104), the liquid phase overfall of the 4th diene still and dashpot (307)
Import be connected；The input port that import is carbon five of the 5th dosing pump (505), the outlet of the 5th dosing pump (505) divides
Not with the second charging aperture of the second diene still (102), the second charging aperture of the 3rd diene still (103), the 4th diene still
(104) the second charging aperture is connected, the second diene still (102), the 3rd diene still (103), the 4th diene still (104)
The import having gas phase pipeline and the 3rd pipe bundle condenser (204) with the top of dashpot (307) respectively is connected, and the 3rd
The liquid-phase outlet of pipe bundle condenser (204) and the second diene still (102) are connected；The liquid-phase outlet of dashpot (307) leads to
Cross the first material pump (506) to be connected with the import of the second falling film evaporator (205), the gas of the second falling film evaporator (205)
Export mutually and be connected with the import reclaiming carbon five measuring tank (304) by the 4th pipe bundle condenser (206), reclaim carbon five
The outlet of measuring tank (304) is connected with the import reclaiming carbon five storage tank (303), reclaims the outlet of carbon five storage tank (303)
Import with the first dosing pump (501) is connected, the of the outlet of the first dosing pump (501) and the first diene still (101)
Two charging apertures are connected；The liquid-phase outlet of the second falling film evaporator (205) is connected, slightly with the import of crude product groove (308)
The outlet of product groove (308) is connected with the import of membrane evaporator (207) by the second material pump (507), membrane evaporator
(207) gaseous phase outlet and the import of the 5th pipe bundle condenser (208) are connected, and the liquid phase of membrane evaporator (207) goes out
Mouth is connected with the import of methyl tetrahydro phthalic anhydride groove (309), the liquid-phase outlet of the 5th pipe bundle condenser (208) and light group
The import of part groove (310) is connected, the gaseous phase outlet of the 5th pipe bundle condenser (208) and vacuum buffer tank (311)
Import is connected；The outlet of methyl tetrahydro phthalic anhydride groove (309) bottom is connected with the import of the 3rd material pump (508), the
The outlet that outlet is methyl tetrahydro phthalic anhydride product of three material pumps (508).
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| Application Number | Priority Date | Filing Date | Title |
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| CN201620469855.3U CN205774230U (en) | 2016-05-20 | 2016-05-20 | The device of continuous prodution methyl tetrahydro phthalic anhydride |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201620469855.3U CN205774230U (en) | 2016-05-20 | 2016-05-20 | The device of continuous prodution methyl tetrahydro phthalic anhydride |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107629024A (en) * | 2017-10-13 | 2018-01-26 | 山东尚舜化工有限公司 | A kind of continuous synthesizer of rubber vulcanization accelerator M and its production technology |
| 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 |
| CN112661735A (en) * | 2021-01-15 | 2021-04-16 | 浙江正大新材料科技股份有限公司 | Continuous production system and method for methyl tetrahydrophthalic anhydride |
| CN112973612A (en) * | 2021-02-10 | 2021-06-18 | 中国科学院过程工程研究所 | System device and method for continuously synthesizing methyl tetrahydrophthalic anhydride |
-
2016
- 2016-05-20 CN CN201620469855.3U patent/CN205774230U/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107629024A (en) * | 2017-10-13 | 2018-01-26 | 山东尚舜化工有限公司 | A kind of continuous synthesizer of rubber vulcanization accelerator M and its production technology |
| 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 |
| CN111732564B (en) * | 2020-06-13 | 2023-06-02 | 嘉兴南洋万事兴化工有限公司 | Method for preparing methyltetrahydrophthalic anhydride and synthesis system |
| CN112661735A (en) * | 2021-01-15 | 2021-04-16 | 浙江正大新材料科技股份有限公司 | Continuous production system and method for methyl tetrahydrophthalic anhydride |
| CN112661735B (en) * | 2021-01-15 | 2023-12-22 | 浙江正大新材料科技股份有限公司 | Continuous production system and method for methyltetrahydrophthalic anhydride |
| CN112973612A (en) * | 2021-02-10 | 2021-06-18 | 中国科学院过程工程研究所 | System device and method for continuously synthesizing methyl tetrahydrophthalic anhydride |
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