CN1974516A - Process of producing 3,5-xylenol - Google Patents
Process of producing 3,5-xylenol Download PDFInfo
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- CN1974516A CN1974516A CN 200610134601 CN200610134601A CN1974516A CN 1974516 A CN1974516 A CN 1974516A CN 200610134601 CN200610134601 CN 200610134601 CN 200610134601 A CN200610134601 A CN 200610134601A CN 1974516 A CN1974516 A CN 1974516A
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Abstract
The present invention relates to coal chemical technology, and is especially process of producing 3, 5-xylenol. The materials including industrial xylenol and after fraction and has 3, 5-xylenol content greater than 40 %. Through once intermittent rectifying process in a rectifying tower with theoretical plate number of 50-80, 3, 5-xylenol product with content over 95 % is obtained. In the same time, 3, 4-xylenol product with content over 95 % may be also obtained through crystallization, washing and suction filtering.
Description
Technical field the present invention relates to technical field of coal chemical industry, is a kind of 3, the production method of 5-xylenol.
Background technology
In the prior art, 3, the 5-xylenol does not have suitability for industrialized production, and the method for testing laboratory has following several:
Complexometry: principle is for utilizing metal halogen and 3, and 4-xylenol and 3,5-xylenol have the character of selecting complexing and it is separated from phenol mixture, and this method is because need complexing-decomplexing reaction, and technological process is long, the production cost height.
Adsorption method of separation: use zeolite as adsorption separating agent, desorbing agent adopts alkyl alcohol, this isolation technique is by absorption, concentrate, the several elementary operations of recovery of desorption and desorbing agent circulate continuously realizes, but this method product yield is low, the adsorbent reactivation difficulty.
Azeotropic distillation: 3, add 1.8～2.5 times tar bases in the 5-xylenol raw material, azeotropic distillation under reduced pressure, this method needs entrainer, and energy consumption is big.
The fusion-crystallization method: according to the solid-liquid equilibrium relation, adopt two sections crystallization processs to separate, this kind method Crystallization Separation equipment requirements is higher, and investment is big.
Through the domestic literature retrieval, find and two pieces of this project pertinent literatures:
Document 1: " from dimethylphenol, extracting 3,5-xylenol experimental study ", periodical name: Sichuan metallurgy, 2002.024 (002) .-49-50,55;
Document 2: " from technical xylenol, separating 3, the research of 5-xylenol ", periodical name: fuel and chemical industry, 2002.033 (002) .-89-92.
By rectifying, crystallization produces 3 to document one report, the method for 5-xylenol from dimethylphenol.The method that document two report adopts atmospheric distillations and solvent recrystallization to combine separates 3 from technical xylenol, the 5-xylenol, can obtain after the rectifying purity greater than 90% 3,5-xylenol narrow fraction can obtain purity greater than 99% product through recrystallization again.
Result for retrieval is with to look into the contrast of new point as follows: innovative point one is described, is raw material with technical xylenol and after cut (contain 3, the 5-xylenol is greater than 40%), and a rectifying obtains 3,5-xylenol (content is greater than 95%); The finished product mentioned in pertinent literature one, two are identical with this authorized item, but raw materials used different with this authorized item with technology.Innovative point two is described, is producing 3, in the time of the 5-xylenol, can also obtain content greater than 70% 3, the 4-xylenol can obtain 3 through Crystallization Separation, 4-xylenol (content is greater than 95%).In pertinent literature, do not appear in the newspapers.
Conclusion is as follows: the method that adopts atmospheric distillation and solvent recrystallization to combine, from technical xylenol, separate 3, the 5-xylenol, existing bibliographical information, this client is a raw material with technical xylenol and after cut (contain 3, the 5-xylenol is greater than 40%), a rectifying obtains 3,5-xylenol (content is greater than 95%), and producing 3, in the time of the 5-xylenol, can also obtain content greater than 70% 3,4-xylenol cut can obtain 3 through Crystallization Separation, 4-xylenol (content is greater than 95%).
Summary of the invention
The purpose of this invention is to provide a kind of 3, the production method of 5-xylenol, this method is a raw material with technical xylenol and after cut, the method that adopts batch fractionating is through a rectifying of rectifying tower, obtain 3,5-xylenol content greater than 95% 3,5-xylenol product is in rectifying separation 3, in the time of the 5-xylenol, also can obtain 3 through crystallization, washing, suction filtration, 4-xylenol content greater than 95% 3,4-xylenol product.
For achieving the above object, the present invention is achieved through the following technical solutions:
A kind of 3, the production method of 5-xylenol is characterized in that: this method is a raw material with manufacture xylenol and after cut, and in the raw material 3,5-xylenol content is greater than 40%; Adopt method rectifying in rectifying tower of batch fractionating, the rectifying tower number of theoretical plate is 50～80; Obtain content greater than 95% 3,5-xylenol product.
Rectifying still still temperature is at 250 ℃～300 ℃, still pressure maintenance 0.005～0.020Mpa.
The rectifying tower top temperature is at 200 ℃～230 ℃.
Reflux ratio is 10～30.
In rectifying separation 3, in the time of the 5-xylenol, also can obtain 3 through crystallization, washing, suction filtration, 4-xylenol content greater than 95% 3,4-xylenol product.
The invention has the beneficial effects as follows: with technical xylenol and after cut is raw material, and the method that adopts batch fractionating obtains 3 through a rectifying of rectifying tower, 5-xylenol content greater than 95% 3,5-xylenol product; In rectifying separation 3, in the time of the 5-xylenol, also can obtain 3 through crystallization, washing, suction filtration, 4-xylenol content greater than 95% 3,4-xylenol product.
Embodiment
A kind of 3, the production method of 5-xylenol, this method is a raw material with manufacture xylenol and after cut, in the raw material 3,5-xylenol content is greater than 40%, and the method that adopts batch fractionating is produced in number of theoretical plate is 50～80 rectifying tower, obtain content greater than 95% 3,5-xylenol product; Its production process is: raw material is packed in the rectifying still into heating then, rectifying in rectifying tower; Rectifying still still temperature is pressed at 250 ℃～300 ℃, still and is kept 0.005～0.020Mpa, and the rectifying tower top temperature is at 200 ℃～230 ℃, in reflux ratio is to cut fraction respectively under 10～30 the condition; Priority recovered water, foreshot, industrial cresols, 3,5-xylenol content greater than 40% 3,5-xylenol fraction, 3,5-xylenol content greater than 95% 3,5-xylenol product, 3,4-xylenol content greater than 70% 3,4-xylenol fraction, stop extraction then, extract the still raffinate when treating still temperature drop to 100 ℃ out; 3,4-xylenol content greater than 70% 3,4-xylenol cut is through crystallization, Tc is 20 ℃～30 ℃, washs with ethanol or cyclohexane solvent, 3, the volume ratio of 4-xylenol cut and solvent is 1: 1～3, centrifugally obtain 3, and 4-xylenol content is greater than 95% product.
Claims (5)
1, a kind of 3, the production method of 5-xylenol is characterized in that: this method is a raw material with manufacture xylenol and after cut, and in the raw material 3,5-xylenol content is greater than 40%; Adopt method rectifying in rectifying tower of batch fractionating, the rectifying tower number of theoretical plate is 50～80; Obtain content greater than 95% 3,5-xylenol product.
2, according to claim 1 a kind of 3, the production method of 5-xylenol is characterized in that: rectifying still still temperature is pressed and is kept 0.005～0.020Mpa at 250 ℃～300 ℃, still.
3, according to claim 1 a kind of 3, the production method of 5-xylenol is characterized in that: the rectifying tower top temperature is at 200 ℃～230 ℃.
4, according to claim 1 a kind of 3, the production method of 5-xylenol is characterized in that: reflux ratio is 10～30.
5, according to claim 1,2,3 or 4 described a kind of 3, the production method of 5-xylenol is characterized in that: in rectifying separation 3, in the time of the 5-xylenol, also can obtain 3 through crystallization, washing, suction filtration, 4-xylenol content greater than 95% 3,4-xylenol product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610134601 CN1974516A (en) | 2006-12-08 | 2006-12-08 | Process of producing 3,5-xylenol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610134601 CN1974516A (en) | 2006-12-08 | 2006-12-08 | Process of producing 3,5-xylenol |
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| Publication Number | Publication Date |
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| CN1974516A true CN1974516A (en) | 2007-06-06 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 200610134601 Pending CN1974516A (en) | 2006-12-08 | 2006-12-08 | Process of producing 3,5-xylenol |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108689806A (en) * | 2018-05-06 | 2018-10-23 | 陕西巴斯腾科技有限公司 | A kind of method of cresols product rectifying still raffinate recycling cresols |
| CN109251130A (en) * | 2017-07-13 | 2019-01-22 | 鞍钢股份有限公司 | A kind of technique of organic heat carrier heating technique normal pressure production 3,5- xylenol |
| CN109251131A (en) * | 2017-07-13 | 2019-01-22 | 鞍钢股份有限公司 | A kind of technique of organic heat carrier heating technique decompression production 3,5- xylenol |
-
2006
- 2006-12-08 CN CN 200610134601 patent/CN1974516A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109251130A (en) * | 2017-07-13 | 2019-01-22 | 鞍钢股份有限公司 | A kind of technique of organic heat carrier heating technique normal pressure production 3,5- xylenol |
| CN109251131A (en) * | 2017-07-13 | 2019-01-22 | 鞍钢股份有限公司 | A kind of technique of organic heat carrier heating technique decompression production 3,5- xylenol |
| CN108689806A (en) * | 2018-05-06 | 2018-10-23 | 陕西巴斯腾科技有限公司 | A kind of method of cresols product rectifying still raffinate recycling cresols |
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