CN206767974U - A kind of continuous hydrogenation produces the device of methylhexahydrophthalic anhydride - Google Patents
A kind of continuous hydrogenation produces the device of methylhexahydrophthalic anhydride Download PDFInfo
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Abstract
The utility model discloses the device that a kind of continuous hydrogenation produces methylhexahydrophthalic anhydride, belong to field of chemical equipment.The device splits tubular fixed-bed reactor using three-level, respectively splits and is connected by feedstock circulation series connection of pumps between tubular fixed-bed reactor；Described is split inside tubular fixed-bed reactor using tubular structure is split, and solid catalyst is filled between tube side, is hot coal Jie's passage in shell side；Every grade splits tubular fixed-bed reactor bottom air inlet and connects Hydrogen Line by valve in parallel respectively, and every grade splits gas outlet at the top of tubular fixed-bed reactor and connects hydrogen gas compressor by pipeline；Every grade splits tubular fixed-bed reactor its top feed mouth connection feedstock circulation pump；Every grade splits tubular fixed-bed reactor inner top and is respectively fixed with distributing device.The device can realize that the continuous hydrogenation of methyl tetrahydrophthalic anhydride prepares methylhexahydrophthalic anhydride, and hydrogenation conversion is close to 100%.Continuous hydrogenation process generates without waste gas and other accessory substances, realizes clean manufacturing.
Description
Technical field
The utility model belongs to field of chemical equipment, is related to a kind of anhydride product continuous hydrogenation process units, especially relates to
And a kind of methyl tetrahydrophthalic anhydride continuous hydrogenation prepares the device of methylhexahydrophthalic anhydride.
Background technology
Methylhexahydrophthalic anhydride (Methylhexahydrophthalic anhydride, abbreviation MeHHPA,
CAS25550-51-0 it is) that one kind contains alicyclic acid anhydrides, is widely used because of its excellent Wuli-Shili-Renli system approach.As one
The non-toxic epoxy curing agent of kind excellent performance, it is with that can form tridimensional network after epoxy resin cure, through high temperature
After solidification, weatherability, heat resistance, water resistance, corrosion resistance and dielectric properties are excellent；It is applied to dipping large-scale component, also fits
For pouring into a mould, binding, the technique such as being laminated.It is widely used in electrical and electronic component, electrically conductive ink, automobile case coating, wood preservation
Deng.
In existing industrialized production, methylhexahydrophthalic anhydride generally use methyl tetrahydrophthalic anhydride is prepared
For raw material, device therefor is stirring-type reaction kettle, and production method is batch production.The method produces methyl hexahydro O-phthalic
Acid anhydrides, occupation area of equipment is big, and installation cost is high, and product quality stability is poor, and at 100~140 DEG C, pressure needs hydrogenation temperature
Reach more than 8MPa, hydrogenation time needs 15~20h, and hydrogenation finishes, and directly carries out distillation procedure, catalyst with largely after evaporate
Divide and mix, turn into waste residue, can not recycle, cause environmental pollution.Therefore, research and development hydrogenation conversion is high, energy consumption is low,
Green, steady quality, continuous hydrogenation prepares the device of methylhexahydrophthalic anhydride as the urgent of existing market
Demand.
The content of the invention
In view of the shortcomings of the prior art, the purpose of this utility model is to provide, a kind of hydrogenation efficiency is high, power consumption is low, quality is steady
What fixed, catalyst regeneration cycle used prepares methylhexahydrophthalic anhydride by methyl tetrahydrophthalic anhydride continuous hydrogenation
Device.
The purpose of this utility model is achieved through the following technical solutions：
The continuous hydrogenation prepares the device of methylhexahydrophthalic anhydride, including splits tubular fixed-bed reactor, former
Expect circulating pump, it is characterised in that tubular fixed-bed reactor is split using three-level, respectively splits and passes through original between tubular fixed-bed reactor
Material circulating pump is connected in series；Described is split inside tubular fixed-bed reactor using tubular structure is split, and solid is filled between tube side
Catalyst, it is hot coal Jie's passage that shell side is interior；Every grade splits tubular fixed-bed reactor bottom air inlet and is connected respectively by valve in parallel
Hydrogen Line is connect, every grade splits gas outlet at the top of tubular fixed-bed reactor and connects hydrogen gas compressor by pipeline；Every grade splits tubular type
Fixed bed reactors its top feed mouth connects feedstock circulation pump；Every grade splits tubular fixed-bed reactor inner top and is respectively fixed with cloth
Glassware；Every grade splits tubular fixed-bed reactor bottom discharge mouth and is provided with on-line sampler, and hydrogenation conversion is examined online
Survey.
Hot coal in shell side, which is situated between, selects hot water or deep fat, circulates.
It is described to split tubular fixed-bed reactor, it is made up of upper low head and kettle, makes respectively between upper low head and kettle
It is attached with high-strength bolt.Upper low head is mounted on man-hole opening, mirror mouth.Distributing device is installed at the top of upper cover.
Tubulation is vertically arranged in parallel inside kettle, isometric with kettle, the upper orifice of every tubulation and the circular hole being distributed on upper cover bottom plate
Corresponding connection, lower nozzle connection corresponding with the circular hole on low head bottom plate, tubulation are additionally arranged at the bottom screen pack.Install additional and protect outside kettle
Warm layer, thermo detector are located at kettle side, and thermo detector one end and tubulation wall contacts.
The device innovative point that continuous hydrogenation described in the utility model prepares methylhexahydrophthalic anhydride is：
1st, using multistage continuously hydrogen adding, between each stage reactor the conveying of material conveyed using high pressure pipe pump, liquid phase
It can continuously circulate and reactor top is respectively mounted distributing device, be easy to material and be evenly distributed to reactor to split in pipe, fully contact
Catalyst, be advantageous to improve the conversion ratio of hydrogenation reaction.
2nd, split and hot coal Jie is passed through in tubular fixed-bed reactor shell side, the material in tube side can be interfaced with fully with hot coal
Touch, heat exchange efficiency is high, and heat-energy losses are small, hydrogenation process temperature stabilization, so as to effectively improve hydrogenation conversion.
3rd, high pressure hydrogen enters inside reactor, the process that hydrogen rises in tube side from reactor bottoms at different levels are in parallel
In, fully contacted with liquid phase in solid catalyst surface, be advantageous to improve the conversion ratio of hydrogenation reaction, and the hydrogen that unreacted is complete
Hydrogen gas compressor is returned from reactor top, is recycled again by re-compressing.
4th, on-line sampler is mounted in the outlet of every stage reactor, can be in the state of circulation not be stopped, at different levels
Hydrogenation process is monitored in reactor.Until reach required conversion ratio.After three-level splits pipe reactor, obtained production
Product are directly entered next process.
5th, in the technique using methyl tetrahydrophthalic anhydride as raw material continuous hydrogenation methylhexahydrophthalic anhydride,
It is composite catalyst to split the solid catalyst filled in pipe, forms and is：100 parts of Raney's nickel, palladium/aluminum oxide are Raney's nickel weight
Part 0.1~0.4 times, palladium content is 1% in described palladium/aluminum oxide, and Raney's nickel and palladium/aluminum oxide surface structure are a diameter of
0.5~2mm spherical particles.
The beneficial effects of the utility model are：1st, it can realize that the continuous hydrogenation of methyl tetrahydrophthalic anhydride prepares first
Base hexahydrophthalic anhydride, hydrogenation conversion is close to 100%.2nd, methyl tetrahydrophthalic anhydride is at normal temperatures with liquid phase shape
State is present, it is not necessary to adds i.e. recyclable hydrogenation under conditions of any solvent, continuous hydrogenation process is without waste gas and other accessory substances
Generation, can fully achieve clean manufacturing.3rd, raw material methyl tetrahydrophthalic anhydride and hydrogen are splitting tubular fixed-bed reaction
Catalyst surface in device is evenly distributed, and composite catalyst is selectively good and is easily recycled, and the filling of catalyst
It is simple and easy to do with reclaiming.4th, fixed bed reactors floor space is small, is readily disassembled.It is uniform to split pipe heat exchanger heat exchange, reaction temperature
With, stably, greatly shorten hydrogenation time, effectively improve hydrogenation efficiency.This method has good industrial applications prospect.
Brief description of the drawings
Fig. 1 is the utility model structure diagram, 1- material inlets in figure, 2- distributing devices, 3- visors, 4-man-hole opening, 5-
Hydrogen inlet, 6- hydrogen outlets, 7- pressure gauges, 8- solid catalysts, 9- split pipe, 10- heat-insulation layers, 11- thermals source inlet and outlet, 12-
Thermo detector, 13- upper covers, 14- low heads, 15- material outlets, 16- primary cycle pumps, 17- first-stage reactors, 18- two levels are followed
Ring pump, 19- second reactors, 20- three-level circulating pumps, 21- third-stage reactors, 22- on-line samplers, 23- hydrogen gas compressors.
Embodiment
In order to which preferably the utility model is described in detail, give an actual example as follows：
Embodiment 1：
The production that methylhexahydrophthalic anhydride is prepared using methyl tetrahydrophthalic anhydride as raw material continuous hydrogenation fills
Put, including split tubular fixed-bed reactor, feedstock circulation pump.It is characterized in that：Respectively split tubular fixed-bed reactor 17,19,21
Between connected by feedstock circulation series connection of pumps, it is described to split using tubular structure is split inside tubular fixed-bed reactor, by upper envelope
First 13, low head 14 and kettle composition.Upper cover 13 is provided with charging aperture 1, distributing device 2, mirror mouth 3, man-hole opening 4, hydrogen and gone out
Mouth 6, pressure gauge 7.Respectively split pipe 9 in kettle to be vertically arranged in parallel, upper orifice and the upper cover bottom of every piece tubulation 9 isometric with kettle
The corresponding connection of circular hole being distributed on plate, lower nozzle connection corresponding with the circular hole on low head bottom plate, every splits filled solid in pipe 9
Catalyst 8, split the bottom of pipe 9 and 325 mesh screen packs are installed with low head junction；Thermo detector 12 is located at the outer side of kettle, one end with
The wall contacts of tubulation 9, kettle are externally provided with heat-insulation layer 10, prevent thermal loss.Low head 14 be provided with mirror mouth 3, man-hole opening 4,
Hydrogen inlet 5, material outlet 15.Upper low head 13,14 uses high strength exploitation with kettle respectively.Every grade splits tubular type and fixes
Bed reactor bottom discharging opening is provided with on-line sampler 22, and on-line checking is carried out to hydrogenation conversion.
Course of reaction：Lead to hot coal Jie hot water or conduction oil or steam in shell side, raw material is uniformly heated；Hydrogen is distinguished
The entrance in parallel of pipe reactor bottom 5 is split from different levels, unreacted hydrogen passes through outlet 6 after splitting pipe and returns to hydrogen gas compressors
23.Raw material methyl tetrahydrophthalic anhydride is transported to the top of first-stage reactor 17 by one-level high-pressure circulation pump 16, through charging
Mouthful 1 enters distributing device 2, is equably sprayed onto first-stage reactor 17 and splits the surface of solid catalyst 8 inside pipe 9, after reaction, liquid phase
Secondary cycle pump 18 is entered by outlet 15, then is transported in second reactor 19, after as above reacting, liquid phase again passes by three-level
Circulating pump 20 is transported in third-stage reactor 21.Line sampler 22, Ke Yifen is separately mounted in the bottom of reactor 17,19,21
Do not detect after every stage reactor, the hydrogenation conversion of liquid phase；After third-stage reactor 21, obtained product enters next
Procedure.
Embodiment 2：Industrial applications
100 parts of Raney's nickel, 20 parts of palladium/aluminum oxide, in straight empty dry, the mixing 1.5h of double-cone dryer.Split tubular fixed-bed
Reactor unloads upper cover, and it is 5m to be passed through flow by reactor bottom hydrogen inlet 53/ h nitrogen, counterincision pipe are purged
10min, nitrogen flow are adjusted to 1m3/ h, split being pre-mixed dried catalyst and being filled into by kettle top in pipe, heap
Product density is 0.1~0.5g/ml.After the completion of filling, upper cover is connected.Nitrogen flow is adjusted to 5m3/ h, continue to purge
10min, stop logical nitrogen.
Regulation Hydrogen Vapor Pressure is 6MPa, and hydrogen enters from 17,19,21 bottom inlet of reactor 5 is in parallel, unreacted hydrogen
The reacted upper outlet 6 of device 17,19,21 is returned in hydrogen gas compressor 23.Controlling reaction temperature is 100 DEG C, is contained with quality percentage
The methyl tetrahydrophthalic anhydride measured as more than 98% is raw material, and inlet amount 500Kg/h, it is equal that pressure piping circulates pump pressure
For 8MPa, raw material is delivered to the charging aperture 1 on the top of first-stage reactor 17 by one-level high-pressure circulation pump 16, uniform by distributing device 2
Ground is sprayed onto the splitting in pipe 9 of first-stage reactor 17, is reacted on the surface of composite catalyst 8 with hydrogen, liquid phase passes through one-level
Reactor splits pipe 9, enters two level high-pressure circulation pump 18 by outlet 15, is transported to second reactor 19, is urged again compound
The surface of agent 8 is reacted with hydrogen, then by three-level high-pressure circulation pump 20, into third-stage reactor 21, is continued compound
Catalyst surface is reacted with hydrogen；It is 2 hours that liquid phase splits retention time in tubular fixed-bed reactor in three-level.Sampling inspection
Survey, by first-stage reactor, hydrogenation conversion is 60~70%, and by second reactor, hydrogenation rate of rotation is 85~95%, is passed through
Third-stage reactor, hydrogenation conversion are 95~99%.Liquid phase is directly transferred to next process after third-stage reactor.
Embodiment 3：Industrial applications
100 parts of Raney's nickel, 40 times of palladium/aluminum oxide, in straight empty dry, the mixing 1.5h of double-cone dryer.Split tubular fixed-bed
Reactor unloads upper cover, and it is 5m to be passed through flow by reactor bottom hydrogen inlet 53/ h nitrogen, counterincision pipe are purged
10min, nitrogen flow are adjusted to 1m3/ h, split being pre-mixed dried catalyst and being filled into by kettle top in pipe, heap
Product density is 0.1~0.5g/ml.After the completion of filling, upper cover is connected.Nitrogen flow is adjusted to 5m3/ h, continue to purge
10min, stop logical nitrogen.
Regulation Hydrogen Vapor Pressure is 3MPa, and hydrogen enters from 17,19,21 bottom inlet of reactor 5 is in parallel, unreacted hydrogen
The reacted upper outlet 6 of device 17,19,21 is returned in hydrogen gas compressor 23.Controlling reaction temperature is 80 DEG C, with weight/mass percentage composition
Methyl tetrahydrophthalic anhydride for more than 98% is raw material, and inlet amount 1000Kg/h, it is equal that pressure piping circulates pump pressure
For 8MPa, raw material is delivered to the charging aperture 1 on the top of first-stage reactor 17 by one-level high-pressure circulation pump 16, uniform by distributing device 2
Ground is sprayed onto the splitting in pipe 9 of first-stage reactor 17, is reacted on the surface of composite catalyst 8 with hydrogen, liquid phase passes through one-level
Reactor splits pipe 9, enters two level high-pressure circulation pump 18 by outlet 15, is transported to second reactor 19, is urged again compound
The surface of agent 8 is reacted with hydrogen, then by three-level high-pressure circulation pump 20, into third-stage reactor 21, is continued compound
Catalyst surface is reacted with hydrogen；It is 3 hours that liquid phase splits retention time in tubular fixed-bed reactor in three-level.Sampling inspection
Survey, by first-stage reactor, hydrogenation conversion is 70~75%, and by second reactor, hydrogenation rate of rotation is 85~95%, is passed through
Third-stage reactor, hydrogenation conversion are 95~99%.Liquid phase is directly transferred to next process after third-stage reactor.
Prepare methylhexahydrophthalic anhydride with the utility model device continuous hydrogenation, quality index and technological parameter with
Original batch hydrogenation prepares methylhexahydrophthalic anhydride contrast：
Claims (3)
1. a kind of continuous hydrogenation produces the device of methylhexahydrophthalic anhydride, including splits tubular fixed-bed reactor, raw material
Circulating pump, it is characterised in that：Tubular fixed-bed reactor is split using three-level, respectively splits and passes through raw material between tubular fixed-bed reactor
Circulating pump is connected in series；Described splits using tubular structure is split inside tubular fixed-bed reactor, and filling solid between tube side urges
Agent, it is hot coal Jie's passage that shell side is interior；Every grade splits tubular fixed-bed reactor bottom air inlet and is connected respectively by valve in parallel
Hydrogen Line, every grade splits gas outlet at the top of tubular fixed-bed reactor and connects hydrogen gas compressor by pipeline；Every grade splits tubular type and consolidates
Fixed bed reactor head charging aperture connects feedstock circulation pump；Every grade splits tubular fixed-bed reactor inner top and is respectively fixed with cloth
Device；Every grade splits tubular fixed-bed reactor bottom discharge mouth and is provided with on-line sampler, and on-line checking is carried out to hydrogenation conversion.
2. continuous hydrogenation according to claim 1 produces the device of methylhexahydrophthalic anhydride, it is characterised in that：Split
Tubular fixed-bed reactor is made up of upper low head and kettle, is connected with respectively between upper low head and kettle；Envelope up and down
Head is separately installed with man-hole opening, mirror mouth；Distributing device is installed at the top of upper cover；Tubulation is vertically arranged in parallel inside kettle,
Isometric with kettle, the upper orifice of every tubulation is corresponding with the circular hole being distributed on upper cover bottom plate to be connected, lower nozzle and low head bottom
The corresponding connection of circular hole on plate, tubulation are additionally arranged at the bottom screen pack；Installing heat-insulation layer outside kettle additional, thermo detector is located at kettle side,
And thermo detector one end and tubulation wall contacts.
3. continuous hydrogenation according to claim 1 or 2 produces the device of methylhexahydrophthalic anhydride, its feature exists
In：Hot coal in shell side, which is situated between, selects hot water or deep fat or steam, circulates.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111821919A (en) * | 2020-07-10 | 2020-10-27 | 吉林凯莱英制药有限公司 | Continuous catalytic hydrogenation equipment and continuous catalytic hydrogenation method for pyridine compounds |
| CN113083165A (en) * | 2019-12-23 | 2021-07-09 | 西安市尚华科技开发有限责任公司 | Ultra-high efficiency cluster reactor device |
-
2017
- 2017-05-16 CN CN201720542628.3U patent/CN206767974U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113083165A (en) * | 2019-12-23 | 2021-07-09 | 西安市尚华科技开发有限责任公司 | Ultra-high efficiency cluster reactor device |
| CN113083165B (en) * | 2019-12-23 | 2022-10-25 | 西安市尚华科技开发有限责任公司 | Ultra-high efficiency cluster reactor device |
| CN111821919A (en) * | 2020-07-10 | 2020-10-27 | 吉林凯莱英制药有限公司 | Continuous catalytic hydrogenation equipment and continuous catalytic hydrogenation method for pyridine compounds |
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