CN107973718A - A kind of post-processing approach of isooctyl nitrate crude product - Google Patents
A kind of post-processing approach of isooctyl nitrate crude product Download PDFInfo
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- CN107973718A CN107973718A CN201610916909.0A CN201610916909A CN107973718A CN 107973718 A CN107973718 A CN 107973718A CN 201610916909 A CN201610916909 A CN 201610916909A CN 107973718 A CN107973718 A CN 107973718A
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- crude product
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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 Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The present invention relates to a kind of isooctyl ester nitrate（2‑EHN）A kind of post-processing approach of reaction solution, and in particular to post-processing approach of the isooctyl nitrate crude product isolated by reaction solution.Using static mixer as neutralization reactor in the present invention, the post processing of isooctyl nitrate crude product is carried out using shell and tube porous membrane tube filter as desalting dewatering device, simplifies operation, to avoid the generation of solid waste in processing procedure, reduces washes amount；Product water content is not more than 200ppm, is mainly used for the post processing of isooctyl nitrate crude product.
Description
Technical field
The present invention relates to a kind of isooctyl ester nitrate（2-EHN）The post-processing approach of reaction solution, and in particular to one kind is by reacting
The post-processing approach of the isolated isooctyl nitrate crude product of liquid.
Background technology
Isooctyl ester nitrate is a kind of important diesel cetane-number improver, is added to as additive in diesel oil, can be with
Diesel oil spontaneous combustion activation energy is substantially reduced, improves flammability, improves Cetane number.
Generally use nitric-sulfuric acid and the method for isooctanol reaction produce, the isolated organic phase generally use of reaction solution
The post processings such as alkali cleaning, washing, drying obtain product.Alkali cleaning at present, washing usually carry out in a kettle；The method of drying and dehydrating
There are vacuum dehydration, adsorbent adsorption dewatering, utilize oleophilic drainage material dehydration.It is de- that CN1031525A discloses vacuum drying
The method of water, such a method need special vacuum equipment, and investment and operating cost are high.CN1045773A discloses a kind of using close
Oily hydrophobic material dehydrating process, dehydrating material are mainly malthoid, such a material dehydration energy force difference, need further adsorption dewatering.
CN1903829A discloses a kind of dewatering using anhydrous sodium sulfate as adsorbent, anhydrous sodium sulfate water suction easily knot in the method
Block, influences fluid flowing；In addition regeneration and dismounting trouble, need to be handled using the Waste Sulfuric Acid sodium formed after a certain period of time.
CN101696168B disclose it is a kind of with the method that silica gel carries out slightly dehydration, molecular sieve carries out smart dehydration, silica gel in this method, point
Son sieve extends with usage time, and adsorption dewatering reduced capability, silica gel, molecular sieve can not regenerate after regeneration for several times, forms solid waste,
Need in addition it handle.
The content of the invention
It is an object of the invention to provide a kind of post-processing approach of isooctyl ester nitrate reaction solution, and in particular to one kind reaction
The post-processing approach of the isolated isooctyl nitrate crude product of liquid.
The above-mentioned purpose of the present invention is achieved through the following technical solutions：The post processing side of isooctyl nitrate crude product
Method, it is characterized in that using static mixer as neutralization reactor, using shell and tube porous membrane tube filter as desalting dewatering device into
The post processing of row isooctyl nitrate crude product, comprises the following steps：
1）Lye and isooctyl nitrate crude product are squeezed into static mixer respectively, entered in being reacted in static mixer with rear
Oil-moisture liquid device, divides and removes inorganic phase, organic phase enters pans；The relative discharge of lye and organic phase is adjusted, controls the pH to be
7-9；
2）Organic phase after neutralization is sent into shell and tube porous membrane tube filter, after circulating 0.5-5h, is discharged to products pot, is passed through
Required product is obtained after filtering means dehydration.
The shell and tube porous membrane tube filter is cleaned after operation a period of time, shell and tube porous membrane tube mistake during cleaning
Filter A, switch valve to another shell and tube porous membrane tube filter B in parallel；Filter is fed the water into pump, cleans shell and tube
Porous membrane tube filter A, after the completion of cleaning, keeps porous membrane tube in filter A to be soaked in water.
The porous membrane tube is modified ceramic porous membrane tube or stainless steel porous membrane tube.
The modification is that the hydrophilic ability of oleophylic of ceramic membrane is modified, and modified material is polytetrafluoroethylene (PTFE), polysulfide
Ether, polybenzoate one or more of mixture therein.
The size of the perforated membrane of the porous membrane tube is 10-200nm.
The circulation time is 1-1.5h.
The lye amount is adjusted according to the acid-base value of material at static mixer outlet.
Organic phase post-processing approach in the present invention has the advantage that compared with prior art：
1）N-process is carried out in static mixer alternative reaction kettle, improves mixed effect, required space is small；
2）Desalination is removed water with perforated membrane tube filter, good filtration effect, cleaning is simple, easily recovers strainability, no solid
Waste produces, and drastically reduce the area washes.
Brief description of the drawings
Fig. 1 is aftertreatment technology flow diagram in present invention method.
Fig. 2 is A and B filters schematic diagram in present invention method.
In figure, 1- cleaning solutions into valve, 2- cleaning solutions into valve, 3- filtering after product go out valve, 4- filtering after product go out valve, 5-
Cleaning solution goes out valve 1,6-cleaning solution goes out valve 2,7- crude products are into valve 1,8- crude products into valve 2.
Embodiment
Below by embodiment and attached drawing, the present invention is further elaborated, but is not limited only to the present embodiment.
Following embodiments method is referring to attached Fig. 1 and 2.
Embodiment 1
The isooctyl ester nitrate crude product that water content is 10025ppm is squeezed into static mixing with 190ml/min, liquid caustic soda with 10ml/min
Device, enters oil-moisture liquid device after being mixed in static mixer, divides and removes inorganic phase, and inorganic phase pH value is 8；Opening valve 7,
Valve 3, closes remaining valve, the organic phase after neutralization is squeezed into shell and tube porous membrane tube filter, porous membrane tube is poly- four
Fluoride modified 30nm ceramic tubes, in filter circulate 3.0 it is small when after obtain isooctyl ester nitrate, product water content
100ppm。
Embodiment 2
The isooctyl ester nitrate crude product that water content is 10025ppm is squeezed into static mixing with 190ml/min, liquid caustic soda with 12ml/min
Device, enters oil-moisture liquid device after being mixed in static mixer, divides and removes inorganic phase, and inorganic phase pH value is 9；Opening valve 7,
Valve 3, closes remaining valve, the organic phase after neutralization is squeezed into shell and tube porous membrane tube filter, porous membrane tube is poly- four
Fluoride modified 80nm ceramic tubes, in filter circulate 3.0 it is small when after discharge, product water content 190ppm.
Embodiment 3
Polytetrafluoroethylmodified modified 30nm ceramic tubes are changed to polytetrafluoroethylmodified modified 30nm stainless steels by process with embodiment 1
Pipe, product water content 120ppm.
Embodiment 4
Circulation time in filter is changed to 1.5h, product water content 150ppm by process with embodiment 1.
Embodiment 5
Ceramic tube pore size is changed to 80nm, product water content 180ppm by process with embodiment 1.
Embodiment 6
Filter A crude products are closed into valve（7）, product goes out valve after filtering（3）, close filter B cleaning solution and go out valve（6）, cleaning
Liquid is into valve（2）, filter A cleaning solutions are opened into valve（1）, cleaning solution go out valve（5）, filter B crude product is opened into valve（8）, mistake
Product goes out valve after filter（4）, make filter B normal filtration product, filter A is rinsed, and is squeezed into 250ml/min clear water
Filter A, after rinsing 30min, stops intake pump, closes valve 1 and valve 5, keeps porous membrane tube in filter A to be soaked in water
In.
Claims (7)
1. a kind of post-processing approach of isooctyl nitrate crude product, it is characterized in that using static mixer as neutralization reactor, with
Shell and tube porous membrane tube filter carries out the post processing of isooctyl nitrate crude product for desalting dewatering device, comprises the following steps：
1）Lye and isooctyl nitrate crude product are squeezed into static mixer respectively, entered in being reacted in static mixer with rear
Oil-moisture liquid device, divides and removes inorganic phase, organic phase enters pans；The relative discharge of lye and organic phase is adjusted, controls the pH to be
7-9；
2）Organic phase after neutralization is sent into shell and tube porous membrane tube filter, after circulating 0.5-5h, is discharged to products pot, is passed through
Required product is obtained after filtering means dehydration.
2. the post-processing approach of isooctyl nitrate crude product as claimed in claim 1, it is characterised in that the shell and tube perforated membrane
Pipe filter is cleaned after operation a period of time, shell and tube porous membrane tube filter A during cleaning, switch valve to another simultaneously
Join shell and tube porous membrane tube filter B；Filter is fed the water into pump, cleans shell and tube porous membrane tube filter A, cleaning is completed
Afterwards, porous membrane tube in filter A is kept to be soaked in water.
3. the post-processing approach of isooctyl nitrate crude product as claimed in claim 1, it is characterised in that the porous membrane tube is
Modified ceramic porous membrane tube or stainless steel porous membrane tube.
4. the post-processing approach of isooctyl nitrate crude product as claimed in claim 3, it is characterised in that the modification is to pottery
The hydrophilic ability of oleophylic of porcelain film is modified, and modified material is polytetrafluoroethylene (PTFE), polythiaether, polybenzoate one or more therein
Mixture.
5. the post-processing approach of isooctyl nitrate crude product as claimed in claim 1, it is characterised in that the porous membrane tube
The size of perforated membrane is 10-200nm.
6. the post-processing approach of isooctyl nitrate crude product as claimed in claim 1, it is characterised in that circulation time 1-1.5h.
7. the post-processing approach of isooctyl nitrate crude product as claimed in claim 1, it is characterised in that the lye amount according to
The acid-base value of material is adjusted at static mixer outlet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610916909.0A CN107973718A (en) | 2016-10-21 | 2016-10-21 | A kind of post-processing approach of isooctyl nitrate crude product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610916909.0A CN107973718A (en) | 2016-10-21 | 2016-10-21 | A kind of post-processing approach of isooctyl nitrate crude product |
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| CN107973718A true CN107973718A (en) | 2018-05-01 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610916909.0A Pending CN107973718A (en) | 2016-10-21 | 2016-10-21 | A kind of post-processing approach of isooctyl nitrate crude product |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110526822A (en) * | 2018-05-24 | 2019-12-03 | 中国石油化工股份有限公司 | A kind of synthetic method of isooctyl ester nitrate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1045773A (en) * | 1990-03-28 | 1990-10-03 | 齐鲁石油化工公司研究院 | Production process and equipment of isooctyl nitrate |
| CN1814581A (en) * | 2006-02-27 | 2006-08-09 | 中国石油化工集团公司 | Method for synthesizing isooctyl nitrate |
| CN101698646A (en) * | 2009-11-04 | 2010-04-28 | 西安万德化工有限公司 | Continuous production technology for isooctyl nitrate |
| CN103357205A (en) * | 2012-12-27 | 2013-10-23 | 华东理工大学 | Efficient separation recycling method for solid particles of terephthalic acid oxidized mother liquor |
-
2016
- 2016-10-21 CN CN201610916909.0A patent/CN107973718A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1045773A (en) * | 1990-03-28 | 1990-10-03 | 齐鲁石油化工公司研究院 | Production process and equipment of isooctyl nitrate |
| CN1814581A (en) * | 2006-02-27 | 2006-08-09 | 中国石油化工集团公司 | Method for synthesizing isooctyl nitrate |
| CN101698646A (en) * | 2009-11-04 | 2010-04-28 | 西安万德化工有限公司 | Continuous production technology for isooctyl nitrate |
| CN103357205A (en) * | 2012-12-27 | 2013-10-23 | 华东理工大学 | Efficient separation recycling method for solid particles of terephthalic acid oxidized mother liquor |
Non-Patent Citations (2)
| Title |
|---|
| 王唯一 等: "《过滤介质及其选用》", 31 May 2008, 中国纺织出版社 * |
| 王德诚 等 （译）: "《静态混合器 基础和应用》", 30 April 1985, 纺织工业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110526822A (en) * | 2018-05-24 | 2019-12-03 | 中国石油化工股份有限公司 | A kind of synthetic method of isooctyl ester nitrate |
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Application publication date: 20180501 |