CN102557884A - Preparation method of thymol - Google Patents
Preparation method of thymol Download PDFInfo
- Publication number
- CN102557884A CN102557884A CN201210011824XA CN201210011824A CN102557884A CN 102557884 A CN102557884 A CN 102557884A CN 201210011824X A CN201210011824X A CN 201210011824XA CN 201210011824 A CN201210011824 A CN 201210011824A CN 102557884 A CN102557884 A CN 102557884A
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- CN
- China
- Prior art keywords
- thymol
- propylene
- preparation
- reaction
- conducting
- 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.)
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- MGSRCZKZVOBKFT-UHFFFAOYSA-N thymol Chemical compound CC(C)C1=CC=C(C)C=C1O MGSRCZKZVOBKFT-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 239000005844 Thymol Substances 0.000 title claims abstract description 27
- 229960000790 thymol Drugs 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims abstract description 15
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims abstract description 15
- RLSSMJSEOOYNOY-UHFFFAOYSA-N m-cresol Chemical compound CC1=CC=CC(O)=C1 RLSSMJSEOOYNOY-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229940100630 metacresol Drugs 0.000 claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 10
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 7
- 238000009834 vaporization Methods 0.000 claims abstract description 6
- 230000008016 vaporization Effects 0.000 claims abstract description 6
- 238000005516 engineering process Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 239000002808 molecular sieve Substances 0.000 claims abstract description 5
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 5
- 150000001896 cresols Chemical class 0.000 claims description 5
- 239000002994 raw material Substances 0.000 abstract description 8
- 239000000047 product Substances 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 3
- 238000000034 method Methods 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract 2
- 238000000926 separation method Methods 0.000 abstract 1
- 230000000295 complement effect Effects 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 206010020852 Hypertonia Diseases 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a preparation method of thymol, which adopts the shape selective catalysis technology, selects a ZSM-5 molecular sieve based catalyst and obtains the thymol through alkylate reaction of metacresol and propylene. The method includes the following steps: conducting preheating and vaporization on the raw material metacresol and the propylene, introducing the material metacresol and the propylene into a fixed bed reactor, conducting heating on the mixture, conducting catalytic reaction on the mixture through the ZSM-5 molecular sieve based catalyst, introducing a reaction product into a separator for separation, conducting vacuum rectification on the reaction product and conducting slice cutting to obtain the thymol with high purity. The preparation method of the thymol is high in target product selectivity and low in material consumption and energy consumption.
Description
Technical field
The invention belongs to the chemical production field, especially a kind of preparation method of thymol.
Background technology
Thymol not only can be used as spices, because it has preservative property, can also be as Medicines, and well received.In the prior art, thymol generally adopts chemical method to obtain, as making through meta-cresol liquid phase propylated reaction on activated alumina; But temperature of reaction that this method is required and hypertonia, side reaction is violent, and catalyst deactivation is fast; Target product selectivity is low, and economy is relatively poor.
Summary of the invention
The objective of the invention is to overcome the weak point of prior art, provide a kind of target product selectivity high, reduce the preparation method of material consumption energy consumption.
A kind of preparation method of thymol, it adopts the shape selective catalysis technology, selects the ZSM-5 sieve catalyst for use; Alkylated reaction through meta-cresol and propylene is produced thymol, and its step is following: stock yard cresols and propylene feed fixed-bed reactor after the preheating vaporization; Heating, through ZSM-5 sieve catalyst catalyzed reaction, reaction product feeds separator separates; Rectification under vacuum promptly obtains the high purity thymol after the section.When making catalyzer with molecular sieve, reaction is mainly carried out at intracrystalline, and has only those sizes and shape and molecular sieve pore passage to be complementary, and the molecule that can spread access way just can become reactant and product, and the shape selective catalysis technology has improved the selectivity of title product.
As of the present invention preferred, the mol ratio of said propylene and meta-cresol is 0.7 ~ 0.8, and it is best that the transformation efficiency of proportioning raw materials meta-cresol between this and gained thymol selectivity reach.
As of the present invention preferred, Heating temperature is 250 ~ 300 ℃, and temperature of reaction is between this, and it is best that the transformation efficiency of meta-cresol and gained thymol selectivity reach.
The present invention compared with prior art; Have significantly outstanding advantage and beneficial effect: choose the ZSM-5 sieve catalyst; Its duct size is complementary with thymol molecular diameter size; Its intracrystalline structure provides enough movability for the thymol molecule, but has hindered the carrying out of by product effectively, has increased the title product amount.
Embodiment
Below in conjunction with embodiment the present invention is done further explain.
This specific embodiment only is to explanation of the present invention; It is not a limitation of the present invention; Those skilled in the art can make the modification that does not have creative contribution to present embodiment as required after reading this specification sheets, but as long as in claim scope of the present invention, all receive the protection of patent law.
Embodiment 1
Choose propylene and meta-cresol mol ratio and be 0.75 raw material, stock yard cresols and propylene feed fixed-bed reactor after the preheating vaporization; Be heated to 275 ℃; Raw material is through ZSM-5 sieve catalyst catalysis generation alkylated reaction, and reaction product feeds separator separates, rectification under vacuum; Promptly obtain the high purity thymol after the section, the selectivity of gained thymol reaches 94.3%.
Embodiment 2
Choose propylene and meta-cresol mol ratio and be 0.7 raw material, stock yard cresols and propylene feed fixed-bed reactor after the preheating vaporization; Be heated to 275 ℃; Raw material is through ZSM-5 sieve catalyst catalysis generation alkylated reaction, and reaction product feeds separator separates, rectification under vacuum; Promptly obtain the high purity thymol after the section, the selectivity of gained thymol reaches 94.8%.
Embodiment 3
Choose propylene and meta-cresol mol ratio and be 0.8 raw material, stock yard cresols and propylene feed fixed-bed reactor after the preheating vaporization; Be heated to 250 ℃; Raw material is through ZSM-5 sieve catalyst catalysis generation alkylated reaction, and reaction product feeds separator separates, rectification under vacuum; Promptly obtain the high purity thymol after the section, the selectivity of gained thymol reaches 94.6%.
Claims (3)
1. the preparation method of a thymol is characterized in that: its adopts shape selective catalysis technology, selects for use the ZSM-5 molecular sieve as catalyzer; Alkylated reaction through meta-cresol and propylene is produced thymol, and its step is following: stock yard cresols and propylene feed fixed-bed reactor after the preheating vaporization; Heating, through ZSM-5 sieve catalyst catalyzed reaction, reaction product feeds separator separates; Rectification under vacuum promptly obtains the high purity thymol after the section.
2. the preparation method of a kind of thymol according to claim 1, it is characterized in that: the mol ratio of said propylene and meta-cresol is 0.7 ~ 0.8.
3. the preparation method of a kind of thymol according to claim 1, it is characterized in that: said Heating temperature is 250 ~ 300 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210011824XA CN102557884A (en) | 2012-01-16 | 2012-01-16 | Preparation method of thymol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210011824XA CN102557884A (en) | 2012-01-16 | 2012-01-16 | Preparation method of thymol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102557884A true CN102557884A (en) | 2012-07-11 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210011824XA Pending CN102557884A (en) | 2012-01-16 | 2012-01-16 | Preparation method of thymol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102557884A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103951546A (en) * | 2014-05-13 | 2014-07-30 | 宿迁科思化学有限公司 | Novel synthetic process of thymol |
-
2012
- 2012-01-16 CN CN201210011824XA patent/CN102557884A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103951546A (en) * | 2014-05-13 | 2014-07-30 | 宿迁科思化学有限公司 | Novel synthetic process of thymol |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C05 | Deemed withdrawal (patent law before 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120711 |