CN1140487C - Synthetic process for 2,3,5-trimethylphenol - Google Patents
Synthetic process for 2,3,5-trimethylphenol Download PDFInfo
- Publication number
- CN1140487C CN1140487C CNB011150068A CN01115006A CN1140487C CN 1140487 C CN1140487 C CN 1140487C CN B011150068 A CNB011150068 A CN B011150068A CN 01115006 A CN01115006 A CN 01115006A CN 1140487 C CN1140487 C CN 1140487C
- Authority
- CN
- China
- Prior art keywords
- steam
- adopt
- tower
- rectifying
- jacket pipe
- 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.)
- Expired - Fee Related
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a synthesis technology for 2, 3, 5-trimethylphenol. The method comprises the procedures of batching, preheating, vaporization, overheating, reaction and continuous rectification. The synthesis technology of the present invention solves the problems of material coking and temperature control through the heating of molten salt, the heat preservation of a jacket pipe and continuous rectification and purification. The present invention has the advantages of even heat transmission, quick temperature raising, high energy utilization rate, high product yield, stable quality and simple operation.
Description
Technical field
The present invention relates to a kind of 2,3, the synthesis technique of 5-pseudocuminol.
Background technology
Adopting 3,5-xylenol and methyl alcohol Synthetic 2,3, in the 5-pseudocuminol traditional technology, product is purified and is adopted single tower or double tower intermittently slightly to heat up in a steamer, batchwise operation, the energy consumption height, yield is low, and output is little, the quality shakiness.When heat source for reaction is electrically heated, all adopt steam companion pipe or electrical tracing pipe that material pipe is accompanied heat, each interchanger all directly contacts heat supply with material, easily produces local superheating, causes the material coking, the temperature control difficulty.
Summary of the invention
Purpose of the present invention is exactly the weak point that overcomes above-mentioned prior art, provides a kind of continuous rectification to purify, adopt 2,3 of fused salt heating, jacket pipe insulation, the synthesis technique of 5-pseudocuminol.
The present invention seeks to reach like this:
Synthesis technique of the present invention is:
(1) batching: 3, the 5-xylenol is squeezed in the preheater with volume pump with after methyl alcohol, water mix;
(2) preheating: the logical steam of preheater is warming up to 120 ℃;
(3) vaporization, overheated: the material after the preheating is sent in the vaporizer, adopted the fused salt heating to make temperature rise to 220-240 ℃, and adopt the steam-jacket pipe insulation; And then pump in the superheater, adopt the fused salt heating to make temperature rise to 300-320 ℃, and adopt the steam-jacket pipe insulation;
Described fused salt is 7 by SODIUMNITRATE, Sodium Nitrite, three kinds of salt of saltpetre by weight: the mixed of 35--45: 48--58 is formed; The steam-jacket pipe insulation is to put a metal tube again in the outside of materail tube, feeds steam or hot water thermal insulating between materail tube and metal tube;
(4) reaction: material is sent in the reactor, under the catalyst action condition, carried out the high temperature methylation reaction; Reactor adopts the fused salt heating; Heating temperature is 300-330 ℃, continuously feeding, and adopt the steam-jacket pipe insulation; Obtain thick product;
(5) continuous rectification: earlier thick product is pumped in rectifying one tower, adopt atmospheric distillation, pure water separates from cat head, and material is discharged at the bottom of tower; Again material is pumped in the header tank, behind standing demix, suction rectifying two towers, under reduced pressure, low-boiling-point substances such as cresols, xylenol are separated from cat head, leftover materials directly pump into rectifying three towers at the bottom of tower, rectifying to take a sample qualified after, finished product is separated from cat head; Remaining tetramethyl phenol high boiling material is regularly discharged at the bottom of tower.
Synthesis technique of the present invention has adopted fused salt heating, jacket pipe insulation and continuous rectification to purify, and has solved material coking and temperature control problem; Conduct heat evenly, heat up rapidly the capacity usage ratio height; The product yield height, steady quality, simple to operate.
Embodiment
Embodiment: during batching 3, you mixed 5-xylenol and methyl alcohol, hydromassage than 1: 1: 1, and the liquid hourly space velocity of squeezing in the preheater with volume pump is 1.0h; Fused salt is that 7: 40: 53 mixed is formed by SODIUMNITRATE, Sodium Nitrite, three kinds of salt of saltpetre by weight; Temperature of reactor is 305--320 ℃, continuously feeding; Catalyzer adopts magnesium oxide and aluminium sesquioxide compounding catalyst.According to above-mentioned technology make 2,3,5-pseudocuminol, yield are 47.6%, cost can reduce by 10%, energy consumption can fall 41%, steady quality.
Adopt the poly-metal deoxide composite catalyst as above-mentioned catalyzer, all the other processing condition are all same as the previously described embodiments, and yield is 65.1%, and cost can reduce by 15%, and energy consumption can reduce by 62%, steady quality.This poly-metal deoxide composite catalyst the applicant separate case simultaneously submits patent application to.
Claims (1)
1, a kind of 2,3, the synthesis technique of 5-pseudocuminol is characterized in that:
(1) batching: 3, the 5-xylenol is squeezed in the preheater with volume pump with after methyl alcohol, water mix;
(2) preheating: the logical steam of preheater is warming up to 120 ℃;
(3) vaporization, overheated: the material after the preheating is sent in the vaporizer, adopted the fused salt heating to make temperature rise to 220-240 ℃, and adopt the steam-jacket pipe insulation; And then pump in the superheater, adopt the fused salt heating to make temperature rise to 300-320 ℃, and adopt the steam-jacket pipe insulation;
Described fused salt is 7 by SODIUMNITRATE, Sodium Nitrite, three kinds of salt of saltpetre by weight: the mixed of 35--45: 48--58 is formed; The steam-jacket pipe insulation is to put a metal tube again in the outside of materail tube, feeds steam or hot water thermal insulating between materail tube and metal tube;
(4) reaction: material is sent in the reactor, under the catalyst action condition, carried out the high temperature methylation reaction; Reactor adopts the fused salt heating; Heating temperature is 300-330 ℃, continuously feeding; And adopt steam-jacket pipe to be incubated; Obtain thick product;
(5) continuous rectification: earlier thick product is pumped in rectifying one tower, adopt atmospheric distillation, pure water separates from cat head, and material is discharged at the bottom of tower; Again material is pumped in the header tank, behind standing demix, suction rectifying two towers, under reduced pressure, cresols, xylenol low-boiling-point substance are separated from cat head, leftover materials directly pump into rectifying three towers at the bottom of tower, rectifying to take a sample qualified after, finished product is separated from cat head; Remaining tetramethyl phenol high boiling material is regularly discharged at the bottom of tower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011150068A CN1140487C (en) | 2001-06-06 | 2001-06-06 | Synthetic process for 2,3,5-trimethylphenol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011150068A CN1140487C (en) | 2001-06-06 | 2001-06-06 | Synthetic process for 2,3,5-trimethylphenol |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1326917A CN1326917A (en) | 2001-12-19 |
| CN1140487C true CN1140487C (en) | 2004-03-03 |
Family
ID=4661602
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011150068A Expired - Fee Related CN1140487C (en) | 2001-06-06 | 2001-06-06 | Synthetic process for 2,3,5-trimethylphenol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1140487C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100366592C (en) * | 2006-04-12 | 2008-02-06 | 哈尔滨市依兰中太化工有限公司 | 2,3,5-trimethylphenol and preparation method for the same |
-
2001
- 2001-06-06 CN CNB011150068A patent/CN1140487C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1326917A (en) | 2001-12-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104341298B (en) | A kind of take methyl ricinolcic acid as raw material cracking for the device of methyl undecylenate and technique | |
| CN103613501B (en) | Method with macropore strong acid cation exchanger resin for catalyst preparing tributyl citrate | |
| CN101020838A (en) | Biodiesel oil preparing process and apparatus | |
| CN105503530A (en) | Multi-effect thermal coupling rectification production apparatus and technological method of alkali process sodium methoxide preparation | |
| CN112028757B (en) | Preparation method of 3-methyl-2-cyclopentene-1-ketone | |
| CN102381940A (en) | Production method of C5 enol | |
| US2936321A (en) | Process for hydrolyzing lower aliphatic esters and separation of resulting products | |
| CN101337890B (en) | Method for preparing methyl acetoacetate by using novel composite catalyst | |
| CN100362009C (en) | 2-deoxidized glucose preparation method | |
| CN102070189A (en) | Method for removing vanadium from titanium tetrachloride | |
| CN1140487C (en) | Synthetic process for 2,3,5-trimethylphenol | |
| CN106748631A (en) | A kind of monochloro methane energy-saving processing technique and device | |
| CN105439824A (en) | Synthesis method of piceatannol | |
| CN112375011A (en) | Preparation method of N, N-diethylhydroxylamine | |
| CN110483283A (en) | A kind of synthetic method and synthesizer of propyl propionate | |
| CN1324760A (en) | Production process of potassium dihydrogen phosphate | |
| CN110343035A (en) | A method of injection continuous hydrolysis prepares natural benzaldehyde | |
| JPS54135710A (en) | Preparation of isobutene by decomposition of tertiary butanol | |
| CN203072835U (en) | Syrup heater | |
| CN201426985Y (en) | Novel glycerin distillation device | |
| JPH058693B2 (en) | ||
| CN208791523U (en) | A kind of purification alpha-pyrrolidone steams the device of slag | |
| CN106977397A (en) | A kind of synthetic method of 3,4,5 trimethoxybenzoic acid | |
| CN112142571A (en) | Method for preparing citral precursor by continuously catalytically cracking acetal | |
| CN111214843A (en) | Distillation device and production method of high-quality sodium methyl taurate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20040303 Termination date: 20130606 |