CN110433515A - Plate distillation column purifies reaction system - Google Patents
Plate distillation column purifies reaction system Download PDFInfo
- Publication number
- CN110433515A CN110433515A CN201910581883.2A CN201910581883A CN110433515A CN 110433515 A CN110433515 A CN 110433515A CN 201910581883 A CN201910581883 A CN 201910581883A CN 110433515 A CN110433515 A CN 110433515A
- Authority
- CN
- China
- Prior art keywords
- condenser
- tower
- reaction system
- plate distillation
- distillation column
- 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.)
- Pending
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to fluorine chemistry fields, and in particular to a kind of Plate distillation column purifying reaction system, including reaction kettle, condenser and partitioned column；Reaction kettle includes autoclave body, the feed inlet being arranged at the top of autoclave body and interface and the discharge gate that autoclave body bottom is arranged in；Interface is connected to by connector with condenser；Condenser is connected to by pipeline with partitioned column；Partitioned column includes tower body and the partition along the setting of tower height direction；The tower bottom of partitioned column is provided with heating mantle, tower top is provided with condenser pipe；The left-hand end of destilling tower is provided with pre-separation product inlet, and right-hand end is provided with separation product outlet；Control valve is provided on pipeline.The present invention provides a kind of Plate distillation columns to purify reaction system, and using the setting of tower body partition, it can be achieved that a rectifying removes low boiling point and high-boiling-point impurity simultaneously, purity > 99.9% of perfluor isobutyl acyl fluorides is even higher after purification.
Description
Technical field
The invention belongs to fluorine chemistry fields, and in particular to a kind of Plate distillation column purifying reaction system.
Background technique
Perfluor isobutyl acyl fluorides is a kind of important fluorochemical, and using relatively broad, it is clear to can be used for electronics industry
Lotion, etchant, pesticide intermediate, fluorine material monomer etc..
The method for preparing perfluor butyryl fluorine has very much, such as electrochemical process or chemical synthesis, wherein reaction kettle liquid phase
Method is common chemical combination synthetic method, its advantage is that it is easy to operate, but it is reacted since one kettle way feeds intake, so often
Low output.And when preparing perfluor isobutyl acyl fluorides as raw material using hexafluoropropene and carbonyl fluoride, there are the by-products of seven carbon ketone of perfluor
Object, although seven carbon ketone of perfluor can be used conventional vacuum distillation with perfluor butyryl fluorine and be separated, in conventional method
But it is difficult for seven carbon ketone of perfluor to be kept completely separate, to influence the quality of perfluor isobutyl acyl fluorides.Perfluor is prepared for one pot reaction
When isobutyl acyl fluorides, low output, and it is difficult to the defects of separating seven carbon ketone of perfluor, therefore be badly in need of a kind of simply and easily perfluor isobutyryl
Fluorine prepares purification devices.
Summary of the invention
The purpose of the present invention is to provide a kind of Plate distillation columns to purify reaction system.
The present invention to achieve the above object, using following technical scheme:
A kind of Plate distillation column purifying reaction system, including reaction kettle, condenser and partitioned column；The reaction kettle packet
Include autoclave body, the feed inlet being arranged at the top of the autoclave body and interface and the discharge gate that the autoclave body bottom is set；Institute
The interface stated is connected to by connector with condenser；The condenser is connected to by pipeline with partitioned column；The partitioned column
Including tower body and along the partition of tower height direction setting；The tower bottom of the partitioned column is provided with heating mantle, tower top be provided with it is cold
Solidifying pipe；The left-hand end of the destilling tower is provided with pre-separation product inlet, and right-hand end is provided with separation product outlet；Described
Region between the upper end and tower top of partition is liquid dispensing section；Region between the lower end and tower bottom of the partition is gas
Dispensing section；Control valve is provided on the pipeline.
Serpentine condenser road is provided in the condenser and the condenser pipe；The serpentine condenser road two
End is respectively arranged with refrigerant inlet and refrigerant exit.
The condenser both ends are respectively arranged with refluxing opening and exhaust outlet；The refluxing opening and the autoclave body
Orifice；The exhaust outlet is connected to the pre-separation product inlet of the partitioned column.
Described condenser pipe one end is provided with liquid reflux mouth；Connect at the top of the liquid reflux mouth and the tower body
It is logical.
The reaction kettle is for synthesizing perfluor isobutyl acyl fluorides；The partitioned column is for separating seven carbon ketone of perfluor；It is described
Reaction kettle in have that raw material is hexafluoropropene and carbonyl fluoride, catalyst are 2- perfluoroalkyl benzothiazole compound, solvent
For acetonitrile.
The molar ratio of the hexafluoropropene, carbonyl fluoride and 2- perfluoroalkyl benzothiazole compound are as follows: 1:1-2:
0.05-0.1。
The 2- perfluoroalkyl benzothiazole compound is 2- perfluoropropane base benzothiazole compound, 2- perfluor
Butane group benzothiazole compound or 2- perflenapent base benzothiazole compound.
Preparation method in reaction kettle is specifically include the following steps: be raw material, 2- perfluorinated butane base by hexafluoropropene, carbonyl fluoride
Benzothiazole and solvent are put into reaction kettle, are heated to 75-85 DEG C of reaction, are reacted 2-5 hours.
Compared with prior art, the beneficial effects of the present invention are:
The present invention provides a kind of Plate distillation columns to purify reaction system, using the setting of tower body partition, it can be achieved that primary
Rectifying removes low boiling point and high-boiling-point impurity simultaneously, and purity > 99.9% of perfluor isobutyl acyl fluorides is even higher after purification.Meanwhile
It can be dissolved in acetonitrile solvent, uniformly using 2- perfluoroalkyl benzothiazole compound as catalyst in the application
Be wrapped in around raw material hexafluoropropene, its own electron donor receptor performance having can be by phosphinylidyne fluoro free radical, hexafluoro third
The isobutyryl fluoro free radical generated under alkene free radical and alkaline condition is closely linked, and helps and shortens the reaction time, mentions
High yield, therefore combine the application volume device and method to be not only able to improve the yield of perfluor isobutyl acyl fluorides and can utilize
Partitioned column removes the seven carbon ketone of perfluor of trace.
Detailed description of the invention
Fig. 1 is the overall structure diagram that Plate distillation column of the present invention purifies reaction system；
Specific embodiment
In order to make those skilled in the art more fully understand technical solution of the present invention, with reference to the accompanying drawing and most
The present invention is described in further detail for good embodiment.
Fig. 1 shows a kind of Plate distillation column purifying reaction system, including reaction kettle 1, condenser 2 and partitioned column 3；It is described
Reaction kettle include autoclave body 11, the feed inlet being arranged at the top of the autoclave body 12 and interface 13 and the kettle be set
The discharge gate 14 of body bottom；The interface is connected to by connector with condenser；The condenser passes through pipeline and partition
Tower connection；The partitioned column includes tower body 31 and the partition 32 along the setting of tower height direction；The tower bottom of the partitioned column is set
It is equipped with heating mantle 33, tower top is provided with condenser pipe 34；The left-hand end of the destilling tower is provided with pre-separation product inlet 35, right
Side is provided with separation product outlet 36；Region between the upper end and tower top of the partition is liquid dispensing section；Described
Region between the lower end and tower bottom of partition is gas dispensing section；Control valve is provided on the pipeline.The condenser
And serpentine condenser road is provided in the condenser pipe；The serpentine condenser road both ends are respectively arranged with refrigerant inlet
And refrigerant exit.The condenser both ends are respectively arranged with refluxing opening 21 and exhaust outlet 22；The refluxing opening and institute
The orifice for the autoclave body stated；The exhaust outlet is connected to the pre-separation product inlet of the partitioned column.The condensation
Pipe one end is provided with liquid reflux mouth 341；The liquid reflux mouth is connected to the top of the tower body.
Embodiment 1: a method of perfluor isobutyl acyl fluorides being prepared using the device, is included the following steps: with hexafluoro
Propylene 1mol, carbonyl fluoride 1.5mol are raw material, 2- perfluorinated butane base benzothiazole 0.08mol is catalyst, are added to 100ml second
In nitrile solution, 85 DEG C of heating detect the content of target product in 2h, 3h, 4h, 5h, 6h respectively.It see the table below 1 respectively.Reaction terminates
After will open control valve, make product flow into Plate distillation column in distilled, detected in obtained product through GC-MS, show to produce
Seven carbon ketone of perfluor is not contained in object.
Table 1
| Reaction time | Yield |
| 2h | 92% |
| 3h | 93.5% |
| 4h | 93.2% |
| 5h | 91.6% |
| 6h | 91.25% |
Embodiment 2: embodiment 2 and the difference of embodiment are only that the catalyst of use is different, are 2- perflenapent base
Benzothiazole, rule of the reaction rule to 2- perfluorinated butane base benzothiazole in 2-6h is similar, but yield is less than in embodiment 1
With the yield of 2- perfluorinated butane base benzothiazole, this is no longer going to repeat them.
The above is only a preferred embodiment of the present invention, for those of ordinary skill in the art, according to the present invention
Thought, there will be changes in the specific implementation manner and application range, and the content of the present specification should not be construed as to the present invention
Limitation.
Claims (8)
1. a kind of Plate distillation column purifies reaction system, which is characterized in that including reaction kettle, condenser and partitioned column；It is described
Reaction kettle include autoclave body, the feed inlet being arranged at the top of the autoclave body and interface and the autoclave body bottom be set
Discharge gate；The interface is connected to by connector with condenser；The condenser is connected to by pipeline with partitioned column；Institute
The partitioned column stated includes tower body and the partition along the setting of tower height direction；The tower bottom of the partitioned column is provided with heating mantle, tower
Top is provided with condenser pipe；The left-hand end of the destilling tower is provided with pre-separation product inlet, and right-hand end is provided with separation product
Outlet；Region between the upper end and tower top of the partition is liquid dispensing section；Between the lower end and tower bottom of the partition
Region be gas dispensing section；Control valve is provided on the pipeline.
2. Plate distillation column according to claim 1 purifies reaction system, which is characterized in that the condenser and institute
Serpentine condenser road is provided in the condenser pipe stated；The serpentine condenser road both ends are respectively arranged with refrigerant inlet and cold
Matchmaker outlet.
3. Plate distillation column according to claim 1 purifies reaction system, which is characterized in that the condenser both ends point
It is not provided with refluxing opening and exhaust outlet；The orifice of the refluxing opening and the autoclave body；The exhaust outlet and institute
The pre-separation product inlet for the partitioned column stated is connected to.
4. Plate distillation column according to claim 1 purifies reaction system, which is characterized in that described condenser pipe one end is set
It is equipped with liquid reflux mouth；The liquid reflux mouth is connected to the top of the tower body.
5. Plate distillation column according to claim 1 purifies reaction system, which is characterized in that the reaction kettle is for closing
At perfluor isobutyryl fluorine；The partitioned column is for separating seven carbon ketone of perfluor；Have in the reaction kettle raw material be hexafluoropropene,
And carbonyl fluoride, catalyst are 2- perfluoroalkyl benzothiazole compound, solvent is acetonitrile.
6. Plate distillation column according to claim 5 purifies reaction system, which is characterized in that the hexafluoropropene, carbon
The molar ratio of acyl fluorides and 2- perfluoroalkyl benzothiazole compound are as follows: 1:1-2:0.05-0.1.
7. Plate distillation column according to claim 5 purifies reaction system, which is characterized in that the 2- perfluoroalkyl benzene
And thiazole compound be 2- perfluoropropane base benzothiazole compound, 2- perfluorinated butane base benzothiazole compound or
2- perflenapent base benzothiazole compound.
8. Plate distillation column according to claim 5 purifies reaction system, which is characterized in that preparation method has in reaction kettle
Body includes the following steps: hexafluoropropene, carbonyl fluoride to be that raw material, 2- perfluorinated butane base benzothiazole and solvent put into reaction
In kettle, it is heated to 75-85 DEG C of reaction, is reacted 2-5 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910581883.2A CN110433515A (en) | 2019-06-30 | 2019-06-30 | Plate distillation column purifies reaction system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910581883.2A CN110433515A (en) | 2019-06-30 | 2019-06-30 | Plate distillation column purifies reaction system |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110433515A true CN110433515A (en) | 2019-11-12 |
Family
ID=68429363
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910581883.2A Pending CN110433515A (en) | 2019-06-30 | 2019-06-30 | Plate distillation column purifies reaction system |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110433515A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101798528A (en) * | 2010-01-22 | 2010-08-11 | 天津大学 | Partial energy coupled separation system of carbon 3, carbon 4 and carbon 5 used in predepropanization technological process and operation method |
| CN108031139A (en) * | 2017-11-23 | 2018-05-15 | 兰州寰球工程有限公司 | A kind of energy conserving system of acetonitrile method extracting butadiene |
| CN108299167A (en) * | 2018-01-31 | 2018-07-20 | 天津大学 | The method and apparatus for detaching polymethoxy dimethyl ether using next door tower |
| CN109336751A (en) * | 2018-11-18 | 2019-02-15 | 北京宇极科技发展有限公司 | The method that gas phase prepares perfluor ketone |
| CN109608413A (en) * | 2019-01-16 | 2019-04-12 | 郑州大学 | A kind of 2- perfluoroalkyl benzothiazole compound and preparation method thereof |
| CN109748814A (en) * | 2017-11-07 | 2019-05-14 | 浙江蓝天环保高科技股份有限公司 | A kind of preparation method of perfluor isobutyronitrile and its intermediate |
-
2019
- 2019-06-30 CN CN201910581883.2A patent/CN110433515A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101798528A (en) * | 2010-01-22 | 2010-08-11 | 天津大学 | Partial energy coupled separation system of carbon 3, carbon 4 and carbon 5 used in predepropanization technological process and operation method |
| CN109748814A (en) * | 2017-11-07 | 2019-05-14 | 浙江蓝天环保高科技股份有限公司 | A kind of preparation method of perfluor isobutyronitrile and its intermediate |
| CN108031139A (en) * | 2017-11-23 | 2018-05-15 | 兰州寰球工程有限公司 | A kind of energy conserving system of acetonitrile method extracting butadiene |
| CN108299167A (en) * | 2018-01-31 | 2018-07-20 | 天津大学 | The method and apparatus for detaching polymethoxy dimethyl ether using next door tower |
| CN109336751A (en) * | 2018-11-18 | 2019-02-15 | 北京宇极科技发展有限公司 | The method that gas phase prepares perfluor ketone |
| CN109608413A (en) * | 2019-01-16 | 2019-04-12 | 郑州大学 | A kind of 2- perfluoroalkyl benzothiazole compound and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101391975B (en) | Process for separation and purification of N-vinyl pyrrolidone | |
| TWI612031B (en) | Method and device for co-production of cyclohexanol and alkanol | |
| CN107337656B (en) | Reaction system and method for continuously preparing gamma-undecalactone | |
| CN1385408A (en) | Preparation for alpha, beta-unsaturated higher alcohols | |
| RU2015126664A (en) | METHOD FOR PRODUCING DIMETHYLOXALATE | |
| JP5200023B2 (en) | Method for continuously separating a mixture containing morpholine (MO), monoaminodiglycol (ADG), ammonia and water by distillation | |
| CN109293525B (en) | Micro-channel reactor and method for preparing N-alkoxy oxalyl alanine ester by using same | |
| CN110237570A (en) | A kind of hexamethylene diamine lye separation system | |
| CN106831360B (en) | Process method for continuously preparing β -naphthyl methyl ether | |
| CN110433515A (en) | Plate distillation column purifies reaction system | |
| CN105016974A (en) | Separation method for optimizing butanol-octanol product structures | |
| CN100427468C (en) | Apparatus and method for separating 5-bromo-2-methyl pyridine isomer by intermittent rectification under vacuum | |
| JP5837586B2 (en) | Method for producing chlorohydrin composition and method for producing epichlorohydrin using chlorohydrin composition produced by the method | |
| CN109721469A (en) | A kind of preparation method of cyclopentanone | |
| CN105366692B (en) | A kind of high purity liquid HCN and system | |
| CN210993045U (en) | Baffle distillation column purification reaction system | |
| CN210698862U (en) | Isopropyl hydroxylamine rectification system of high yield | |
| CN103649029B (en) | The manufacture method of hexalin, hexalin and the manufacture method of hexanodioic acid | |
| JP2009275019A (en) | Method for refining water-alcohol composition | |
| CN104672397B (en) | High-efficient apparatus for producing of unsaturated resins | |
| CN111704577A (en) | Preparation method of cinacalcet hydrochloride | |
| CN111377798B (en) | Purification equipment and process of 3-methyl-3-butene-1-ol | |
| CN106565438A (en) | Preparation method of isophthalaldehyde | |
| CN202898016U (en) | Equipment for reducing impurity content in iodine pentafluoride | |
| CN111377799B (en) | 3-methyl-3-butene-1-ol dehydration method and device thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20191112 |
|
| RJ01 | Rejection of invention patent application after publication |