CN106699569A - Continuous production process of isooctyl nitrate - Google Patents
Continuous production process of isooctyl nitrate Download PDFInfo
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- CN106699569A CN106699569A CN201610989347.2A CN201610989347A CN106699569A CN 106699569 A CN106699569 A CN 106699569A CN 201610989347 A CN201610989347 A CN 201610989347A CN 106699569 A CN106699569 A CN 106699569A
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- acid
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- continuous production
- isooctanol
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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
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a continuous production process of isooctyl nitrate. The continuous production process comprises the following steps: metering concentrated sulfuric acid and concentrated nitric acid via a metering tank, adding the concentrated sulfuric acid and the concentrated nitric acid into a stirring kettle for uniformly stirring and mixing; respectively injecting mixed acid and isooctanol into two coolers for cooling, injecting the mixed acid and the isooctanol into a reactor assembly for mixing and reacting after the mixed acid and isooctanol are cooled to be lower than or equal to 15 DEG C, and firstly mixing in an efficient mixer in the reactor assembly; adding the uniformly-mixed material into a reaction thin tube through a distribution tank for reacting, and filling the periphery of the fine tube with cooling water; collecting reaction products via a collector, then adding the reaction products into a centrifugal machine for separating acid ester, and removing waste acid; refining and deacidifying coarse products via a 10wt% sodium hydroxide solution in an alkaline washing tower; enabling deacidified products to continuously flow into a settling tank from the alkaline washing tower for settling and dewatering, and adding the deacidified products into a drying tower for drying to obtain a product. Through the production process, the problem about safety in the existing process is solved; the production efficiency is improved; the production stability is improved; the cost is reduced.
Description
Technical field
The present invention relates to petrochemical field, and in particular to a kind of continuous production processes of isooctyl ester nitrate.
Background technology
Isooctyl ester nitrate is that, used as diesel cetane-number improver, prior synthesizing method is the nitre with the concentrated sulfuric acid as catalyst
Change isooctanol to be obtained.The reaction characteristicses are：（1）When reacting initial temperature is more than 30 DEG C, almost moment completes for reaction, and isooctanol is each
The reaction speed of nitration mixture depends on certainly in the mass transfer rate of two-phase.（2）Exothermic heat of reaction amount is big, it has been reported that the exothermic heat of reaction amount is
700KJ/Kg alcohol.（3）Reaction generation heat makes system material（The mixture of isooctyl ester nitrate and nitration mixture）When temperature is increased to 40 DEG C,
Radical reaction is easily resolved into the oxidation acid environment of product isooctyl ester nitrate, bigger heat is produced, ultimately resulted in quick-fried
It is fried.At present, the production technology of existing isooctyl ester nitrate mainly has autoclave to produce, injection is produced and the trans reaction process of micro-pipe.Kettle
Formula is produced and injection production system retaining amount is big, and system film-cooled heat is small, reaction temperature runaway blast easily out of control, low production efficiency, no
Continuous production can be realized；Micro-tubular reaction process, production process is unstable, and the technique improve production efficiency is by acid alcohol arranged side by side point
Carry out improve production efficiency with quantity and the micro- reaction tube quantity of increase, have the disadvantage：Charging must respectively be managed by distribution pipe, and distribution pipe
Flow is equal, but actual production, because of the reason such as capillary inside diameter precision and pipeline length, bending, causes each distribution pipe flow not
Uniformly, when the nitre alcohol ratio in micro-pipe reactor is entered less than 1, the complete isooctanol of unreacted into ester acid knockout drum is had, not
The isooctanol for having reacted can flow into the middle excess nitric acid reaction of ester acid knockout drum with other micro-pipes, so as to cause ester acid knockout drum temperature
Degree rises, and ultimately results in temperature runaway blast.And side-by-side reactions pipe quantity is more, above-mentioned situation is more also easy to produce.Thus limit wall scroll
The production capacity of production line.Meanwhile, nitration mixture will be preheated before entering micro-pipe reactor with isooctanol, and reacting initial temperature is 40 ~ 70 DEG C,
Initial reaction temperature is too high, and almost moment completes for reaction, and generation heat is big, is also easy to produce bombing event, makes production be forced to stop.Cause
This, there is provided a kind of continuous production processes of isooctyl ester nitrate, it is critical only that：Nitration mixture and the abundant mass transfer of alcohol should be ensured, controlled again
Reaction speed processed, therefore control starting material feeding temperature, reduce reaction speed critically important.Heat energy power is removed in reinforcing cooling, makes body
It is temperature of charge critically important less than 40 DEG C.
The content of the invention
The technical problem to be solved：It is an object of the invention to provide a kind of continuous production processes of isooctyl ester nitrate, overcome
The safety problem of existing process, improve production efficiency improves production stability, reduces cost.
Technical scheme：A kind of continuous production processes of isooctyl ester nitrate, comprise the following steps：
The first step：The concentrated sulfuric acid and concentrated nitric acid are measured by measuring tank, is stirred in putting into stirred tank for 0.4-0.8 by volume
Mix well mixed；
Second step：By nitration mixture and isooctanol by measuring pump by volume flow ratio for 0.6-1.3 is injected separately into two coolers
In cooled down, less than or equal to 15 DEG C after hybrid reaction is carried out in injecting reactor component, the first height among reactor assemblies
First mixed in effect blender, incorporation time is 5-20ms；
3rd step：Well mixed material by being reacted in distributing trough entrance reaction tubule, is connected with cooling again around tubule
Water, the reaction time is 5-25s；
4th step：Product carries out ester acid and separates after current collector afflux into centrifuge, removes spent acid；
5th step：Crude product carries out in caustic wash tower refined depickling with 10wt% sodium hydroxide solutions, wherein, crude product and hydrogen-oxygen
The volume ratio for changing sodium solution is 1:1.5-1:2；
6th step：Deacidified prod continuously flows into settling tank and carries out deposition dehydrating from caustic wash tower, enters back into and be drying to obtain in drying tower
Product.
Further, reactor assemblies include in second step：Alcohol feed pipe, sour feed pipe, Hi-mixer, reaction are thin
Pipe, current collector and discharge nozzle.
Further, in second step and the 3rd step nitration mixture and isooctanol respectively after the distributing trough of Hi-mixer is distributed
Collision type mixing is carried out, wherein distributing trough is divided into 8 grooves successively according to one-to-two, two point four, four point eight etc., and acid alcohol is by distribution
After branch groove collisional mixing, then distributing trough after concentrating collisional mixing uniform again in Hi-mixer again by one-to-two, two point four,
After four point of eight grade is divided into 8 plumes successively, reacted into the reaction tubule being connected with Hi-mixer；Reacted product
Several tributaries are concentrated into by a big stream by the afflux groove in current collector and enter discharge nozzle.
Further, the equivalent latus rectum of the distributing trough of the distributing trough of Hi-mixer and current collector is 0.5-4mm；Reaction is thin
Manage the acidproof steel pipe for 0.5mm-4mm for caliber.
Further, cooling water temperature is 10-18 DEG C in the 3rd step, and flow velocity is 1.5m/s-3.0m/s.
Beneficial effect：A kind of continuous production processes of isooctyl ester nitrate of the invention, acid alcohol feeding temperature is controlled at 15 DEG C
Hereinafter, the residence time be less than 20ms, mixed using collision type Forced Mixing device, that is, ensure that mass transfer velocity, control again
The extent of reaction of the material in blender, will not produce bombing event, safety.While this technique is consecutive production, small investment,
Production efficiency is high, it is easy to industrialize.
Brief description of the drawings
Fig. 1 is a kind of schematic diagram of the reactor assemblies used in continuous production processes of isooctyl ester nitrate.
Specific embodiment
Embodiment 1
A kind of continuous production processes of isooctyl ester nitrate, comprise the following steps：
The first step：The concentrated sulfuric acid and concentrated nitric acid are measured by measuring tank, it is mixed to be stirred in 0.8 input stirred tank by volume
Close uniform；
Second step：Nitration mixture and isooctanol are injected separately into in two coolers and carried out for 1 by measuring pump by volume flow ratio
Cooling, temperature is that hybrid reaction is carried out in injecting reactor component after 15 DEG C, first the Hi-mixer among reactor assemblies
Middle first to be mixed, incorporation time is 10ms；
3rd step：Well mixed material by being reacted in distributing trough entrance reaction tubule, is connected with cooling again around tubule
Water, the reaction time is 23s, and cooling water temperature is 10 DEG C, and flow velocity is 3.0m/s；
4th step：Product carries out ester acid and separates after current collector afflux into centrifuge, removes spent acid；
5th step：Crude product carries out in caustic wash tower refined depickling with 10wt% sodium hydroxide solutions, wherein, crude product and hydrogen-oxygen
The volume ratio for changing sodium solution is 1:2；
6th step：Deacidified prod continuously flows into settling tank and carries out deposition dehydrating from caustic wash tower, enters back into and be drying to obtain in drying tower
Product.
Gained product yield is 96.7%, and purity is 99.3%.
Embodiment 2
A kind of continuous production processes of isooctyl ester nitrate, comprise the following steps：
The first step：The concentrated sulfuric acid and concentrated nitric acid are measured by measuring tank, it is mixed to be stirred in 0.7 input stirred tank by volume
Close uniform；
Second step：Nitration mixture and isooctanol are passed through into measuring pump by volume flow ratio for 0.91 is injected separately into in two coolers
Row cooling, temperature is that hybrid reaction is carried out in injecting reactor component after 13 DEG C, the first efficient mixing among reactor assemblies
First mixed in device, incorporation time is 15ms；
3rd step：Well mixed material by being reacted in distributing trough entrance reaction tubule, is connected with cooling again around tubule
Water, the reaction time is 15s, and cooling water temperature is 12 DEG C, and flow velocity is 2.5m/s；
4th step：Product carries out ester acid and separates after current collector afflux into centrifuge, removes spent acid；
5th step：Crude product carries out in caustic wash tower refined depickling with 10wt% sodium hydroxide solutions, wherein, crude product and hydrogen-oxygen
The volume ratio for changing sodium solution is 1:1.5；
6th step：Deacidified prod continuously flows into settling tank and carries out deposition dehydrating from caustic wash tower, enters back into and be drying to obtain in drying tower
Product.
Gained product yield is 97.4%, and purity is 99.2%.
Embodiment 3
A kind of continuous production processes of isooctyl ester nitrate, comprise the following steps：
The first step：The concentrated sulfuric acid and concentrated nitric acid are measured by measuring tank, it is mixed to be stirred in 0.4 input stirred tank by volume
Close uniform；
Second step：Nitration mixture and isooctanol are passed through into measuring pump by volume flow ratio for 0.6 is injected separately into in two coolers
Row cooling, temperature is that hybrid reaction is carried out in injecting reactor component after 10 DEG C, the first efficient mixing among reactor assemblies
First mixed in device, incorporation time is 5ms；
3rd step：Well mixed material by being reacted in distributing trough entrance reaction tubule, is connected with cooling again around tubule
Water, the reaction time is 5s, and cooling water temperature is 15 DEG C, and flow velocity is 1.5m/s；
4th step：Product carries out ester acid and separates after current collector afflux into centrifuge, removes spent acid；
5th step：Crude product carries out in caustic wash tower refined depickling with 10wt% sodium hydroxide solutions, wherein, crude product and hydrogen-oxygen
The volume ratio for changing sodium solution is 1:1.7；
6th step：Deacidified prod continuously flows into settling tank and carries out deposition dehydrating from caustic wash tower, enters back into and be drying to obtain in drying tower
Product.
Gained product yield is 97.1%, and purity is 99.1%.
Embodiment 4
A kind of continuous production processes of isooctyl ester nitrate, comprise the following steps：
The first step：The concentrated sulfuric acid and concentrated nitric acid are measured by measuring tank, it is mixed to be stirred in 0.5 input stirred tank by volume
Close uniform；
Second step：Nitration mixture and isooctanol are passed through into measuring pump by volume flow ratio for 1.3 are injected separately into in two coolers
Row cooling, carries out hybrid reaction, first the Hi-mixer among reactor assemblies in injecting reactor component after 15 DEG C of temperature
Middle first to be mixed, incorporation time is 20ms；
3rd step：Well mixed material by being reacted in distributing trough entrance reaction tubule, is connected with cooling again around tubule
Water, the reaction time is 10s, and cooling water temperature is 18 DEG C, and flow velocity is 2.0m/s；
4th step：Product carries out ester acid and separates after current collector afflux into centrifuge, removes spent acid；
5th step：Crude product carries out in caustic wash tower refined depickling with 10wt% sodium hydroxide solutions, wherein, crude product and hydrogen-oxygen
The volume ratio for changing sodium solution is 1:1.6；
6th step：Deacidified prod continuously flows into settling tank and carries out deposition dehydrating from caustic wash tower, enters back into and be drying to obtain in drying tower
Product.
Gained product yield is 97.9%, and purity is 99.8%.
Embodiment 5
A kind of continuous production processes of isooctyl ester nitrate, comprise the following steps：
The first step：The concentrated sulfuric acid and concentrated nitric acid are measured by measuring tank, it is mixed to be stirred in 0.6 input stirred tank by volume
Close uniform；
Second step：Nitration mixture and isooctanol are passed through into measuring pump by volume flow ratio for 0.9 is injected separately into in two coolers
Row cooling, temperature is that hybrid reaction is carried out in injecting reactor component after 12 DEG C, the first efficient mixing among reactor assemblies
First mixed in device, incorporation time is 12ms；
3rd step：Well mixed material by being reacted in distributing trough entrance reaction tubule, is connected with cooling again around tubule
Water, the reaction time is 25s, and cooling water temperature is 16 DEG C, and flow velocity is 2.2m/s；
4th step：Product carries out ester acid and separates after current collector afflux into centrifuge, removes spent acid；
5th step：Crude product carries out in caustic wash tower refined depickling with 10wt% sodium hydroxide solutions, wherein, crude product and hydrogen-oxygen
The volume ratio for changing sodium solution is 1:1.9；
6th step：Deacidified prod continuously flows into settling tank and carries out deposition dehydrating from caustic wash tower, enters back into and be drying to obtain in drying tower
Product.
Gained product yield is 97.2%, and purity is 99.5%.
Claims (5)
1. a kind of continuous production processes of isooctyl ester nitrate, it is characterised in that：Comprise the following steps：
The first step：The concentrated sulfuric acid and concentrated nitric acid are measured by measuring tank, is stirred in putting into stirred tank for 0.4-0.8 by volume
Mix well mixed；
Second step：By nitration mixture and isooctanol by measuring pump by volume flow ratio for 0.6-1.3 is injected separately into two coolers
In cooled down, less than or equal to 15 DEG C after hybrid reaction is carried out in injecting reactor component, the first height among reactor assemblies
First mixed in effect blender, incorporation time is 5-20ms；
3rd step：Well mixed material by being reacted in distributing trough entrance reaction tubule, is connected with cooling again around tubule
Water, the reaction time is 5-25s；
4th step：Product carries out ester acid and separates after current collector afflux into centrifuge, removes spent acid；
5th step：Crude product carries out in caustic wash tower refined depickling with 10wt% sodium hydroxide solutions, wherein, crude product and hydrogen-oxygen
The volume ratio for changing sodium solution is 1:1.5-1:2；
6th step：Deacidified prod continuously flows into settling tank and carries out deposition dehydrating from caustic wash tower, enters back into and be drying to obtain in drying tower
Product.
2. continuous production processes of a kind of isooctyl ester nitrate according to claim 1, it is characterised in that：In the second step
Reactor assemblies include：Alcohol feed pipe（1）, sour feed pipe（2）, Hi-mixer（3）, reaction tubule（4）, current collector（5）With
Discharge nozzle（6）.
3. continuous production processes of a kind of isooctyl ester nitrate according to claim 1, it is characterised in that：The second step and
Nitration mixture and isooctanol pass through Hi-mixer respectively in 3rd step（3）Distributing trough distribution after carry out collision type mixing, wherein dividing
It is divided into 8 grooves successively according to one-to-two, two point four, four point eight etc. with groove, acid alcohol is after distributing branch groove collisional mixing, then concentrates
Distributing trough after collisional mixing is uniform again in Hi-mixer is divided into 8 plumes successively by one-to-two, two point four, four point eight etc. again
Afterwards, into the reaction tubule being connected with Hi-mixer（4）In reacted；Reacted product passes through current collector（5）In
Several tributaries are concentrated into a big stream and enter discharge nozzle by afflux groove（6）.
4. continuous production processes of a kind of isooctyl ester nitrate according to claim 2, it is characterised in that：The efficient mixing
Device（3）Distributing trough and current collector（5）Distributing trough equivalent latus rectum be 0.5-4mm；Described reaction tubule（4）For caliber is
The acidproof steel pipe of 0.5mm-4mm.
5. continuous production processes of a kind of isooctyl ester nitrate according to claim 1, it is characterised in that：In 3rd step
Cooling water temperature is 10-18 DEG C, and flow velocity is 1.5m/s-3.0m/s.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610989347.2A CN106699569A (en) | 2016-11-10 | 2016-11-10 | Continuous production process of isooctyl nitrate |
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| CN201610989347.2A CN106699569A (en) | 2016-11-10 | 2016-11-10 | Continuous production process of isooctyl nitrate |
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| CN201610989347.2A Pending CN106699569A (en) | 2016-11-10 | 2016-11-10 | Continuous production process of isooctyl nitrate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107935857A (en) * | 2017-12-11 | 2018-04-20 | 中国科学院大连化学物理研究所 | A kind of production method of isooctyl ester nitrate |
| CN108147968A (en) * | 2018-01-02 | 2018-06-12 | 山东益丰生化环保股份有限公司 | A kind of continuous aftertreatment technology of isooctyl ester nitrate and equipment |
| CN108325492A (en) * | 2018-03-14 | 2018-07-27 | 荆门市熊兴化工有限公司 | A kind of nitration processes and device preparing H acid |
| CN110803991A (en) * | 2019-12-03 | 2020-02-18 | 江西西林科股份有限公司 | Method for synthesizing isooctyl nitrate by micro-reaction technology |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101698646A (en) * | 2009-11-04 | 2010-04-28 | 西安万德化工有限公司 | Continuous production technology for isooctyl nitrate |
| CN101733056A (en) * | 2008-11-07 | 2010-06-16 | 中国科学院大连化学物理研究所 | Impinging stream micro-channel reactor and application |
| CN104557556A (en) * | 2015-01-26 | 2015-04-29 | 大连微凯化学有限公司 | Device and process method for producing isooctyl nitrate |
-
2016
- 2016-11-10 CN CN201610989347.2A patent/CN106699569A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101733056A (en) * | 2008-11-07 | 2010-06-16 | 中国科学院大连化学物理研究所 | Impinging stream micro-channel reactor and application |
| CN101698646A (en) * | 2009-11-04 | 2010-04-28 | 西安万德化工有限公司 | Continuous production technology for isooctyl nitrate |
| CN104557556A (en) * | 2015-01-26 | 2015-04-29 | 大连微凯化学有限公司 | Device and process method for producing isooctyl nitrate |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107935857A (en) * | 2017-12-11 | 2018-04-20 | 中国科学院大连化学物理研究所 | A kind of production method of isooctyl ester nitrate |
| CN108147968A (en) * | 2018-01-02 | 2018-06-12 | 山东益丰生化环保股份有限公司 | A kind of continuous aftertreatment technology of isooctyl ester nitrate and equipment |
| CN108325492A (en) * | 2018-03-14 | 2018-07-27 | 荆门市熊兴化工有限公司 | A kind of nitration processes and device preparing H acid |
| CN108325492B (en) * | 2018-03-14 | 2023-12-19 | 湖北丽康源化工有限公司 | Nitration technology and device for preparing H acid |
| CN110803991A (en) * | 2019-12-03 | 2020-02-18 | 江西西林科股份有限公司 | Method for synthesizing isooctyl nitrate by micro-reaction technology |
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Application publication date: 20170524 |