CN105566117A - Isooctyl nitrate crude product deacidification method - Google Patents
Isooctyl nitrate crude product deacidification method Download PDFInfo
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- CN105566117A CN105566117A CN201510985897.2A CN201510985897A CN105566117A CN 105566117 A CN105566117 A CN 105566117A CN 201510985897 A CN201510985897 A CN 201510985897A CN 105566117 A CN105566117 A CN 105566117A
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- Prior art keywords
- sodium hydroxide
- crude product
- isooctyl ester
- ester nitrate
- nitrate crude
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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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention discloses an isooctyl nitrate crude product deacidification process, which is characterized that: sodium hydroxide is selected as a deacidification agent, and specifically, a saturated sodium chloride solution of sodium hydroxide is selected. Process steps are as follows: at room temperature, 2.5-10% of saturated sodium chloride solution of sodium hydroxide is added into an isooctyl nitrate crude product for reaction while stirring for 0.5 to 2 hours, the solution is statically stratified, an organic phase is an isooctyl nitrate product, and after an aqueous phase is analyzed, the aqueous phase is recycled by addition of sodium hydroxide. According to the isooctyl nitrate crude product deacidification process, the organic phase and the aqueous phase are quick to separate, the organic phase isooctyl nitrate residue is extremely less in the aqueous phase, and the final product acid number is below 2mg / KOH / 100ml. The isooctyl nitrate crude product deacidification process is simple in operation and low in cost, and the acid value of the product is very ideal.
Description
Technical field
The invention belongs to the production technical field of petrochemicals nitric ether, be specifically related to a kind of acid stripping method of isooctyl ester nitrate crude product.
Technical background
Isooctyl ester nitrate is a kind of diesel cetane-number improver of excellent property, effectively can improve the combustionproperty of diesel oil after adding, and shortens ignition time, and improve locomotive thermal condition kinetics, oil-saving effect is fairly obvious.
The present stage production of isooctyl ester nitrate generally adopts mixed acid process, namely at low temperatures, is added by isooctyl alcohol in the nitration mixture of the vitriol oil and concentrated nitric acid and reacts, react complete separatory, organic phase alkali cleaning, washing, and dry, purifying obtains isooctyl ester nitrate product.
Acid number is the important indicator weighing isooctyl ester nitrate product quality.According to the production technique of existing isooctyl ester nitrate, all need alkali cleaning to remove the free inorganic acid contained in isooctyl ester nitrate crude product, the alkali generally as de-acidying agent is sodium bicarbonate, sodium carbonate and ammoniacal liquor.Chinese invention patent application number is 200610045162.2, and disclose a kind of antacid method of employing ammoniacal liquor, the method needs to be heated to 58-60 DEG C, and energy consumption is higher, and heating isooctyl ester nitrate has potential danger.Adopt sodium bicarbonate and aqueous sodium carbonate to be difficult to reach acid number lower than 3mg/KOH/100ml, and the acid number preserving improper isooctyl ester nitrate product is easy to bounce-back.
Summary of the invention
The object of this invention is to provide a kind of deacidifying process of easy isooctyl ester nitrate crude product, this explained hereafter cost is low, and aqueous phase can recycle, and environmental stress is little, by the isooctyl ester nitrate product acid number of present method process lower than 2mg/KOH/100ml.
The technical solution used in the present invention is:
A kind of acid stripping method of isooctyl ester nitrate crude product, its concrete steps are: the saturated nacl aqueous solution adding 2.5-10% sodium hydroxide in isooctyl ester nitrate crude product, wherein the saturated nacl aqueous solution of sodium hydroxide and isooctyl nitrate crude quality are than being 1:3-5, stir 0.5-2 hour, static separatory, organic phase is isooctyl ester nitrate product, adds appropriate sodium hydroxide recycle after aqueous phase analysis.
Acid in isooctyl ester nitrate crude product is free inorganic acid, adopts inorganic strong alkali to remove.At ambient temperature, with rare sodium hydroxide solution depickling, be easy to during layering produce local emulsification phenomenon.Sodium-chlor is added in rare sodium hydroxide solution, layering is rapid, the residual denier of isooctyl ester nitrate in aqueous phase simultaneously, improve yield, aqueous phase after layering by analysis after, add the saturated nacl aqueous solution recycle that appropriate sodium hydroxide is made into 2.5-10% sodium hydroxide again, alleviate environmental protection pressure, reduce production cost.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1:
A kind of acid stripping method of isooctyl ester nitrate crude product, its concrete steps are: joined by the saturated nacl aqueous solution of 200 gram of 4% sodium hydroxide in 650 grams of isooctyl ester nitrate crude products, stirring reaction 1 hour, static layering, obtain isooctyl ester nitrate product, analysis acid number is 1.2mg/KOH/100ml.Analyze to add after aqueous phase 8 grams of sodium hydroxide make the saturated nacl aqueous solution of 6% sodium hydroxide after for subsequent use.
Embodiment 2:
A kind of acid stripping method of isooctyl ester nitrate crude product, its concrete steps are: joined by the saturated nacl aqueous solution of 200 gram of 6% sodium hydroxide in 800 grams of isooctyl ester nitrate crude products, stirring reaction 1.5 hours, static layering, obtain isooctyl ester nitrate product, analysis acid number is 1.3mg/KOH/100ml.Analyze to add after aqueous phase 9 grams of sodium hydroxide make the saturated nacl aqueous solution of 8% sodium hydroxide after for subsequent use.
Embodiment 3:
A kind of acid stripping method of isooctyl ester nitrate crude product, its concrete steps are: joined by the saturated nacl aqueous solution of 200 gram of 8% sodium hydroxide in 970 grams of isooctyl ester nitrate crude products, stirring reaction 1.5 hours, static layering, obtain isooctyl ester nitrate product, analysis acid number is 0.9mg/KOH/100ml.Analyze to add after aqueous phase 6 grams of sodium hydroxide make the saturated nacl aqueous solution of 8% sodium hydroxide after for subsequent use.
Most preferred embodiment of the present invention is illustrated, and the various change made by those of ordinary skill in the art or remodeling all can not depart from the scope of the present invention.
Claims (5)
1. the acid stripping method of an isooctyl ester nitrate crude product, the steps include: the saturated nacl aqueous solution adding 2.5-10% sodium hydroxide in isooctyl ester nitrate crude product, wherein the saturated nacl aqueous solution of sodium hydroxide and the mass ratio of isooctyl ester nitrate crude product are 1:3-5, stir 0.5-2 hour, static separatory, organic phase is isooctyl ester nitrate product, adds sodium hydroxide recycle after aqueous phase analysis.
2. the acid stripping method of a kind of isooctyl ester nitrate crude product as claimed in claim 1, is characterized in that: described de-acidying agent is sodium hydroxide, is specially the saturated nacl aqueous solution of sodium hydroxide.
3. the acid stripping method of a kind of isooctyl ester nitrate crude product as claimed in claim 2, is characterized in that: the concentration of the saturated nacl aqueous solution of described sodium hydroxide is 2.5-10%.
4. the acid stripping method of a kind of isooctyl ester nitrate crude product as claimed in claim 1, is characterized in that: the saturated nacl aqueous solution of sodium hydroxide and the weight ratio of isooctyl ester nitrate crude product are 1:3-5.
5. the acid stripping method of a kind of isooctyl ester nitrate crude product as claimed in claim 1, it is characterized in that: aqueous phase recycle, concrete steps are that the aqueous phase after separatory adds a certain amount of sodium hydroxide by analysis afterwards, make the saturated nacl aqueous solution that concentration is 2.5-10% sodium hydroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510985897.2A CN105566117A (en) | 2015-12-25 | 2015-12-25 | Isooctyl nitrate crude product deacidification method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510985897.2A CN105566117A (en) | 2015-12-25 | 2015-12-25 | Isooctyl nitrate crude product deacidification method |
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| CN105566117A true CN105566117A (en) | 2016-05-11 |
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| CN201510985897.2A Pending CN105566117A (en) | 2015-12-25 | 2015-12-25 | Isooctyl nitrate crude product deacidification method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106518685A (en) * | 2016-08-15 | 2017-03-22 | 江西苏克尔新材料有限公司 | Method for removing acids and water from isooctyl nitrate |
| 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 |
| CN110922332A (en) * | 2019-12-11 | 2020-03-27 | 江西西林科股份有限公司 | Method for purifying isooctyl nitrate |
| 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 |
| CN112174825A (en) * | 2020-10-30 | 2021-01-05 | 山东益丰生化环保股份有限公司 | Method for reducing acidity of isooctyl nitrate synthesized by using waste acid as raw material |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009080755A1 (en) * | 2007-12-20 | 2009-07-02 | Dsm Fine Chemicals Austria Nfg Gmbh & Co Kg | Formation of nitrate esters in microreactors and millireactors using a continuous product extraction in a turbulent flow regime |
| CN101698646A (en) * | 2009-11-04 | 2010-04-28 | 西安万德化工有限公司 | Continuous production technology for isooctyl nitrate |
| CN102557953A (en) * | 2011-12-29 | 2012-07-11 | 北京理工大学 | Method for preparing alkyl straight chain hydrocarbon monohydric alcohol nitrate ester with 4-10 carbon atoms |
| CN103911194A (en) * | 2013-01-04 | 2014-07-09 | 高剑峰 | Composite type diesel fuel cetane number improver and production process thereof |
| CA2918554A1 (en) * | 2013-08-15 | 2015-02-19 | Josef Meissner Gmbh & Co. Kg | Method and device for removing contaminants arising during the production of aliphatic nitrate esters |
-
2015
- 2015-12-25 CN CN201510985897.2A patent/CN105566117A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009080755A1 (en) * | 2007-12-20 | 2009-07-02 | Dsm Fine Chemicals Austria Nfg Gmbh & Co Kg | Formation of nitrate esters in microreactors and millireactors using a continuous product extraction in a turbulent flow regime |
| CN101698646A (en) * | 2009-11-04 | 2010-04-28 | 西安万德化工有限公司 | Continuous production technology for isooctyl nitrate |
| CN102557953A (en) * | 2011-12-29 | 2012-07-11 | 北京理工大学 | Method for preparing alkyl straight chain hydrocarbon monohydric alcohol nitrate ester with 4-10 carbon atoms |
| CN103911194A (en) * | 2013-01-04 | 2014-07-09 | 高剑峰 | Composite type diesel fuel cetane number improver and production process thereof |
| CA2918554A1 (en) * | 2013-08-15 | 2015-02-19 | Josef Meissner Gmbh & Co. Kg | Method and device for removing contaminants arising during the production of aliphatic nitrate esters |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106518685A (en) * | 2016-08-15 | 2017-03-22 | 江西苏克尔新材料有限公司 | Method for removing acids and water from isooctyl nitrate |
| 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 |
| 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 |
| CN110922332A (en) * | 2019-12-11 | 2020-03-27 | 江西西林科股份有限公司 | Method for purifying isooctyl nitrate |
| CN110922332B (en) * | 2019-12-11 | 2022-11-25 | 江西西林科股份有限公司 | Method for purifying isooctyl nitrate |
| CN112174825A (en) * | 2020-10-30 | 2021-01-05 | 山东益丰生化环保股份有限公司 | Method for reducing acidity of isooctyl nitrate synthesized by using waste acid as raw material |
| CN112174825B (en) * | 2020-10-30 | 2022-10-28 | 益丰新材料股份有限公司 | Method for reducing acidity of isooctyl nitrate synthesized by using waste acid as raw material |
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Application publication date: 20160511 |
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