CN102911049A - Method for preparing dinonyl adipate by utilizing refining agent - Google Patents
Method for preparing dinonyl adipate by utilizing refining agent Download PDFInfo
- Publication number
- CN102911049A CN102911049A CN 201210459073 CN201210459073A CN102911049A CN 102911049 A CN102911049 A CN 102911049A CN 201210459073 CN201210459073 CN 201210459073 CN 201210459073 A CN201210459073 A CN 201210459073A CN 102911049 A CN102911049 A CN 102911049A
- Authority
- CN
- China
- Prior art keywords
- dinonyl adipate
- finishing agent
- refining
- weight ratio
- utilizing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for preparing dinonyl adipate by utilizing a refining agent. The method comprises the following steps: esterifying, namely, putting adipic acid, nonyl alcohol and concentrated sulfuric acid in a reaction kettle, stirring, carrying micro vacuumizing, heating to boil, reacting, and separating out water in the reaction under the condition that the boiling reflux state is maintained, wherein the weight ratio of adipic acid to nonyl alcohol to concentrated sulfuric acid is 1:2.2:(0.002-0.005); and then washing, dealcoholizing, refining and filtering. According to the refining method of dinonyl adipate, in the refining step, due to use of the refining agent, the color of the obtained product is light, the obtained product can be sold without high-vacuum refining treatment, and the quality of the prepared product completely meets the technical index requirements.
Description
Technical field
The invention belongs to the organic compound preparation field, especially a kind of method of utilizing finishing agent to prepare dinonyl adipate.
Background technology
In industrial production, plastics industry and war production, dinonyl adipate has more and more widely and uses as a kind of important organic compounds and cold resistant plasticizer.The common production method of dinonyl adipate is the direct esterification reaction, obtain the color of product for yellow, be difficult to sell as product, must further make with extra care, the refinement treatment that namely reduces pressure step, the problem that this type of preparation method exists: 1. owing to needing to use expensive high-vacuum pump to realize in the decompression refinement treatment step, therefore, there is the problem that production unit is many, expense is high in the method, thereby is difficult to reduce cost; 2. because decompression refinement treatment step is to produce essential and very consuming time production stage in the dinonyl adipate process, therefore, there is the problem that the production time is long, production efficiency is low in the method, is unfavorable for the raising of Business Economic Benefit.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of dinonyl adipate preparation method that can save facility investment, reduce cost, shorten the production time and can enhance productivity is provided.
It is to realize by the following technical solutions that the present invention solves its technical problem:
A kind of method of utilizing finishing agent to prepare dinonyl adipate, method may further comprise the steps:
⑴ step of esterification
Hexanodioic acid, nonyl alcohol, the vitriol oil are dropped in the reactor, stir, be heated to boiling reaction, keep boiling reflux state separation moisture wherein;
⑵ water-washing step
To add entry in the mixture after the esterification, after stirring, standing demix is removed water layer wherein;
⑶ dealcoholysis step
With the mixture after the washing, dealcoholysis obtains the dinonyl adipate crude product;
⑷ purification step
To add finishing agent in the crude product after the dealcoholysis, stirred refining 1 hour;
⑸ filtration step
Mixed solution after refining is filtered, obtain the dinonyl adipate product.
Described finishing agent is yellow soda ash, magnesiumcarbonate, gac, sal epsom weight ratio, mixes by 0.5:1:2:1.5.
The weight ratio of described finishing agent and hexanodioic acid is 0.005-0.01:1
Described hexanodioic acid, nonyl alcohol, the weight ratio of the vitriol oil is 1:2.2:0.002-0.005
The weight ratio of described water and hexanodioic acid is 0.5:1.
Advantage of the present invention and positively effect are:
1. this utilizes finishing agent to prepare the method for dinonyl adipate in purification step, use finishing agent (yellow soda ash, magnesiumcarbonate, gac, sal epsom mixture), the product colour that obtains shoals, do not need the high vacuum refinement treatment namely to can be used as product and sell, prepared quality product meets the technical requirements fully.
2. the finishing agent that uses of this method of utilizing finishing agent to prepare dinonyl adipate is yellow soda ash, magnesiumcarbonate, gac, sal epsom mixture, have cheap, the characteristics that are easy to purchase.
3. this method of utilizing finishing agent to prepare dinonyl adipate has easy to operately, simplely is convenient to realize suitability for industrialized production, enhances productivity.
4. the present invention uses finishing agent fully to guarantee quality product and prolonged storage stability in process of production, and it is simple that simultaneously the present invention has realization, easy to operate characteristics, and the investment of having saved production unit has improved production efficiency.
5. this preparation method has saved the high vacuum purification step when producing, and has avoided the input of high-vacuum pump equipment, therefore, has saved facility investment, reduces production costs, and has improved the competitiveness of product in market.
Embodiment
Below in conjunction with embodiment, following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
Embodiment 1
A kind of method of utilizing finishing agent to prepare dinonyl adipate may further comprise the steps:
⑴ step of esterification
To one with heating unit, electricity stirs, and drops into successively the hexanodioic acid double centner in 500 liters of reactors of thermometer water circulation condenser and water-and-oil separator, 220 kilograms of nonyl alcohols, 0.3 kilogram of the vitriol oil, under agitation, micro-vacuum, be heated to simultaneously boiling reaction, keep the boiling reflux state, constantly from water-and-oil separator with moisture from going out, until after not having moisture to generate, stopped heating, esterification stops.
⑵ water-washing step
Obtain after the esterification to such an extent that add 50 kg water in the mixed solution, after stirring, standing demix is removed water layer wherein.
⑶ dealcoholysis step
With the mixture after the washing, dealcoholysis obtains crude product, dinonyl adipate.
⑷ purification step
Add 0.5 kilogram of finishing agent (yellow soda ash, magnesiumcarbonate, gac, sal epsom mixture mix by weight 0.5:1:2:1.5) in the crude product after the dealcoholysis, mix 1 hour.
⑸ filtration step
Refined mixed solution is filtered, and the liquid that obtains is the dinonyl adipate finished product, this dinonyl adipate content 99.5%, and color is less than No. 30 (platinum-cobalt colorimetric).
Embodiment 2
A kind of method of utilizing finishing agent to prepare dinonyl adipate may further comprise the steps:
⑴ step of esterification
To one with heating unit, electricity stirs, and drops into successively the hexanodioic acid double centner in 500 liters of reactors of thermometer water circulation condenser and water-and-oil separator, 220 kilograms of nonyl alcohols, 0.3 kilogram of the vitriol oil, under agitation, micro-vacuum, be heated to simultaneously boiling reaction, keep the boiling reflux state, constantly from water-and-oil separator with moisture from going out, until after not having moisture to generate, stopped heating, esterification stops.
⑵ water-washing step
Obtain after the esterification to such an extent that add 50 kg water in the mixed solution, after stirring, standing demix is removed water layer wherein.
⑶ dealcoholysis step
With the mixture after the washing, dealcoholysis obtains crude product, dinonyl adipate.
⑷ purification step
Add 0.6 kilogram of finishing agent (yellow soda ash, magnesiumcarbonate, gac, sal epsom mixture mix by weight 0.5:1:2:1.5) in the crude product after the dealcoholysis, mix 1 hour.
⑸ filtration step
Refined mixed solution is filtered, and the liquid that obtains is the dinonyl adipate finished product, this dinonyl adipate content 99.5%, and color is less than No. 30 (platinum-cobalt colorimetric).
Embodiment 3
A kind of method of utilizing finishing agent to prepare dinonyl adipate may further comprise the steps:
⑴ step of esterification
To one with heating unit, electricity stirs, and drops into successively the hexanodioic acid double centner in 500 liters of reactors of thermometer water circulation condenser and water-and-oil separator, nonyl alcohol `220 kilogram, 0.3 kilogram of the vitriol oil, under agitation, micro-vacuum, be heated to simultaneously boiling reaction, keep the boiling reflux state, constantly from water-and-oil separator with moisture from going out, until after not having moisture to generate, stopped heating, esterification stops.
⑵ water-washing step
Obtain after the esterification to such an extent that add 50 kg water in the mixed solution, after stirring, standing demix is removed water layer wherein.
⑶ dealcoholysis step
With the mixture after the washing, dealcoholysis obtains crude product, dinonyl adipate.
⑷ purification step
Add 0.7 kilogram of finishing agent (yellow soda ash, magnesiumcarbonate, gac, sal epsom mixture mix by weight 0.5:1:2:1.5) in the crude product after the dealcoholysis, mix 1 hour.
⑸ filtration step
Refined mixed solution is filtered, and the liquid that obtains is the dinonyl adipate finished product, this dinonyl adipate content 99.5%, and color is less than No. 30 (platinum-cobalt colorimetric).
Claims (3)
1. method of utilizing finishing agent to prepare dinonyl adipate, it is characterized in that: method may further comprise the steps:
⑴ step of esterification
Hexanodioic acid, nonyl alcohol, the vitriol oil are dropped in the reactor, stir, be heated to boiling reaction, keep boiling reflux state separation moisture wherein;
The weight ratio of described hexanodioic acid, nonyl alcohol, the vitriol oil is 1:2.2:0.002-0.005;
⑵ water-washing step
To add entry in the mixture after the esterification, after stirring, standing demix is removed water layer wherein;
⑶ dealcoholysis step
With the mixture after the washing, dealcoholysis obtains the dinonyl adipate crude product;
⑷ purification step
To add finishing agent in the crude product after the dealcoholysis, stirred refining 1 hour;
Described finishing agent is yellow soda ash, magnesiumcarbonate, gac, sal epsom weight ratio, mixes by 0.5:1:2:1.5;
⑸ filtration step
Mixed solution after refining is filtered, obtain the dinonyl adipate product.
2. the method for utilizing finishing agent to prepare dinonyl adipate according to claim 1, it is characterized in that: the weight ratio of described finishing agent and hexanodioic acid is 0.005-0.01:1.
3. the method for utilizing finishing agent to prepare dinonyl adipate according to claim 1, it is characterized in that: the weight ratio of described water and hexanodioic acid is 0.5:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210459073 CN102911049A (en) | 2012-11-14 | 2012-11-14 | Method for preparing dinonyl adipate by utilizing refining agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210459073 CN102911049A (en) | 2012-11-14 | 2012-11-14 | Method for preparing dinonyl adipate by utilizing refining agent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102911049A true CN102911049A (en) | 2013-02-06 |
Family
ID=47609655
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201210459073 Pending CN102911049A (en) | 2012-11-14 | 2012-11-14 | Method for preparing dinonyl adipate by utilizing refining agent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102911049A (en) |
-
2012
- 2012-11-14 CN CN 201210459073 patent/CN102911049A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102249909A (en) | Method for preparing bis(2-ethylhexyl)adipate | |
| CN101914018A (en) | Method for preparing sebacic acid di-n-butyl ester | |
| CN102320975A (en) | Method for refining tri-n-octyl trimellitate and used refining agent thereof | |
| CN103288638A (en) | Preparation method of diisooctyl adipate | |
| CN102249923A (en) | Method for refining tris(2-ethylhexyl)trimellitate and refining agent used thereby | |
| CN106518679A (en) | Method for preparing di-n-butyl adipate | |
| CN101891611B (en) | Method for preparing dipropyl adipate | |
| CN101906035A (en) | Refining method of high-purity butyl stearate | |
| CN102911049A (en) | Method for preparing dinonyl adipate by utilizing refining agent | |
| CN102911051A (en) | Refining method of dinonyl adipate | |
| CN102942481A (en) | Preparation method of dinonyl adipate | |
| CN102249925A (en) | Method for refining trioctyl trimellitate and refining agent for same | |
| CN102249924A (en) | Method for refining tri-n-hexyl trimellitate and refining agent used in method | |
| CN102911050A (en) | Preparation method of diisobutyl adipate | |
| CN102267909A (en) | Method for refining tris(2-ethylhexyl) trimellitate and refining agent used in same | |
| CN102320965A (en) | The method of the own benzyl ester of a kind of refining hexanodioic acid 2-ethyl and used finishing agent thereof | |
| CN101928218A (en) | Preparation method of adipic acid-di-n-propyl ester | |
| CN102249912A (en) | Refining agent for synthesizing dioctyl sebacate and preparation method for dioctyl sebacate | |
| CN102267908B (en) | Method for refining trioctyl trimellitate and refining agent used thereby | |
| CN102320964A (en) | Method for refining adipate2-benzyl ethylhexyl and used refining agent thereof | |
| CN102320972B (en) | Method for refining trioctyl trimellate and refining agent used in refining | |
| CN101914019A (en) | Refining method of di-n-butyl sebacic acid | |
| CN102911047A (en) | Diisooctyl adipate preparation method | |
| CN102936200A (en) | Method for refining diisobutyl adipate | |
| CN102911048A (en) | Preparation method of diisobutyl adipate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130206 |