CN105330531B - To the continuous production processes of methyl benzoyl chloride - Google Patents
To the continuous production processes of methyl benzoyl chloride Download PDFInfo
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- CN105330531B CN105330531B CN201510931007.XA CN201510931007A CN105330531B CN 105330531 B CN105330531 B CN 105330531B CN 201510931007 A CN201510931007 A CN 201510931007A CN 105330531 B CN105330531 B CN 105330531B
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- methyl benzoyl
- benzoyl chloride
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/58—Preparation of carboxylic acid halides
- C07C51/60—Preparation of carboxylic acid halides by conversion of carboxylic acids or their anhydrides or esters, lactones, salts into halides with the same carboxylic acid part
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/58—Preparation of carboxylic acid halides
- C07C51/64—Separation; Purification; Stabilisation; Use of additives
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of continuous production processes to methyl benzoyl chloride, belong to technical field of fine.Described continuous production processes are under phase transfer catalyst existence condition, p-methylbenzoic acid is added in reactor with thionyl chloride and reacted, obtain reaction solution, then reaction solution is added in rectifying column and carries out atmospheric distillation to reclaim thionyl chloride therein, obtain to methyl benzoyl chloride crude product, methyl benzoyl chloride crude product will be added in thin film evaporator and be evaporated under reduced pressure, obtained to methyl benzoyl chloride.The present invention solves the problems, such as that unstable product quality present in batch process, automation degree of equipment are low and labor intensity is big, with process route it is succinct, with short production cycle, product yield is high the characteristics of, while production capacity is improved, the generation of side reaction turn avoid.
Description
Technical field
The present invention relates to a kind of continuous production processes to methyl benzoyl chloride, belong to technical field of fine.
Background technology
With the fast development of high polymer material, a kind of important chemical intermediate is increasingly becoming to methyl benzoyl chloride,
Increasingly paid close attention to by numerous researchers, its excellent performance is in medicine, agricultural chemicals, dyestuff and photosensitive material production etc.
It is widely used.Prepared mostly using the production technology of batch (-type) to methyl benzoyl chloride, batch process tool at present
There is the characteristics of equipment is simple, versatility is wide, it is relatively inexpensive using this method when demand is relatively low, but with production scale
Expansion, during using batch process to produce to methyl benzoyl chloride, exist different batches of product quality is unstable, equipment from
The problems such as dynamicization degree is low and labor intensity is big.
The content of the invention
It is an object of the invention to provide a kind of continuous production processes to methyl benzoyl chloride, have technical process it is simple,
With short production cycle, the characteristics of product yield is high.
Continuous production processes of the present invention to methyl benzoyl chloride, be under phase transfer catalyst existence condition,
P-methylbenzoic acid is added in reactor with thionyl chloride and reacted, reaction solution is obtained, is then added to reaction solution
Atmospheric distillation is carried out in rectifying column to reclaim thionyl chloride therein, is obtained to methyl benzoyl chloride crude product, will be to methylbenzene first
Crude acid chloride is added in thin film evaporator and is evaporated under reduced pressure, and obtains to methyl benzoyl chloride.
Wherein：
Described phase transfer catalyst is any one or more in quaternary ammonium salt and tertiary amine with ion pair, wherein,
Quaternary ammonium salt with ion pair is benzyltriethylammoinium chloride, TBAB, tetrabutylammonium chloride, tetrabutyl hydrogen sulfate
Ammonium, tri-n-octyl methyl ammonium chloride, DTAC and tetradecyl trimethyl ammonium chloride；Tertiary amine be tri-n-butylamine and
Pyridine.
Described p-methylbenzoic acid and the mol ratio of thionyl chloride are 1:1.05-1.15.
Described phase transfer catalyst dosage is the 0.05-0.1wt% of p-methylbenzoic acid.
Described reaction temperature is 25-45 DEG C, reaction time 4-10h, has reacted the follow-up warm 0.5h of continuation of insurance.
The temperature of described vacuum distillation is 115-127 DEG C, and the vacuum of vacuum distillation is 630-750mmHg.
The thin film evaporator used in the present invention has heat transfer coefficient height, evaporation intensity is big, low-temperature evaporation effect is good, material
The range of viscosities that residence time is short, applicable is wide and the characteristics of operating flexibility is big, in the row such as chemical industry, light industry, pharmacy, environmental protection and food
Progressively it is promoted and applies in industry.
Beneficial effects of the present invention are as follows：
The continuous production processes of the present invention have the characteristics of process route is succinct, with short production cycle, product yield is high, are carrying
While high productive capacity, the generation of side reaction turn avoid.
Embodiment
The present invention is described further with reference to embodiments.
Embodiment 1
It is as follows to the continuous production processes of methyl benzoyl chloride：
(1) 1000kg p-methylbenzoic acids and 917.49kg thionyl chlorides are added in reactor, then add 0.5kg
Benzyltriethylammoinium chloride, 9h is reacted at 25 DEG C, until being emerged without gas, be further continued for insulation 0.5 hour, obtain reaction solution；
(2) reaction solution is added in rectifying column, entering tower flow rate 4.7kg/min, the tower reactor of rectifying column is added using steam
Heat, for temperature control at 95 DEG C, the extraction flow of tower top light component is 4.2kg/min, is back to after the condensed device condensation of light component
In reactor, after testing, the content of thionyl chloride is 96.8wt% in light component；
(3) tower bottom of rectifying tower is added in thin film evaporator to methyl benzoyl chloride crude product, feed rate is
3.9kg/min, regulation vacuum are 630mmHg, are evaporated under reduced pressure at 127 DEG C, obtain 1102.5kg to toluyl
Chlorine, yield 97.1%, after testing, to the chromatographic content 99% of methyl benzoyl chloride.
Embodiment 2
It is as follows to the continuous production processes of methyl benzoyl chloride：
(1) 870kg p-methylbenzoic acids and 836kg thionyl chlorides are added in reactor, then add 0.6525kg
Tetradecyl trimethyl ammonium chloride, 7h is reacted at 29 DEG C, until being emerged without gas, be further continued for insulation 0.5 hour, reacted
Liquid；
(2) reaction solution is added in rectifying column, entering tower flow rate 4.7kg/min, the tower reactor of rectifying column is added using steam
Heat, for temperature control at 99 DEG C, the extraction flow of tower top light component is 4.2kg/min, is back to after the condensed device condensation of light component
In reactor, after testing, the content of thionyl chloride is 97.2wt% in light component；
(3) tower bottom of rectifying tower is added in thin film evaporator to methyl benzoyl chloride crude product, feed rate is
3.9kg/min, regulation vacuum are 690mmHg, are evaporated under reduced pressure at 120 DEG C, obtain 963.2kg to toluyl
Chlorine, yield 97.5%, after testing, to the chromatographic content 99.1% of methyl benzoyl chloride.
Embodiment 3
It is as follows to the continuous production processes of methyl benzoyl chloride：
(1) 1360kg p-methylbenzoic acids and 1366kg thionyl chlorides are added in reactor, then add 1.36kg
Tetradecyl trimethyl ammonium chloride, 4h is reacted at 45 DEG C, until being emerged without gas, be further continued for insulation 0.5 hour, reacted
Liquid；
(2) reaction solution is added in rectifying column, entering tower flow rate 4.7kg/min, the tower reactor of rectifying column is added using steam
Heat, for temperature control at 105 DEG C, the extraction flow of tower top light component is 4.2kg/min, is back to after the condensed device condensation of light component
In reactor, after testing, the content of thionyl chloride is 96.9wt% in light component；
(3) tower bottom of rectifying tower is added in thin film evaporator to methyl benzoyl chloride crude product, feed rate is
3.9kg/min, regulation vacuum are 630mmHg, are evaporated under reduced pressure at 127 DEG C, obtain 1516.5kg to toluyl
Chlorine, yield 98.2%, after testing, to the chromatographic content 99.4% of methyl benzoyl chloride.
Claims (1)
- A kind of 1. continuous production processes to methyl benzoyl chloride, it is characterised in that：Step is as follows：(1) 1000kg p-methylbenzoic acids and 917.49kg thionyl chlorides are added in reactor, then add 0.5kg Benzyltriethylammoinium chloride, 9h is reacted at 25 DEG C, until being emerged without gas, be further continued for insulation 0.5 hour, obtain reaction solution；(2) reaction solution being added in rectifying column, entering tower flow rate 4.7kg/min, the tower reactor of rectifying column is heated using steam, For temperature control at 95 DEG C, the extraction flow of tower top light component is 4.2kg/min, and reaction is back to after the condensed device condensation of light component In kettle, after testing, the content of thionyl chloride is 96.8wt% in light component；(3) tower bottom of rectifying tower is added in thin film evaporator to methyl benzoyl chloride crude product, feed rate 3.9kg/ Min, regulation vacuum are 630mmHg, are evaporated under reduced pressure at 127 DEG C, obtain 1102.5kg to methyl benzoyl chloride, receive Rate is 97.1%, after testing, to the chromatographic content 99% of methyl benzoyl chloride.
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| CN201510931007.XA CN105330531B (en) | 2015-12-14 | 2015-12-14 | To the continuous production processes of methyl benzoyl chloride |
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| CN201510931007.XA CN105330531B (en) | 2015-12-14 | 2015-12-14 | To the continuous production processes of methyl benzoyl chloride |
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| CN105330531A CN105330531A (en) | 2016-02-17 |
| CN105330531B true CN105330531B (en) | 2018-03-16 |
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| CN101717333B (en) * | 2009-10-30 | 2012-08-22 | 周成云 | Preparation method of (-)-di(p-toluoyl)tartaric acid |
| CN102093291B (en) * | 2010-12-10 | 2012-10-24 | 上海应用技术学院 | Preparation method of N-[4-(triethyl aminomethyl) benzoyl] caprolactam bromide |
| CN103641706B (en) * | 2013-12-04 | 2015-08-05 | 山东凯盛新材料有限公司 | The preparation method of pyromellitic trimethylsilyl chloride |
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Address after: Double Yang Zichuan District 255190 Shandong city of Zibo Province Applicant after: Shandong Kaisheng New Materials Co.,Ltd. Address before: Double Yang Zichuan District 255190 Shandong city of Zibo Province Applicant before: SHANDONG KAISHENG NEW MATERIALS CO., LTD. |
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Inventor after: Zhang Congcong Inventor after: Xiao Zhiyu Inventor after: Bi Yixia Inventor after: Zhang Taiming Inventor after: Wang Zhiliang Inventor after: Xie Shengbin Inventor after: Zhang Shanmin Inventor after: Zhang Liang Inventor after: Liu Song Inventor after: Shi Yufei Inventor before: Zhang Congcong Inventor before: Bi Yixia Inventor before: Zhang Taiming Inventor before: Xie Shengbin Inventor before: Zhang Shanmin Inventor before: Wang Zhiliang |
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