CN106518668A - Trimellitate tri C8-C10 refinement method - Google Patents
Trimellitate tri C8-C10 refinement method Download PDFInfo
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- CN106518668A CN106518668A CN201510579875.6A CN201510579875A CN106518668A CN 106518668 A CN106518668 A CN 106518668A CN 201510579875 A CN201510579875 A CN 201510579875A CN 106518668 A CN106518668 A CN 106518668A
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- Prior art keywords
- water
- ester
- stirring
- tri trimellitate
- dealcoholysis
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a trimellitate tri C8-C10 refinement method, which comprises: (1) an esterification reaction step, wherein trimellitic acid, C8-C10 alcohol and concentrated sulfuric acid are poured into a reaction kettle, stirring is performed, heating is performed until a boiling state is achieved, a reaction is performed, the boiling reflux state is maintained, and the water is separated; (2) a water washing step, wherein water is added to the mixture obtained after the esterification reaction, uniform stirring is performed, standing layering is performed, and the water layer is removed; (3) an alcohol removing step; (4) a refining step; and (5) a filtering step. According to the present invention, the refining agent used by the preparation method is the mixture of calcium hydroxide, magnesium hydroxide, active carbon and magnesium sulfate, such that the characteristics of low cost and easy purchasing are provided.
Description
Technical field
The invention belongs to field of organic compound preparation, especially a kind of tri trimellitate
C8-C10 esters are easy, effective process for purification.
Background technology
In industrial production, plastics industry and war production, tri trimellitate C8-C10Ester as
A kind of important organic compounds and heat-resisting, high temperature plasticizer, it is more next with good electrical property
More it is widely applied.Tri trimellitate C8-C10The usual production method of ester is that direct esterification is anti-
Should, the color for obtaining product is yellow, is difficult to sell as product, it is necessary to carry out further essence
System, that is, carry out the refinement treatment step that reduces pressure, the problem that such preparation method is present：1, due to
Need to realize using expensive high-vacuum pump in decompression refinement treatment step, therefore,
The method has that production equipment is more, costly, thus is difficult to reduces cost.2, by
In decompression refinement treatment step be production tri trimellitate C8-C10During ester it is essential and
Very time-consuming production stage, therefore, there is production time length, low production efficiency in the method
Problem, is unfavorable for the raising of Business Economic Benefit.
The content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, inclined benzene three is refined using refining agent
Three C of acid8-C10Ester, there is provided one kind can save equipment investment, reduces cost, shorten production
Time is simultaneously capable of the tri trimellitate C of improve production efficiency8-C10Ester preparation method.
It is to employ the following technical solutions realization that the present invention solves its technical problem：
A kind of tri trimellitate C8-C10The process for purification of ester, the method are comprised the following steps：
(1) step of esterification
By trimellitic acid, C8-C10Alcohol, the concentrated sulfuric acid, in input reactor, stirring is heated to
Boiling reaction, keeps boiling reflux state to separate moisture therein.
(2) water-washing step
Water will be added in mixture after esterification, after stirring, stratification is removed
Water layer therein.
(3) dealcoholysis step
By the mixture after washing, dealcoholysis, crude product, tri trimellitate C is obtained8-C10Ester.
(4) purification step
Refining agent will be added in crude product after dealcoholysis, and stirring is refined one hour.
(5) filtration step
Mixed liquor after will be refined is filtered, and obtains tri trimellitate C8-C10Ester product.
The present invention can also adopt following technical scheme：
Described refining agent be calcium hydroxide, magnesium hydroxide, activated carbon, magnesium sulfate weight ratio,
By 1：1：2：1.5 mix.
The weight ratio of described refining agent and trimellitic acid is 0.05 0.1：1
Described trimellitic acid, C8-C10Alcohol, the weight ratio of the concentrated sulfuric acid is 1：2.56：
0.002—0.005
Described water is 0.8 with the weight ratio of trimellitic acid：1.
Advantages of the present invention and good effect are：
1st, this tri trimellitate C8-C10The preparation method of ester in purification step, using refined
Agent (calcium hydroxide, magnesium hydroxide, activated carbon, sulfuric acid magnesium compound), the product face for obtaining
Discoloration is shallow, it is not necessary to which high vacuum refinement treatment can be used as product sale, prepared product matter
Amount complies fully with technical requirement.This preparation method eliminates the refined step of high vacuum in production
Suddenly, it is to avoid the input of high-vacuum pump equipment, therefore, saved equipment investment, reduced production
Cost, improves the competitiveness of product in market.
2nd, this tri trimellitate C8-C10The refining agent that the preparation method of ester is used be calcium hydroxide,
Magnesium hydroxide, activated carbon, sulfuric acid magnesium compound, with cheap, it is easy to the characteristics of purchasing.
3rd, this tri trimellitate C8-C10The preparation method of ester have it is easy to operate, it is simple
Facilitate implementation industrialized production, improve production efficiency.
4th, the present invention in process of production, using refining agent (calcium hydroxide, magnesium hydroxide,
Activated carbon, sulfuric acid magnesium compound), it is ensured that product quality and long term storage stability, while this
Invention is simple with realizing, the characteristics of easy to operate, has saved the investment of production equipment, improves
Production efficiency.
Specific embodiment
Below by specific embodiment, the present invention is further described：
Embodiment 1
This tri trimellitate C8-C10The process for purification of ester is comprised the following steps：
1. step of esterification
Heater, electricity stirring, thermometer water circulation condenser and water-oil separating are carried to one
Trimellitic acid double centner, C is put into successively in 500 liters of reactors of device8-C10256 kilograms of alcohol,
0.3 kilogram of the concentrated sulfuric acid, under agitation, micro-vacuum, while being heated to boiling reaction, keeps boiling
Reflux state is risen, is constantly separated water into away from oil water separator, until no moisture is generated
Afterwards, stop heating, esterification terminates.
2. water-washing step
Obtain adding 250 kilograms of water in mixed liquor to after esterification, it is after stirring, quiet
Layering is put, water layer therein is removed.
3. dealcoholysis step
By the mixture after washing, dealcoholysis, crude product, tri trimellitate C is obtained8-C10Ester.
4. purification step
To in the crude product after dealcoholysis add refining agent (calcium hydroxide, magnesium hydroxide, activated carbon,
Sulfuric acid magnesium compound) 0.5 kilogram, stirring mixing 1 hour.
5. filtration step
Refined mixed liquor is filtered or press filtration, the liquid for obtaining is tri trimellitate C8-C10
Ester finished product, tri trimellitate C8-C10Ester content 99.0%, color are less than No. 2 (iodine colorimetric).
Embodiment 2
This tri trimellitate C8-C10The process for purification of ester is comprised the following steps：
1. step of esterification
Heater, electricity stirring, thermometer water circulation condenser and water-oil separating are carried to one
Trimellitic acid double centner, C is put into successively in 500 liters of reactors of device8-C10256 kilograms of alcohol,
0.3 kilogram of the concentrated sulfuric acid, under agitation, micro-vacuum, while being heated to boiling reaction, keeps boiling
Reflux state is risen, is constantly separated water into away from oil water separator, until no moisture is generated
Afterwards, stop heating, esterification terminates.
2. water-washing step
Obtain adding 250 kilograms of water in mixed liquor to after esterification, it is after stirring, quiet
Layering is put, water layer therein is removed.
3. dealcoholysis step
By the mixture after washing, dealcoholysis, crude product, tri trimellitate C is obtained8-C10Ester.
4. purification step
To in the crude product after dealcoholysis add refining agent (calcium hydroxide, magnesium hydroxide, activated carbon,
Sulfuric acid magnesium compound) 0.6 kilogram, stirring mixing 1 hour.
5. filtration step
Refined mixed liquor is filtered or press filtration, the liquid for obtaining is tri trimellitate C8-C10
Ester finished product, tri trimellitate C8-C10Ester content 99.0%, color are less than No. 2 (iodine colorimetric).
Embodiment 3
The process for purification of this tri trimellitate C8-C10 esters is comprised the following steps：
1. step of esterification
Heater, electricity stirring, thermometer water circulation condenser and water-oil separating are carried to one
Trimellitic acid double centner, C is put into successively in 500 liters of reactors of device8-C10`256 kilogram of alcohol,
0.3 kilogram of the concentrated sulfuric acid, under agitation, micro-vacuum, while being heated to boiling reaction, keeps boiling
Reflux state is risen, is constantly separated water into away from oil water separator, until no moisture is generated
Afterwards, stop heating, esterification terminates.
2. water-washing step
Obtain adding 250 kilograms of water in mixed liquor to after esterification, it is after stirring, quiet
Layering is put, water layer therein is removed.
3. dealcoholysis step
By the mixture after washing, dealcoholysis, crude product, tri trimellitate C is obtained8-C10Ester.
4. purification step
To in the crude product after dealcoholysis add refining agent (calcium hydroxide, magnesium hydroxide, activated carbon,
Sulfuric acid magnesium compound) 0.7 kilogram, stirring mixing 1 hour.
5. filtration step
Refined mixed liquor is filtered, the liquid for obtaining is tri trimellitate C8-C10Ester into
Product, tri trimellitate C8-C10Ester content 99.0%, color are less than No. 2 (iodine colorimetric).
It is emphasized that example of the present invention is illustrative, rather than it is determinate,
Therefore the present invention is not limited to the embodiment described in specific embodiment, every by this area skill
The other embodiment that art personnel's technology according to the present invention scheme draws, also belongs to the present invention
The scope of protection.
Claims (1)
1. a kind of tri trimellitate C8-C10The process for purification of ester, it is characterised in that：The method
Comprise the following steps：
(1) step of esterification
By trimellitic acid, C8-C10Alcohol, the concentrated sulfuric acid, in input reactor, stirring is heated to
Boiling reaction, keeps boiling reflux state to separate moisture therein；
(2) water-washing step
Water will be added in mixture after esterification, after stirring, stratification is removed
Water layer therein；
(3) dealcoholysis step
By the mixture after washing, dealcoholysis, crude product, tri trimellitate C is obtained8-C10Ester；
(4) purification step
Refining agent will be added in crude product after dealcoholysis, and stirring is refined one hour；
(5) filtration step
Mixed liquor after will be refined is filtered, and obtains tri trimellitate C8-C10Ester product；
The present invention can also adopt following technical scheme：
Described refining agent be calcium hydroxide, magnesium hydroxide, activated carbon, magnesium sulfate weight ratio,
By 1：1：2：1.5 mix；
The weight ratio of described refining agent and trimellitic acid is 0.05 0.1：1；
Described trimellitic acid：C8-C10Alcohol：The weight ratio of the concentrated sulfuric acid is 1：2.56：
0.002—0.005；
Described water is 0.8 with the weight ratio of trimellitic acid：1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510579875.6A CN106518668A (en) | 2015-09-11 | 2015-09-11 | Trimellitate tri C8-C10 refinement method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510579875.6A CN106518668A (en) | 2015-09-11 | 2015-09-11 | Trimellitate tri C8-C10 refinement method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106518668A true CN106518668A (en) | 2017-03-22 |
Family
ID=58348110
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510579875.6A Pending CN106518668A (en) | 2015-09-11 | 2015-09-11 | Trimellitate tri C8-C10 refinement method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106518668A (en) |
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2015
- 2015-09-11 CN CN201510579875.6A patent/CN106518668A/en active Pending
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| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170322 |
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| WD01 | Invention patent application deemed withdrawn after publication |