CN109879738A - A kind of refining methd of terephthalaldehyde - Google Patents
A kind of refining methd of terephthalaldehyde Download PDFInfo
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- CN109879738A CN109879738A CN201711277429.5A CN201711277429A CN109879738A CN 109879738 A CN109879738 A CN 109879738A CN 201711277429 A CN201711277429 A CN 201711277429A CN 109879738 A CN109879738 A CN 109879738A
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- terephthalaldehyde
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- refining methd
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Abstract
The invention discloses a kind of refining methds of terephthalaldehyde, and terephthalaldehyde crude product is evaporated under vacuum conditions, after removing impurity, obtain terephthalaldehyde highly finished product by distillation.The present invention does not use any solvent, technical process is environmentally friendly, the impurity such as p-tolyl aldehyde are removed by being evaporated in vacuo, then purification terephthalaldehyde product is obtained by sublimation process, have the characteristics that product purity height and high income, product purity reaches 99% or more, and yield reaches 95% or more.
Description
Technical field
The invention belongs to organic chemistry filed, in particular to a kind of refining methd of terephthalaldehyde, specifically, being related to
A method of by terephthalaldehyde crude product refining at polymer grade terephthalaldehyde.
Background technique
Terephthalaldehyde is the important intermediate of organic synthesis and Polymer Synthesizing, since there are two active aldehyde, institutes for it
With it can autohemagglutination and being copolymerized with other unit to form the compounds of various performances, terephthalaldehyde is mainly used for plastics, perfume (or spice)
The industry such as material, medicine, dyestuff, fluorescent whitening agent, are the important source materials of fine chemistry industry, and there are many route of synthesis of terephthalaldehyde,
P-xylene oxidation Hydrolyze method, paraxylene gas phase air oxidation etc., due to the complexity of reaction, resulting terephthalaldehyde is thick
Impurity content is more in product, needs further to be refined into polymer grade terephthalaldehyde, uses for downstream.
United States Patent (USP) 2888488 discloses a kind of method for preparing terephthalaldehyde, wherein by solvent extraction, drying and
It distils and refined product.However this method needs complicated technique, and uses to the disagreeableness compound chloroform of environment as molten
Agent.
Japan Patent 2001-199910 discloses a kind of by the cooling method for recrystallizing aromatic aldehyde.But this method exists
It obtains and is also restricted on high-purity terephthalaldehyde
Chinese patent CN200580028008.8 disclose one kind using alcohol as solvent, using water be anti-solvent by recrystallize by
The method that terephthalaldehyde crystals containing impurity prepare high-purity terephthalaldehyde, but terephthalaldehyde yield is lower, highest
It is only capable of reaching 79.2%.
Chinese patent CN200780024375.X discloses one kind using dimethyl sulfoxide as solvent, passes through weight by anti-solvent of water
Crystallization by containing impurity terephthalaldehyde crystals prepare high-purity terephthalaldehyde method, but terephthalaldehyde yield compared with
Low, highest is only capable of reaching 87%.
Chinese patent CN200780041280.9 disclose it is a kind of crude product terephthalaldehyde is dissolved in paraxylene, use
Dimethyl sulfoxide etc. is cosolvent, and then by the method for recrystallization preparation high-purity terephthalaldehyde, but it obtains 99% or more
When pure terephthalaldehyde, yield is lower, and highest is only capable of reaching 78.7%.
Goal of the invention
The present invention situation relatively low for terephthalaldehyde purification yield, provides a kind of new refining methd, is obtaining
Purification yield is improved on the basis of the above terephthalaldehyde of 99% purity, and purification yield is made to reach 95% or more.This method technique letter
It is single, any solvent is not used compared with prior art, and technical process is environmentally friendly.
It to achieve the goals above, will be right the invention adopts the following technical scheme: a kind of refining methd of terephthalaldehyde
Phthalaldehyde crude product evaporates under vacuum conditions, after removing impurity, obtains terephthalaldehyde highly finished product by distillation.
Further, vacuum condition is pressure in -90KPa~-30KPa.
It is preferred that vacuum condition is pressure in -70KPa~-30KPa.
Further, being evaporated in vacuo temperature is 20~50 DEG C.
It is preferred that being evaporated in vacuo temperature is 30~50 DEG C.
Further, the temperature of distillation is 80~120 DEG C.
The terephthalaldehyde crude product comprising impurity used is not specifically limited, and including being prepared by known methods
Terephthalaldehyde or commercially available terephthalaldehyde.
Including evaporating terephthalaldehyde crude product under vacuum conditions, is then using the side of sublimation purifying terephthalaldehyde
In method, the present invention does not use any solvent, obtains purification terephthalaldehyde only with the method for evaporation and distillation.Terephthalaldehyde
Contain p-tolyl aldehyde, benzaldehyde, 4- carboxyl benzaldehyde, 4- hydroxy benzaldehyde, terephthalic acid (TPA), benzoic acid, hydrogen in crude product
The impurity such as quinone, wherein p-tolyl aldehyde and benzaldehyde are liquid at room temperature, and terephthalaldehyde and other impurities are at room temperature
For solid-state, therefore the method by being evaporated under vacuum condition, the p-tolyl aldehyde of liquid and benzaldehyde are removed, then passed through
The method of distillation obtains purification terephthalaldehyde.
Compared with the prior art, the advantages of the present invention are as follows any solvent is not used, technical process is environmentally friendly, passes through
It is evaporated in vacuo and removes the impurity such as p-tolyl aldehyde, purification terephthalaldehyde product is then obtained by sublimation process, is had
The characteristics of product purity height and high income, product purity reach 99% or more, and yield reaches 95% or more.
Specific embodiment
Detailed description of the preferred embodiments below, it should be noted however that protection of the invention
Range is not limited to these specific embodiments, but is determined by claims.
Terephthalaldehyde crude product purity and purification terephthalaldehyde product purity all pass through gas chromatography-mass spectrum in embodiment
Analytic approach measures.In embodiment, the purity of terephthalaldehyde crude product used is 97.1%.
Embodiment 1
10g terephthalaldehyde crude product is placed in evaporator, is evaporated under the conditions of -70KPa, 40 DEG C, then will be steamed
Material is heated to 110 DEG C after hair, and terephthalaldehyde distils to obtain purification terephthalaldehyde product.It is total to refine terephthalaldehyde product
Yield is 98.6%, purity 99.5%.
Embodiment 2
10g terephthalaldehyde crude product is placed in evaporator, is evaporated under the conditions of -90KPa, 20 DEG C, then will be steamed
Material is heated to 120 DEG C after hair, and terephthalaldehyde distils to obtain purification terephthalaldehyde product.It is total to refine terephthalaldehyde product
Yield is 98.8%, purity 99.3%.
Embodiment 3
10g terephthalaldehyde crude product is placed in evaporator, is evaporated under the conditions of -30KPa, 50 DEG C, then will be steamed
Material is heated to 80 DEG C after hair, and terephthalaldehyde distils to obtain purification terephthalaldehyde product.It is total to refine terephthalaldehyde product
Yield is 98.3%, purity 99.4%.
Embodiment 4
10g terephthalaldehyde crude product is placed in evaporator, is evaporated under the conditions of -50KPa, 30 DEG C, then will be steamed
Material is heated to 110 DEG C after hair, and terephthalaldehyde distils to obtain purification terephthalaldehyde product.It is total to refine terephthalaldehyde product
Yield is 98.6%, purity 99.5%.
Although a specific embodiment of the invention is described in detail above in conjunction with the embodiments, need to refer to
Out, the scope of protection of the present invention is not limited by these specific embodiments, but is determined by claims.This
Field technical staff can carry out these embodiments in the range of not departing from technical idea and purport of the invention appropriate
Change, and the embodiment after these changes is obviously also included within protection scope of the present invention.
Claims (6)
1. a kind of refining methd of terephthalaldehyde, it is characterised in that: evaporate terephthalaldehyde crude product under vacuum conditions, go
After impurity, terephthalaldehyde highly finished product are obtained by distillation.
2. refining methd according to claim 1, it is characterised in that: the vacuum condition be pressure -90KPa~-
30KPa。
3. refining methd according to claim 1, it is characterised in that: the vacuum condition be pressure -70KPa~-
30KPa。
4. refining methd according to claim 1, it is characterised in that: the vacuum evaporation temperature is 20~50 DEG C.
5. refining methd according to claim 1, it is characterised in that: the vacuum evaporation temperature is 30~50 DEG C.
6. refining methd according to claim 1, it is characterised in that: the temperature of the distillation is 80~120 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711277429.5A CN109879738A (en) | 2017-12-06 | 2017-12-06 | A kind of refining methd of terephthalaldehyde |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711277429.5A CN109879738A (en) | 2017-12-06 | 2017-12-06 | A kind of refining methd of terephthalaldehyde |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109879738A true CN109879738A (en) | 2019-06-14 |
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ID=66923845
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711277429.5A Pending CN109879738A (en) | 2017-12-06 | 2017-12-06 | A kind of refining methd of terephthalaldehyde |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109879738A (en) |
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2017
- 2017-12-06 CN CN201711277429.5A patent/CN109879738A/en active Pending
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| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20190614 |