CN109293611A - A kind of continuous synthesis device and its synthetic method of hexahydrophthalic anhydride - Google Patents
A kind of continuous synthesis device and its synthetic method of hexahydrophthalic anhydride Download PDFInfo
- Publication number
- CN109293611A CN109293611A CN201811158189.1A CN201811158189A CN109293611A CN 109293611 A CN109293611 A CN 109293611A CN 201811158189 A CN201811158189 A CN 201811158189A CN 109293611 A CN109293611 A CN 109293611A
- Authority
- CN
- China
- Prior art keywords
- tank
- liquid
- fixed bed
- gas
- mouth
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The present invention provides the continuous synthesis devices and its synthetic method of a kind of hexahydrophthalic anhydride, including catalysis reaction mechanism, gas-liquid separation mechanism, product concentration mechanism and solvent recovery mechanism, catalysis reaction mechanism includes material-compound tank, first circulation pump, fixed bed reactors and air accumulator, catalyst is filled in fixed bed reactors, air accumulator is connected to fixed bed reactors by compressor, and the discharge gate of fixed bed reactors is also connected with gas-liquid separation mechanism;Gas-liquid separation mechanism includes check valve, sustained release tank, knockout drum and liquid trap, check valve is set at the discharge gate of fixed bed reactors, also pass through check valve into tank mouth and is connected to fixed bed reactors, the first of sustained release tank goes out the feed inlet that tank mouth is connected to knockout drum by pipeline, and second, which goes out tank mouth, is also attached to liquid trap.The setting of mechanism and solvent recovery mechanism is concentrated by catalysis reaction mechanism, gas-liquid separation mechanism, product by the present invention, realizes the recycling and reusing to reaction raw materials.
Description
Technical field
The invention belongs to organic synthesis fields, and in particular to a kind of continuous synthesis device of hexahydrophthalic anhydride and its synthesis side
Method.
Background technique
Hexahydrophthalic anhydride full name hexahydrophthalic anhydride, white to off-white color crystallize, and low melting point solid can be dissolved in tetrahydro
Furans, benzene, in acetone equal solvent.Hexahydrophthalic anhydride is the production indispensable raw material of polyesters coating, is replaced with hexahydrophthalic anhydride
Alkyd amino, polyurethane paint, the powdery paints etc. of aromatic polyvalent acid production, can significantly improve fresh degree of reflecting, the gloss of coating,
Hexahydrophthalic anhydride is alternatively arranged as curing agent, adhesive, plasticizer of epoxy resin etc. simultaneously.
Tetrahydrophthalic anhydride catalytic hydrogenation prepares hexahydrophthalic anhydride, is industrial common process route, there is melting batch process production
Technique and solvent continuity method production technology, batch process auto-processes degree is low, and product quality fluctuation is big, complicated for operation,
Yield is relatively small.Continuity method production technology is mainly reflected in that plant automation degree is high, and production capacity is big, stable product quality, behaviour
Make it is easy, while can also a variety of plasticizer products similar in raw materials for production property.The patent of domestic report is mostly to use at present
It melts batch process and prepares hexahydrophthalic anhydride, production efficiency is lower, and domestic hexahydrophthalic anhydride continuous process is using single molten
Agent, solvent is not easy to remove, while impurity content is higher.
Summary of the invention
To solve the above problems, the present invention provides the continuous synthesis device and its synthetic method of a kind of hexahydrophthalic anhydride, pass through
It is catalyzed the setting of reaction mechanism, gas-liquid separation mechanism, product concentration mechanism and solvent recovery mechanism, reaction raw materials are returned in realization
It receives and recycles.
To achieve the goals above, the technical solution adopted by the present invention are as follows:
A kind of continuous synthesis device of hexahydrophthalic anhydride, including catalysis reaction mechanism, gas-liquid separation mechanism, product concentration mechanism and molten
Agent recovering mechanism, it is characterised in that: the catalysis reaction mechanism includes material-compound tank, first circulation pump, fixed bed reactors and storage
Gas tank, the feed inlet of the discharge port connection first circulation pump of material-compound tank, the discharge port of first circulation pump are also connected with fixed bed reaction
The feed inlet of device is filled with catalyst in the fixed bed reactors, and the air accumulator is connected to the fixation by compressor
Bed reactor, the discharge gate of the fixed bed reactors are also connected with the gas-liquid separation mechanism;The gas-liquid separation mechanism includes
Check valve, sustained release tank, knockout drum and liquid trap, the check valve is set at the discharge gate of fixed bed reactors, described
Sustained release tank include tank body and be set on tank body into tank mouth, first go out tank mouth, second go out tank mouth, the tank body be closed shell
Body, the bottom of tank body are cambered surface towards the hemispherical outside tank body, and the inside of tank body is additionally provided with liquid collecting net, described to be arranged into tank mouth
In the side wall of tank body, described also to pass through the check valve into tank mouth and be connected to the fixed bed reactors, described first goes out tank mouth
Go out tank mouth with described second and be also respectively arranged at the top of tank body and the bottom of tank body, described first goes out tank mouth is connected by pipeline
In the feed inlet of knockout drum, the liquid outlet of knockout drum is connected to the solvent recovery mechanism, and knockout drum goes out
Port is also attached to the air accumulator, and the gas in air accumulator passes through compressor again and is delivered to fixed bed reactors;Described second
Tank mouth is also attached to the liquid trap out;The liquid trap is column type shell, and the bottom of liquid trap is equipped with liquid collection opening, the liquid collecting
Mouth is connected to described second by U-shaped pipe and goes out tank mouth, and the top of liquid trap is equipped with overflow port, and the overflow port is defeated by pipeline
It send to solvent recovery mechanism, the hexahydrophthalic anhydride after solvent recovery mechanism, the concentration of product concentration mechanism is also delivered to product storage
It is stored in tank.
Further, the two material-compound tanks charging for adding tetrahydrophthalic anhydride and mixed solvent respectively is additionally provided on the material-compound tank
Mouthful.
Further, the fixed bed reactors are equipped with inlet, air inlet and discharge gate, and the inlet connects institute
First circulation pump is stated, the air inlet is connected with the air accumulator.
Further, the check valve is lift check valve.
Further, the liquid collecting net be set to it is described go out between tank mouth into tank mouth and described first, liquid collecting net edge
It is horizontally arranged.
Further, the liquid collecting net is stainless steel cloth, and the tank body with sustained release tank is also respectively welded in the periphery of liquid collecting net
It is internal.
Further, the solvent recovery mechanism includes that vacuum flasher, second circulation pump, the first condenser and mixing are molten
Agent tank, the vacuum flasher pump the liquid outlet of connection knockout drum and the overflow port of liquid trap, decompression by second circulation
Flash column is connected to the first condenser by top discharge mouth, and condensed solvent is also delivered to mixed solvent tank, mixed solvent tank
In solvent also pass through pipeline into material-compound tank.
Further, product concentration mechanism includes third circulating pump, thin film evaporator and the second condenser, described thin
Film evaporator is connected to the lower discharge port of vacuum flasher, thin film evaporator top discharge mouth evaporated by second condenser
Solvent also pass through the second condenser condensation after be delivered to mixed solvent tank, the product that thin film evaporator lower discharge port obtains is also defeated
It send to product storage tank.
The present invention also provides a kind of synthetic methods of the continuous synthesis device of hexahydrophthalic anhydride, it is characterised in that: by tetrahydro benzene
Acid anhydride and mixed solvent 1:4 in mass ratio put into material-compound tank, are pumped into the fixed bed reactors equipped with catalyst by first circulation
Interior, the mixed solvent is obtains after tetrahydrofuran and hexamethylene mixing, hydrogen is pressed into fixed bed by compressor in air accumulator
In reactor, charging hydrogen-oil ratio is 1000:1 ~ 5000:1, and controlling temperature in the fixed bed reactors is 40 ~ 60 DEG C, reaction pressure
It is maintained within the scope of 2 ~ 4.0Mpa.The product that tower bottom comes out is sent into sustained release tank continuously across check valve, is sustained pot bottom second
It is sent into vacuum flasher after the collecting action that the liquid that tank mouth is collected out passes sequentially through liquid trap and second circulation pumps, is sustained tank
Top first goes out in the gas feeding knockout drum that tank mouth is collected to be separated again;The hydrogen that knockout drum top row goes out introduces gas storage
Tank is recycled, and the liquid phase of gas-liquid separation tank bottom discharge is pumped into vacuum flasher by second circulation, controls vacuum flashing
Temperature is 80 ~ 110 DEG C in tower, and vacuum pressure is -0.06 ~ 0.095Mpa, the gas phase that vacuum flasher top row goes out, i.e. sudden strain of a muscle top gas warp
First condenser, which is condensed into after liquid, is sent into mixed solvent tank, recycles mixed solvent, the liquid phase of vacuum flashing tower bottom discharge,
I.e. sudden strain of a muscle bottom liquid is pumped into thin film evaporator by third circulation and is evaporated in vacuo, and control thin film evaporator temperature is 80 ~ 110
DEG C, vacuum pressure is -0.08 ~ 0.095Mpa, obtains hexahydrophthalic anhydride product and is sent into product storage tank, the gas being evaporated is through second
Feeding mixed solvent tank recycles after condenser is condensed into liquid.
Further, the volume ratio of the in the mixed solvent tetrahydrofuran and hexamethylene is 3:1 ~ 10:1.
The invention has the benefit that continuous synthesis device of the invention and its synthetic method use continuous feed, discharging,
The residence time is very short in the reactor for tetrahydrophthalic anhydride and mixed solvent, and product stability is high, and production efficiency improves;It is mixed after synthesis
Object is passed through in gas-liquid separation mechanism via check valve, and check valve guarantees the reaction pressure in fixed bed reactors, gas-liquid segregating unit
It is separated at the beginning of the sustained release tank of structure also passes through decompression and liquid collecting net depressurizes the mixture in fixed bed reactors, the gas after separation
It mutually continues on to knockout drum to be separated again, the liquid phase after separation is delivered to solvent recovery mechanism by liquid trap and carries out
Solvent recovery process, is sustained tank and liquid trap realizes that gas-liquid just separates, and improves the efficiency of gas-liquid separation, hydrogen and mixed solvent exist
The amount of consumption need to be only supplemented in system, most of Ke Xunhuanliyong, synthetical recovery reduces the generation of the three wastes.
Detailed description of the invention
Fig. 1 is the flow diagram of invention;
Fig. 2 is the cooperation figure for being sustained tank and liquid trap.
Wherein, each label in figure are as follows: 1, material-compound tank, 2, first circulation pump, 3, air accumulator, 4, compressor, 5, fixed bed it is anti-
Answer device, 6, knockout drum, 7, second circulation pump, 8, vacuum flasher, the 9, first condenser, 10, mixed solvent tank, 11, the
Three circulating pumps, 12, thin film evaporator, the 13, second condenser, 14, product storage tank, 15, check valve, 16, sustained release tank, 17, tank body,
18, liquid trap, 19, liquid collecting net, 20, into tank mouth, 21, first goes out tank mouth, and 22, second goes out tank mouth, 23, liquid collection opening, 24, U-tube
Road, 25, overflow port.
Specific embodiment
In order to which those skilled in the art better understood when technical solution provided by the present invention, below with reference to specific
Embodiment income illustrates.
Fig. 1 be flow diagram of the invention, a kind of continuous synthesis device of hexahydrophthalic anhydride, including catalysis reaction mechanism,
Gas-liquid separation mechanism, product concentration mechanism and solvent recovery mechanism, continuous synthesis device of the invention and its synthetic method use
The residence time is very short in the reactor for continuous feed, discharging, tetrahydrophthalic anhydride and mixed solvent, and product stability is high, production efficiency
It improves.Catalysis reaction mechanism includes material-compound tank 1, first circulation pump 2, fixed bed reactors 5 and air accumulator 3, the discharging of material-compound tank 1
Mouth connection first circulation pumps 2 feed inlet, is additionally provided with two ingredients for adding tetrahydrophthalic anhydride and mixed solvent respectively on material-compound tank 1
Tank feed inlet, fixed bed reactors 5 are equipped with inlet, air inlet and discharge gate, and inlet connects first circulation pump 2, air inlet
Mouth is connected with air accumulator 3, and the discharge port of first circulation pump 2 is also connected with the feed inlet of fixed bed reactors 5, fixed bed reactors
Catalyst is filled in 5, air accumulator 3 is connected to fixed bed reactors 5 by compressor 4, and the discharge gate of fixed bed reactors 5 is also
Connect gas-liquid separation mechanism.
Gas-liquid separation mechanism includes check valve 15, sustained release tank 16, knockout drum 6 and liquid trap 18, and check valve 15 is energy
The lift check valve of enough pressure maintainings, check valve 15 are set at the discharge gate of fixed bed reactors 5, and sustained release tank 16 includes tank body 17
Go out the tank mouth 22 out of tank mouth 21, second into tank mouth 20, first with being set on tank body 17, tank body 17 is closed shell, tank body
17 bottom is cambered surface towards the hemispherical outside tank body 17, and the inside of tank body 17 is additionally provided with liquid collecting net 19, and liquid collecting net 19 is arranged
Go out between tank mouth 21 in into tank mouth 20 and first, liquid collecting net 19 is horizontally disposed, and liquid collecting net 19 is stainless steel cloth, liquid collecting
The periphery of net 19 is also respectively welded with inside the tank body 17 of sustained release tank 16, the side wall of tank body 17 is set into tank mouth 20, into tank mouth
20 are also connected to fixed bed reactors 5 by check valve 15, and first, which goes out tank mouth 21 and second, goes out tank mouth 22 and be also respectively arranged at tank
The top of body 17 and the bottom of tank body 17, first goes out the feed inlet that tank mouth 21 is connected to knockout drum 6 by pipeline, gas-liquid point
Liquid outlet from tank 6 is connected to solvent recovery mechanism, and the gas outlet of knockout drum 6 is also attached to air accumulator 3, in air accumulator 3
Gas pass through compressor 4 again and be delivered to fixed bed reactors 5.
Second, which goes out tank mouth 22, is also attached to liquid trap 18;Liquid trap 18 is column type shell, and the bottom of liquid trap 18 is equipped with collection
Liquid mouth 23, liquid collection opening 23 are connected to second by U-shaped pipe 24 and go out tank mouth 22, and the top of liquid trap 18 is equipped with overflow port 25, overflows
Hexahydrobenzene of the head piece 25 by pipeline to solvent recovery mechanism, after solvent recovery mechanism, the concentration of product concentration mechanism
Acid anhydride is also delivered in product storage tank 14 and stores.
Solvent recovery mechanism includes vacuum flasher 8, second circulation the 7, first condenser 9 of pump and mixed solvent tank 10, is subtracted
Flash column 8 is pressed to pass through the liquid outlet of 7 connection knockout drum 6 of second circulation pump and the overflow port 25 of liquid trap 18, vacuum flashing
Tower 8 is connected to the first condenser 9 by top discharge mouth, and condensed solvent is also delivered to mixed solvent tank 10, mixed solvent tank
Solvent in 10 also passes through pipeline into material-compound tank 1.
It includes third circulating pump 11, thin film evaporator 12 and the second condenser 13, thin film evaporator 12 that mechanism, which is concentrated, in product
The lower discharge port of vacuum flasher 8, the solvent of 12 top discharge mouth evaporated of thin film evaporator are connected to by the second condenser 13
It is delivered to mixed solvent tank 10 after also condensing by the second condenser 13, the product that 12 lower discharge port of thin film evaporator obtains is also defeated
It send to product storage tank 14.
A kind of synthetic method of the continuous synthesis device of hexahydrophthalic anhydride, specifically fixation is urged first on fixed bed reactors
Agent, will be on NiO/SiO2 Catalyst packing to fixed bed reactors 5.First with nitrogen displacement reaction system, keep its oxygen content low
In 0.2%(volume), then switch hydrogen and carries out catalyst reduction, the volume space velocity 2000h-1 of control hydrogen charging, reactor
130 DEG C of temperature, pressure 3.0Mpa, reductase 12 4h.
Then hydrogenation reaction is carried out, it is molten that tetrahydrofuran and hexamethylene are that 5:1 is configured to mix in solvent tank by volume
Tetrahydrophthalic anhydride and mixed solvent 1:4 in mass ratio are put into material-compound tank 1 by agent, are sent by first circulation pump 2 equipped with catalyst
In fixed bed reactors 5, hydrogen is sent into fixed bed reactors 5 by compressor 4 in hydrogen gas tank 3, and charging hydrogen-oil ratio is 3000:
1, controlling temperature in the fixed bed reactors is 50 DEG C, and reaction pressure is maintained at 3.0Mpa.Tower bottom come out product continuously across
Check valve 15 is sent into sustained release tank 16, and sustained release 16 bottom second of tank goes out the liquid that tank mouth 22 is collected and passes sequentially through liquid trap 18 and the
It is sent into vacuum flasher 8 after the collecting action of two circulating pumps 7,16 top first of sustained release tank goes out the gas that tank mouth 21 is collected and is sent into
It is separated again in knockout drum 6;In knockout drum 6, the hydrogen that knockout drum top row goes out introduces hydrogen gas tank 3 and is recycled,
The liquid phase of gas-liquid separation tank bottom discharge is sent into vacuum flasher 8 by second circulation pump 7, is controlled temperature in vacuum flasher and is
100 DEG C, vacuum pressure is -0.080Mpa, the gas phase that vacuum flasher top row goes out is dodged top gas and is condensed into through the first condenser 9
It is sent to mixed solvent tank 10 after liquid, recycles mixed solvent, the liquid phase of vacuum flashing tower bottom discharge, i.e. sudden strain of a muscle bottom liquid pass through the
Three circulating pumps 11 are sent into scraper film evaporator 12 and are evaporated in vacuo, and control thin film evaporator temperature is 100 DEG C, vacuum pressure
Power is -0.080Mpa, obtains hexahydrophthalic anhydride product and is sent into product storage tank 14, product purity reaches 99.3%.The gas being evaporated
Mixed solvent tank 10 is sent to after the second condenser 13 is condensed into liquid to recycle.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
The present invention will not be limited to the embodiments shown herein, and is to fit to special with principles disclosed herein and novelty
The consistent widest scope of point.
Claims (10)
1. a kind of continuous synthesis device of hexahydrophthalic anhydride, including catalysis reaction mechanism, gas-liquid separation mechanism, product concentration mechanism and
Solvent recovery mechanism, it is characterised in that: the catalysis reaction mechanism include material-compound tank, first circulation pump, fixed bed reactors and
Air accumulator, the feed inlet of the discharge port connection first circulation pump of material-compound tank, it is anti-that the discharge port of first circulation pump is also connected with fixed bed
The feed inlet of device is answered, catalyst is filled in the fixed bed reactors, the air accumulator is connected to described solid by compressor
Fixed bed reactor, the discharge gate of the fixed bed reactors are also connected with the gas-liquid separation mechanism;
The gas-liquid separation mechanism includes that check valve, sustained release tank, knockout drum and liquid trap, the check valve are set to fixation
At the discharge gate of bed reactor, the sustained release tank includes tank body and is set to going out tank mouth into tank mouth, first, second going out on tank body
Tank mouth, the tank body are closed shell, and the bottom of tank body is cambered surface towards the hemispherical outside tank body, and the inside of tank body is also set
There is liquid collecting net, the side wall that tank body is set into tank mouth is described to be also connected to the fixation by the check valve into tank mouth
Bed reactor, described first go out tank mouth and described second go out tank mouth be also respectively arranged at the top of tank body and the bottom of tank body, institute
It states first and goes out the feed inlet that tank mouth is connected to knockout drum by pipeline, the liquid outlet of knockout drum is connected to the solvent
Recovering mechanism, the gas outlet of knockout drum are also attached to the air accumulator, and the gas in air accumulator is conveyed by compressor again
To fixed bed reactors;Described second, which goes out tank mouth, is also attached to the liquid trap;The liquid trap is column type shell, liquid trap
Bottom is equipped with liquid collection opening, and the liquid collection opening is connected to described second by U-shaped pipe and goes out tank mouth, and the top of liquid trap is equipped with overflow
Mouthful, the overflow port is by pipeline to solvent recovery mechanism, after solvent recovery mechanism, the concentration of product concentration mechanism
Hexahydrophthalic anhydride is also delivered in product storage tank and stores.
2. a kind of continuous synthesis device of hexahydrophthalic anhydride according to claim 1, it is characterised in that: on the material-compound tank also
Equipped with two material-compound tank feed inlets for adding tetrahydrophthalic anhydride and mixed solvent respectively.
3. a kind of continuous synthesis device of hexahydrophthalic anhydride according to claim 1, it is characterised in that: the fixed bed reaction
Device is equipped with inlet, air inlet and discharge gate, and the inlet connects the first circulation pump, the air inlet and the storage
Gas tank is connected.
4. a kind of continuous synthesis device of hexahydrophthalic anhydride according to claim 1, it is characterised in that: the check valve is to rise
Drop formula check valve.
5. a kind of continuous synthesis device of hexahydrophthalic anhydride according to claim 1, it is characterised in that: the liquid collecting net setting
Go out between tank mouth into tank mouth with described first in described, the liquid collecting net is horizontally disposed.
6. a kind of continuous synthesis device of hexahydrophthalic anhydride according to claim 1, it is characterised in that: the liquid collecting net is not
Become rusty steel wire, and the tank interior with sustained release tank is also respectively welded in the periphery of liquid collecting net.
7. a kind of continuous synthesis device of hexahydrophthalic anhydride according to claim 1, it is characterised in that: the solvent recovery machine
Structure includes that vacuum flasher, second circulation pump, the first condenser and mixed solvent tank, the vacuum flasher pass through second circulation
The liquid outlet of pump connection knockout drum and the overflow port of liquid trap, vacuum flasher are connected to the first condensation by top discharge mouth
Device, condensed solvent are also delivered to mixed solvent tank, and the solvent in mixed solvent tank also passes through pipeline into material-compound tank.
8. a kind of continuous synthesis device of hexahydrophthalic anhydride according to claim 7, it is characterised in that: the product thickener
Structure includes third circulating pump, thin film evaporator and the second condenser, and the thin film evaporator is connected by second condenser
In the lower discharge port of vacuum flasher, the solvent of thin film evaporator top discharge mouth evaporated also passes through defeated after the second condenser condenses
It send to mixed solvent tank, the product that thin film evaporator lower discharge port obtains also is delivered to product storage tank.
9. a kind of synthetic method of the continuous synthesis device of hexahydrophthalic anhydride according to claim 1, it is characterised in that: by four
Hydrogen phthalic anhydride and mixed solvent 1:4 in mass ratio put into material-compound tank, and it is anti-to be pumped into the fixed bed equipped with catalyst by first circulation
It answers in device, the mixed solvent is obtains after tetrahydrofuran and hexamethylene mixing, hydrogen is solid by compressor indentation in air accumulator
In fixed bed reactor, charging hydrogen-oil ratio is 1000:1 ~ 5000:1, and controlling temperature in the fixed bed reactors is 40 ~ 60 DEG C, reaction
Pressure is maintained within the scope of 2 ~ 4.0Mpa, and the product that tower bottom comes out is sent into sustained release tank continuously across check valve, is sustained pot bottom
It is sent into vacuum flasher, delays after second collecting action that the liquid for going out tank mouth collection passes sequentially through liquid trap and second circulation pumps
It releases and is separated again in the gas feeding knockout drum that tank mouth is collected out of tank top first;The hydrogen that knockout drum top row goes out introduces
Air accumulator is recycled, and the liquid phase of gas-liquid separation tank bottom discharge is pumped into vacuum flasher by second circulation, control decompression
Temperature is 80 ~ 110 DEG C in flash column, and vacuum pressure is -0.06 ~ 0.095Mpa, the gas phase that vacuum flasher top row goes out dodges top
Gas is sent into mixed solvent tank after the first condenser is condensed into liquid, recycles mixed solvent, the discharge of vacuum flashing tower bottom
Liquid phase, i.e. sudden strain of a muscle bottom liquid are pumped into thin film evaporator and are evaporated in vacuo by third circulation, control thin film evaporator temperature for 80 ~
110 DEG C, vacuum pressure is -0.08 ~ 0.095Mpa, obtains hexahydrophthalic anhydride product and is sent into product storage tank, the gas warp being evaporated
Feeding mixed solvent tank recycles after second condenser is condensed into liquid.
10. a kind of synthetic method of the continuous synthesis device of hexahydrophthalic anhydride according to claim 9, it is characterised in that: institute
The volume ratio for stating in the mixed solvent tetrahydrofuran and hexamethylene is 3:1 ~ 10:1.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201811158189.1A CN109293611A (en) | 2018-09-30 | 2018-09-30 | A kind of continuous synthesis device and its synthetic method of hexahydrophthalic anhydride |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201811158189.1A CN109293611A (en) | 2018-09-30 | 2018-09-30 | A kind of continuous synthesis device and its synthetic method of hexahydrophthalic anhydride |
Publications (1)
Publication Number | Publication Date |
---|---|
CN109293611A true CN109293611A (en) | 2019-02-01 |
Family
ID=65161501
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201811158189.1A Pending CN109293611A (en) | 2018-09-30 | 2018-09-30 | A kind of continuous synthesis device and its synthetic method of hexahydrophthalic anhydride |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN109293611A (en) |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4244877A (en) * | 1979-05-23 | 1981-01-13 | Bayer Aktiengesellschaft | Process for the preparation of hexahydrophthalic acid anhydride |
CN204485332U (en) * | 2015-02-11 | 2015-07-22 | 张诗山 | A kind of novel evacuated decompression concentrator |
CN104785250A (en) * | 2015-03-13 | 2015-07-22 | 上虞盛晖化工股份有限公司 | Hydrogenation catalyst, its preparation method and its application in preparation of hexahydrophthalic anhydride |
CN205013247U (en) * | 2015-09-25 | 2016-02-03 | 成龙建设集团有限公司 | Tunnel groundwater processing row of leading portable air compressor for construction |
CN106866365A (en) * | 2017-03-30 | 2017-06-20 | 荣成市科盛化工有限公司 | A kind of continuous preparation method of hydrogenated bisphenol A |
CN107011304A (en) * | 2017-05-05 | 2017-08-04 | 安阳工学院 | A kind of catalytic hydrogenation prepares HHPA (HHPA) technique |
-
2018
- 2018-09-30 CN CN201811158189.1A patent/CN109293611A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4244877A (en) * | 1979-05-23 | 1981-01-13 | Bayer Aktiengesellschaft | Process for the preparation of hexahydrophthalic acid anhydride |
CN204485332U (en) * | 2015-02-11 | 2015-07-22 | 张诗山 | A kind of novel evacuated decompression concentrator |
CN104785250A (en) * | 2015-03-13 | 2015-07-22 | 上虞盛晖化工股份有限公司 | Hydrogenation catalyst, its preparation method and its application in preparation of hexahydrophthalic anhydride |
CN205013247U (en) * | 2015-09-25 | 2016-02-03 | 成龙建设集团有限公司 | Tunnel groundwater processing row of leading portable air compressor for construction |
CN106866365A (en) * | 2017-03-30 | 2017-06-20 | 荣成市科盛化工有限公司 | A kind of continuous preparation method of hydrogenated bisphenol A |
CN107011304A (en) * | 2017-05-05 | 2017-08-04 | 安阳工学院 | A kind of catalytic hydrogenation prepares HHPA (HHPA) technique |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN102755759B (en) | Continuous reaction rectification process and rectification equipment for synthesizing isopropyl alcohol | |
CN101531588B (en) | The manufacture method of a kind of new pure terephthalic acid | |
CN101913994B (en) | Method for producing nonyl phenol | |
CN109534999B (en) | Synthesis process and device of dimethyl carbonate | |
CN109369396A (en) | A kind of method that direct esterification prepares high-purity ethylene acetate | |
CN102958870B (en) | Process for the preparation of phenol from cumene | |
CN104130138B (en) | The continuous ammonification production technique of a kind of 2,4-dinitraniline | |
CN104059047B (en) | Urea synthesizing cyclic carbonate continuous reaction process | |
CN108383726A (en) | A kind of continuous producing method of hydroxyethyl methacrylate | |
CN114917848A (en) | Device and method for synthesizing vinyl sulfate | |
CN109293611A (en) | A kind of continuous synthesis device and its synthetic method of hexahydrophthalic anhydride | |
CN109748791B (en) | Energy-saving method for producing dimethyl adipate | |
CN1951900A (en) | Low-energy consumption preparation method of terephthalic acid | |
CN107778131B (en) | Method for preparing cyclohexanol and cyclohexanone based on multilayer double-loop flow guide cylinder bubble reactor | |
CN106914030A (en) | A kind of multi-stage circulating formula mechanical stirs ammonium sulphate crystallizer and carrying and operating method | |
CN114984866B (en) | System and method for preparing dimethyl maleate | |
CN108484565B (en) | System for producing carbonic ester and method for producing carbonic ester by using system | |
CN115554955A (en) | Device and process for continuously producing N, N-dimethylethylenediamine | |
CN112409199B (en) | Continuous production process and device for amino acid methyl ester | |
CN210765084U (en) | Heterogeneous continuous acidolysis device for glyphosate | |
CN105601520A (en) | Device for synthesizing nitromethane and separating products | |
CN109280040A (en) | A kind of continuous production processes of in the mixed solvent synthesis hexahydrophthalic anhydride | |
CN208182893U (en) | A kind of system for continuous esterification production ethyl cyanoacetate | |
CN100447124C (en) | Method for producing meta benzene tricarbonic acid through sequential oxidation by using intermittent multiple cascaded Bubbling oxidation towers | |
CN205420234U (en) | Synthetic and result separator of nitromethane |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190201 |
|
RJ01 | Rejection of invention patent application after publication |