CN107935857A - A kind of production method of isooctyl ester nitrate - Google Patents
A kind of production method of isooctyl ester nitrate Download PDFInfo
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- CN107935857A CN107935857A CN201711305777.9A CN201711305777A CN107935857A CN 107935857 A CN107935857 A CN 107935857A CN 201711305777 A CN201711305777 A CN 201711305777A CN 107935857 A CN107935857 A CN 107935857A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/02—Preparation of esters of nitric acid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/30—Micromixers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
Abstract
The present invention provides a kind of production method of isooctyl ester nitrate, mainly include：Pass through apparatus for feeding metering conveying nitric-sulfuric acid that is reliable, stablizing and isooctanol raw material, two strands of raw materials mix and reaction in micro-mixer, mixed material is in micro- heat exchanger through heat exchange, further reacted into single tube reactor, reaction product isolates the different monooctyl ester of acidic nitric and spent acid in automatic segregator, the different monooctyl ester of acidic nitric is rapidly in a series of micro-mixers through conventional washing, alkali cleaning water-washing process again, most afterwards through dry or stand and remove moisture therein up to product isooctyl ester nitrate.The method of the present invention nitrifying process is safe and efficient, and raw material isooctanol conversion ratio and product selectivity are all higher than 99.5%, and product acidity value can reach 0.
Description
Technical field
The present invention relates to micro-reacting tcchnology nitration processes, and in particular to micro-mixer is combined nitre by one kind with tubular reactor
The technique for changing isooctanol production isooctyl ester nitrate.
Background technology
It is industrially extremely hazardous a kind of reaction that alcohols nitrification, which (also has and be referred to as esterified) nitric acid synthesis ester,.Wherein, nitre
It is dual-use two most valuable products in field respectively to change glycerine and isooctyl ester nitrate.
Isooctyl ester nitrate is a kind of important diesel fuel additive, and bavin can be accelerated by improving diesel cetane-number (CN values)
Oil drop fire, improve engine performance.The production of isooctyl ester nitrate is an extremely hazardous reaction process, in the prior art, generally
Produced using the method for mixed acid nitrification isooctanol, be mainly characterized by being configured to nitration mixture with fuming nitric aicd and the concentrated sulfuric acid, with
Excess nitric acid reacts at low temperature with isooctanol, and traditional reaction process is characterized by isooctanol is slowly added dropwise in nitration mixture.Even
Continuous nitration processes are then with injection nitrification and duct type nitrification for representative, including advanced Nilssen-Brunnberg injection nitrifications
Method and Hercules pipeline nitrification processes.The empty injection different monooctyl ester of nitration processes nitric acid synthesis of Xi'an modern age chemistry pressure used, presses blank pipe
Inside and outside injector mixer is formed respectively with two mother tubes, and nitration mixture, alcohol and the empty premixing of pressure, through spraying larynx, expansion segment is emulsified into uniformly
Emulsion liquid carry out nitration reaction, then separated by cooling method.Pipeline nitrification process is mainly by nitration mixture and alcohol in T-shaped pipe
Mixing, reacts in pipeline nitrator, then through refrigerated separation.
The different monooctyl ester of micro-reacting tcchnology nitric acid synthesis is disclosed by Dalian Inst of Chemicophysics, Chinese Academy of Sciences earliest, patent CN
101462962B is nitrified in micro passage reaction obtains product purity 99.5%, yield 98.9%.Patent CN
A kind of method for taking the different monooctyl ester of micro passage reaction nitric acid synthesis is also disclosed that in 201410202348, is mainly characterized by 0-
When reaction 0.5-1 is small at 5 DEG C, how which realizes that the so high residence time is (micro- if being simultaneously not disclosed in micro passage reaction
When more difficult operation 1-2 is small in channel reactor-1Air speed), do not disclose its patent working effect yet.Corning Incorporated has also applied
The patent (CN104892425A) of the different monooctyl ester of nitric acid synthesis in flow reactor, the main sulfur process for using 88-92%, also takes
Obtained preferable patent working effect.The micro- triumphant chemistry in Dalian is disclosed using microring array in its patent CN 201510037012
Device combines nitration processes production isooctyl ester nitrate with shell-and-tube reactor, is mainly characterized by preparing nitration mixture and nitration reaction continuously exists
Two sets of micro-mixers in shell-and-tube reactor with successively carrying out, and nitric acid and isooctanol molar ratio are with 1.0-1.02 in technical parameter:1 is
Optimum condition, and reaction and product are received all between 0-10 DEG C, and the technological reaction thing high conversion rate is in 99%, product yield
More than 98%.
In above-mentioned patent, CN 101462962B principles propose microreactor nitrification isooctanol basic skills, but by
In lacking the understanding to procedure decomposition mechanism and reaction speed, method is not perfect enough；Patent CN201410202348 reaction temperatures
It is low, low reaction space velocities need to be taken or build very long microchannel structure, space hour efficiency is low；CN 104892425A are due to adopting
With the sulfur process of low concentration, nitric acid content is low in its mixed acid, thus spent acid amount bigger.Patent CN
Shell-and-tube reactor is raw safely for nitrate there may be material skewness problem in 201510037012 combination nitration processes
Production process, it is necessary to ensure that reactant is uniformly distributed；Since it is equally reacted between 0-10 DEG C, shell-and-tube reactor volume is big, nitrification
Device liquid holdup height also brings security risk.
Therefore, isooctanol nitrification production isooctyl ester nitrate must pursue safer efficient reaction technology, it is ensured that production
Process safety, product are outstanding.
The content of the invention
For the present invention on the basis of fully research nitration reaction procedure decomposition mechanism and kinetics, nitre is produced by below in proposition
The technical solution of the different monooctyl ester of acid：
A kind of production method of isooctyl ester nitrate, main production equipments include anti-by micro-mixer, micro- heat exchanger and tubular type
The de-nitrification unit for answering device to form, a reaction product automatic segregator, and one group of micro-mixer for being used for washing reaction product.Its
In, de-nitrification unit micro-mixer has the structure that access road drag characteristic is more than hybrid channel drag characteristic, it is preferable that this is micro-
The access road resistance of two materials of mixer is all more than hybrid channel resistance and follow-up micro- heat exchanger and tubular reactor resistance
The sum of, and existing splitlevel mode is pressed in micro-mixer integrated heat exchange unit, microchannel and the hybrid channel of the heat exchange unit
It is integrated, can countercurrent or cocurrent heat exchange operation；One hydraulic diameter for being noteworthy characterized by hot-side channel of micro- heat exchanger is less than
Cold side channel hydraulic diameter；The tubular reactor is single tube reactor, and single tube reactor can be designed different by production scale
The dimensional structure of bore, the preferably single tube reactor set outer tube, lead to cold fluid in casing, for controlling in tubular reactor
Reaction temperature.
The main production of the present invention includes：Pass through apparatus for feeding that is reliable, stablizing such as pumping system metering conveying nitre sulphur
Nitration mixture and isooctanol raw material, wherein nitric-sulfuric acid are prepared with the concentrated sulfuric acid and fuming nitric aicd, and the mass concentration of nitric acid is in nitration mixture
20%~40%, water quality concentration is no more than 5%；Two strands of raw materials are with constant nitre alcohol molar ratio (1.0-1.3):1 described
Mixing and reaction, preferably suitably can first be passed through the nitration mixture a bit of time in de-nitrification unit micro-mixer, then start alcohol charging
Reacted with nitration mixture in micro-mixer, more preferably two strands of raw materials each control stationary temperature to feed and react, preferably former
Expect that nitration mixture and isooctanol temperature control are 0 DEG C~25 DEG C, be usually no more than 30 DEG C.De-nitrification unit micro-mixer, micro- heat exchanger and
Tubular reactor reaction temperature is respectively 40 ± 10 DEG C, 20 ± 10 DEG C, i.e.,：The temperature control of reaction mass outflow micro-mixer outlet
System drops to 20 ± 10 DEG C in micro- heat exchanger after 40 ± 10 DEG C, reaction mass outflow micro-mixer through heat exchange, finally, reaction
Material, which enters back into, completes reaction in single tube reactor.Enter automatic segregator after reaction product cooling, five minutes residence times
Interior continuously to isolate the different monooctyl ester of acidic nitric and spent acid, the different monooctyl ester of acidic nitric is rapidly in one group of micro-mixer through conventional water
Wash, water-washing process obtains anacidity isooctyl ester nitrate again for alkali cleaning, washing process product can use isometric flow with washings or buck
Depickling is mixed, wherein alkali used in alkaline cleaning procedure (such as NaOH) concentration is 0.1~1.0wt%, most removes it through dry or standing afterwards
In moisture up to product isooctyl ester nitrate.To further improve product quality, the control different monooctyl ester of acidic nitric is in first time water
Residence time before washing is less than 30 minutes, on technical method, reduce to the greatest extent nitration product separator volume, liquid storage sump volume and
System pipeline volume.
Nitration reaction of the present invention uses temperature gradient as described above in micro-mixer, micro- heat exchanger, single tube reactor
Lower progress, so that the reaction time is shorter, process is safer, product quality higher.Since micro-mixer interior reaction temperature is high, reaction
Total empty time control of the material in de-nitrification unit is made as 10~100h-1Magnitude, for example, production scale design is annual for 10,000 tons,
Then total effective volume minimum may be selected to be 10 liters inside de-nitrification unit.
Three equipment of de-nitrification unit of the present invention can take independent heat exchange operation, and at this time, different temperatures may be selected in cold medium
With flow.Series connection gradient type heat exchange operation can also be taken, i.e. heat exchange is sequentially first tubular reactor, then micro- heat exchanger, finally
Micro-mixer, and cold medium is adjusted to relatively low temperature, it is preferably 0-5 DEG C, cold medium temperature and flow modulation press foregoing nitrification
Each range of reaction temperature of unit carries out.
Invention effect
The present invention is proposed in patent CN 101462962B technical foundation.It is empty compared with patent CN 201410202348
Shi Genggao；Compared with patent CN 201510037012, single tube reactor is safer, simultaneously because reacting temperature in micro-mixer section
Degree is high, and the patented technology, thus micro- reaction system volume smaller are higher than when empty.
The present invention controls mixed reaction with the uniform mixed reactant isooctanol of micro-mixer and nitration mixture with micro- heat exchanger
Material enters the temperature of tubular reactor, increases the nitration reaction time with single tube reactor, is set by regulating and controlling de-nitrification unit three
Standby reaction time and temperature, make the nitration reaction carry out efficiently, safely within a short period of time：Raw material isooctanol conversion ratio
More than 99.5%, principal product isooctyl ester nitrate selectivity more than 99.5%, both are all higher than 99.5% under optimal conditions, using this
The isooctyl ester nitrate acid content 2~3% of the method generation of invention is (with H2SO4Meter), product acid removal efficiency can reach 100% (acidity
It is worth for 0mgKOH/100ml products), product quality is excellent.
Brief description of the drawings
The nitration processes flow of Fig. 1-production isooctyl ester nitrate
In figure, 1- micro-mixers, the micro- heat exchangers of 2-, 3- single tube reactors, 4- automatic segregators, 5- is containing sour organic products storage
Groove；11- micro-mixer reaction mass access roades, 12- micro-mixer reaction masses hybrid channel, the heat exchange of 13- micro-mixers are situated between
Matter interface, the micro- heat exchanger hot side material interfaces of 21-, the micro- heat exchanger cold medium interfaces of 22-, the cooling collar of 31- single tube reactors,
The different monooctyl ester outlet of 41- automatic segregator acidic nitrics, the outlet of 42- automatic segregators spent acid；F1- reactants isooctanol or nitration mixture,
F2- reactants nitration mixture or isooctanol, F3- remove the different monooctyl ester of acidic nitric that micro-mixer washs；T1- micro-mixer reaction masses go out
Mouth temperature monitoring point, the micro- heat exchanger reacting material outlet temperature monitoring points of T2-, T3- single tube reactor reacting product outlet temperature
Monitoring point.
Embodiment
Referring to embodiment and embodiment, feature of the invention and technique effect are described.
The present invention decomposes mechanism and kinetics of nitrification data according to isooctyl ester nitrate nitration reaction process product, proposes to use
The nitration processes of production isooctyl ester nitrate as shown in Figure 1 (not including washing flow).By micro-mixer 1, micro- in equipment
Heat exchanger 2, tubular reactor 3, automatic segregator 4 and product storage tank 5 form basic de-nitrification unit.1st area of micro-mixer therein
Not in the prior art, in architectural feature, the resistance drop of 11 part of access road is more than the resistance drop of 12 part of hybrid channel, special
Not, the present invention proposes that the resistance drop of 11 part of access road is more than reaction mass in hybrid channel 12, micro- heat exchanger 2 and tubular type
Overall flow rate resistance in reactor 3, the design are mainly to prevent reaction mass nitration mixture from sour phenomenon occurs.Micro-mixer 1 is same
When also there is the access way 13 of heat transferring medium, connected internal cold medium microchannel and 12 countercurrent or cocurrent of hybrid channel
Operation.During nitrification, reaction mass F1 and F2 enter micro-mixer via access road respectively, are mixed in hybrid channel 12 and anti-
Should, the temperature for controlling micro-mixer to export at T1 with the hot operating parameter of shifting when reacting empty by modulation is 40 ± 10 DEG C.Micro- heat exchange
Device 2 is serially connected with after micro-mixer 1 (for the common connection mode of micro-reacting tcchnology), has hot side (reaction in architectural feature
Material side) passage hydraulic diameter is less than cold side (move thermal medium side) passage hydraulic diameter feature, i.e., connected with material interface 21
The hydraulic diameter of internal microchannel is less than the hydraulic diameter of the inside microchannel connected with cold medium interface 22, the main mesh of the design
For further hybrid reaction material.For the present invention, micro- heat exchanger 2 is still mainly used for continuing to reduce reaction mixture temperature,
It is 20 ± 10 DEG C of sections to control the temperature at micro- heat exchanger exit T2.The reaction mass moved by micro- heat exchanger after heat finally enters
Reaction is completed in 3rd nitrification equipment-single tube reactor 3, single tube reactor 3 preferably sets cooling collar 31 and is used to advise greatly at the same time
Mould production time shift heat, when middle and small scale produces, single tube reactor 3 can not also set cooling collar and take immersion or cold Jie of spray
The mode of matter moves thermal control temperature.Reaction product finally isolates the different monooctyl ester of acidic nitric and spent acid, acid nitre in automatic segregator 4
The different monooctyl ester of acid is collected in storage tank 5, and is exported by pump rapidly, goes in a series of micro-mixers to wash depickling；4 He of automatic segregator
Storage tank 5 and the cumulative volume of connecting pipe need to ensure that holdup time of the different monooctyl ester of acidic nitric before depickling is washed is short, generally not
More than 30 minutes, such as：Total mass flow 3.0m3/ h, then the cumulative volume of automatic segregator and storage tank be no more than 1.5m3, preferably two
Person's cumulative volume is preferably less than 0.5m3, holdup time of the different monooctyl ester of acidic nitric before depickling is washed was no more than 10 minutes.
The technical characterstic and technique effect of the present invention is further illustrated with the following examples.It is micro- that embodiment is only exemplified by part
Mixer, micro- heat exchanger and single tube reactor size or size, these examples are all based on reaction scale and select to implement, at it
Its reaction scale or during for production scale, those skilled in the art, which are not difficult to make, other to be converted and obtains identical technology effect
Fruit, these conversion also should be all covered by the range of the technology of the present invention.
Embodiment 1
Nitration processes equipment：Micro-mixer passes through vacuum by 2 600 plates of Inconel after chemical etching goes out microchannel
Diffusion Welding makes, and requires according to the present invention, micro-mixer access road length and width, it is deep separately design be processed as 150mm, 3mm,
0.75mm, hybrid channel are 16, length and width, deep respectively 100mm, 1mm, 0.75mm.Micro- heat exchanger reaction mass wing passage is
32, length and width depth size is identical with micro-mixer hybrid channel.The reaction of 20 × 2.5 × 3000mm of Ф single tubes is connected after micro- heat exchanger
Device, and sleeve heat exchange is set, single tube reactor outlet connection one glass system automatic segregator separation acid ester mixtures.Single tube reactor
Casing and micro- heat exchanger, the shifting passage of heat sequential concatenation of micro-mixer, the constant flow pump delivery heat transfer using maximum flow as 60L/h
Medium moves heat.
Raw material is prepared and feed pump selection：Nitric-sulfuric acid is prepared in advance, and nitre is prepared as raw material using fuming nitric aicd and the concentrated sulfuric acid
Sour mass concentration 23.6%, the nitration mixture that water quality concentration is 5%.Selection two ranges for the good digital of 12L/h control into
Material pump, and the volume flow that reliable fluid flowmeter is used for meter feedstock acid and octanol is matched in respective outlet.In liquid flow
Connecting fluid check-valves is distinguished again close to micro-mixer entry position in gauge rear end.
Nitration reaction：It is 15 DEG C to pre-adjust nitration mixture raw material and isooctanol material temperature, first with the cooling of 48L/h before reaction
Water cycles through whole nitration reaction system.It is anti-that setting nitration mixture feed pump makes nitration mixture first squeeze into nitrification with the flow of flow 3.6L/h
System is answered, treats that flowmeter is stablized in a moment, isooctanol, isooctanol flow control is squeezed into micro-mixer by another feed pump
3L/h is made as, that is, it is 1.2 to control the molar ratio of reactant nitric acid and isooctanol:1, reaction mixture material is in three de-nitrification units
It is total empty when for 12 it is small when-1.At this time, the temperature that reaction mixture material is exported in micro-mixer, micro- heat exchanger and single tube reactor
Degree is respectively 35 DEG C, 25 DEG C, 25 DEG C.
Product separates and washing：The different monooctyl ester of acidic nitric that nitration product is isolated in automatic segregator is rapidly by the 3rd
Platform pump is squeezed into another micro-mixer mixes depickling with isometric clean water, then via the sodium hydrate aqueous solution of 0.4wt%
Continue washing depickling in other micro-mixers with water.
Product analysis method：9790 chromatographs, 150 DEG C of vaporizer, chromatographic column are stood using good fortune：PEG-20000,30m×
0.32mm × 0.5 μm, Cheng Sheng separate 90 DEG C of constant temperature 2.5 minutes, and 30 DEG C/min speed rises to 150 DEG C of constant temperature 8 minutes, is reduced to initial temperature
90℃；Nitrogen is carrier gas, split ratio 40:1；250 DEG C of fid detector.Production concentration is analyzed with this and calculates reaction-ure conversion-age.
Acidity analysis uses standard K OH/ alcoholic solution titrations.
Product analysis result：Isooctanol conversion ratio 99.59%, principal product isooctyl ester nitrate selectivity 99.26%.After washing
Product acidity is 1.6mgKOH/100ml.
Embodiment 2
Nitration processes equipment：Micro-mixer passes through vacuum by 1 600 plate of Inconel after chemical etching goes out microchannel
Diffusion Welding makes, and micro-mixer access road length and width, deep respectively 150mm, 3mm, 0.5mm, hybrid channel is 8, long,
Wide, deep is respectively 100mm, 1mm, 0.5mm.Micro- heat exchanger reaction mass wing passage is 32, length and width depth size and micro-mixer
Hybrid channel is identical.Ф 6 × 1 × 6000mm single tube reactors, one glass of single tube reactor outlet connection are connected after micro- heat exchanger
Automatic segregator processed separates acid ester mixtures.The heat exchanger channels sequential concatenation of micro- heat exchanger, micro-mixer, using maximum flow as
The constant flow pump of 60L/h conveys 20 DEG C of originally water shifting heats.
Raw material is prepared and feed pump selection is the same as embodiment 1.It is same to set fluid flowmeter and check-valves to be connected to feed pump
Between micro-mixer.
Nitration reaction：It is 15 DEG C to pre-adjust nitration mixture raw material and isooctanol material temperature, first with the flow of 48L/h before reaction
20 DEG C of cooling water circulations are kept to pass through the micro- heat exchanger and micro-mixer in nitration reaction system.Setting nitration mixture feed pump makes nitration mixture
Nitration reaction system is first squeezed into the flow of flow 4.3L/h, treats that flowmeter is stablized in a moment, by another feed pump to micro-
Isooctanol is squeezed into mixer, isooctanol flow control is 3.8L/h, that is, the molar ratio for controlling reactant nitric acid and isooctanol is
1.1:1, during total empty in three de-nitrification units of reaction mixture material for 108 it is small when-1.At this time, reaction mixture material is micro- mixed
The temperature of clutch, micro- heat exchanger and single tube reactor outlet is respectively 45 DEG C, 30 DEG C, 25 DEG C.
For nitration product after separation same as Example 1 and washing process, it is different pungent that analysis obtains the nitrifying process raw material
Alcohol conversion 99.91%, product selectivity 99.63%, the product acidity after washing are 0mgKOH/100ml.
Claims (6)
- A kind of 1. production method of isooctyl ester nitrate, it is characterised in that：Main production includes：Conveying nitric-sulfuric acid and isooctanol raw material are measured by apparatus for feeding, two strands of raw materials are micro- mixed Mixing and reaction, mixed material, through heat exchange, react, after reaction in micro- heat exchanger into tubular reactor in clutch Product enters automatic segregator, isolates the different monooctyl ester of acidic nitric and spent acid, the different monooctyl ester of acidic nitric is rapidly a series of micro- mixed Anacidity isooctyl ester nitrate is obtained through alkali cleaning and water-washing process in clutch, product nitric acid that is finally dry or standing removing moisture therein Different monooctyl ester；Main production equipments included by the production method：One by micro-mixer, micro- heat exchanger and tubular reactor structure Into de-nitrification unit, a reaction product automatic segregator, and one group be used for washing reaction product micro-mixer.
- 2. the production method of isooctyl ester nitrate according to claim 1, it is characterised in that：The de-nitrification unit micro-mixer It is more than the structure of hybrid channel drag characteristic with access road drag characteristic, the access road resistance of preferably micro-mixer is more than Hybrid channel resistance and subsequently the sum of micro- heat exchanger and tubular reactor resistance；Micro- heat exchanger is straight with hot-side channel waterpower Footpath is less than cold side channel hydraulic diameter structure；The tubular reactor is single tube reactor, and the single tube reactor can be by life The dimensional structure of scale design difference bore is produced, preferably single tube reactor sets outer tube, leads to cold fluid in casing, for controlling Reaction temperature in tubular reactor.
- 3. according to the method described in claim 1, it is characterized in that：Three equipment of the de-nitrification unit can take independent heat exchange Series connection gradient type heat exchange operation is operated or takes, wherein, heat exchange order is first tubular reactor in gradient type heat exchange operation of connecting, Micro- heat exchanger again, last micro-mixer, and cold medium is adjusted to relatively low temperature, it is preferably 0-5 DEG C.
- 4. the production method of isooctyl ester nitrate according to claim 1, it is characterised in that：Nitric acid in the nitric-sulfuric acid Mass concentration is 20%~40%, water quality concentration 0~5%；Molar ratio when nitric acid is reacted with isooctanol raw material is (1.0- 1.3):1；De-nitrification unit micro-mixer, micro- heat exchange temperature are respectively 40 ± 10 DEG C, 20 ± 10 DEG C；Reaction mass is single in nitrification During sky in member for 10-100 it is small when-1。
- 5. the production method of isooctyl ester nitrate according to claim 1, it is characterised in that reaction product is in automatic segregator In residence time be more than 0 and no more than 5 minutes.
- 6. the production method of isooctyl ester nitrate according to claim 1, it is characterised in that the different monooctyl ester of acidic nitric is washed Buck concentration used in Cheng Zhong, wherein alkaline cleaning procedure is 0.1~1.0wt%.
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| CN110683953A (en) * | 2019-05-15 | 2020-01-14 | 中国科学院大连化学物理研究所 | Method for continuously synthesizing isooctyl nitrate and extracting residual acid in isooctyl nitrate in microreactor |
| CN110981733A (en) * | 2019-12-03 | 2020-04-10 | 江西西林科股份有限公司 | Novel deacidification process for isooctyl nitrate crude product |
| CN112371075A (en) * | 2020-11-09 | 2021-02-19 | 杭州燕麟科技有限公司 | Continuous tubular reaction equipment and preparation method of cyclic phosphonate |
| CN113511982A (en) * | 2020-04-10 | 2021-10-19 | 中国科学院大连化学物理研究所 | Synthetic method of hydroxyethyl hydrazine nitrate |
| CN113713747A (en) * | 2021-09-09 | 2021-11-30 | 西安思科赛实业有限公司 | Nitration micro-heat pipe reaction device and method on halogen-containing benzene ring |
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