CN105753678A - Process for preparing difluoro chloroacetone - Google Patents
Process for preparing difluoro chloroacetone Download PDFInfo
- Publication number
- CN105753678A CN105753678A CN201610263106.XA CN201610263106A CN105753678A CN 105753678 A CN105753678 A CN 105753678A CN 201610263106 A CN201610263106 A CN 201610263106A CN 105753678 A CN105753678 A CN 105753678A
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- CN
- China
- Prior art keywords
- difluoro
- chlroacetone
- preparation technology
- acid
- tail gas
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/61—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups
- C07C45/65—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by splitting-off hydrogen atoms or functional groups; by hydrogenolysis of functional groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention discloses a process for preparing difluoro chloroacetone.The process comprises the following steps that chlorodifluoroethane ethyl acetoacetate and dilute sulphuric acid are added to a glass reaction bottle with a stirring and rectifying column and a condensation device; temperature rise operation is slowly carried out, and then reaction rectifying operation is carried out; finished fraction products within a certain temperature range at the top of a tower are collected, and the rear portion of a fraction and receiving bottle is connected with a tail gas water absorbing device to reduce the products taken away by CO2; absorbing liquid absorbed by the tail gas water absorbing device and tap water are mixed to obtain sulfuric acid capable of being reused.According to the process, a reaction and rectification device is used for producing and obtaining difluoro chloroacetone, high selectivity is achieved, the conversion rate is high, the production capacity is high, the product purity is high, operation is easy and convenient, energy consumption is low, a reagent is easy to obtain, the adopted sulfuric acid can be reused, cleanliness and environment friendliness are achieved, and safety and reliability are achieved.
Description
Technical field
The invention belongs to chemical production technical field, be specifically related to the preparation technology of a kind of difluoro chlroacetone.
Background technology
Difluoro chlroacetone is a kind of particularly useful fluorine-containing organic fine chemicals, it is possible to synthesize fluorine-containing heterocycles as difluorochloromethyl building block.Existence due to acetonyl, its compound cyclization easily and containing amino, as formed the heterocyclic compounds such as imidazoles containing difluorochloromethyl, thiophene, oxazole with the cyclization such as amide, thioamides, thiourea, aminopyridine, Aminopyrazine, it is mainly used in synthetic drug intermediate or crude drug, has a wide range of applications at medicine, pesticide field.
The synthetic method of difluoro chlroacetone mainly has: 1) chlorine fluorine acetone is the reducing process of raw material, and chlorine fluorine acetone used can be 3,1-bis-chloro-1,1-difluoro acetone, 3,3,1-tri-chloro-1,1-difluoro acetone etc., and they can be obtained by the catalyzed fluoride of corresponding acetone dichloride.This course of reaction is complicated, and condition is harsh, and side reaction is more, is not suitable for industrialized production.2) chloro-1, the 1-bis-fluoro-2-nitropropane of nitro compound 1-is under the effect of highly basic such as sodium alkoxide, potassium alcoholate, generates difluoro chlroacetone through low-temperature oxidation.Reaction needed carries out at-78 DEG C, and the mixture that the product obtained is difluoro chlroacetone, difluoro chlroacetone hydrate, the hemiacetal of difluoro chlroacetone and methanol.This severe reaction conditions, and product separation purification difficult, yield is relatively low.
Summary of the invention
Goal of the invention: the invention aims to solve deficiency of the prior art, there is provided one to adopt reaction and rectification device to produce and draw difluoro chlroacetone, selectivity is high, conversion ratio is high, production capacity is high, product purity is high, easy and simple to handle, energy consumption is low, and reagent is easy to get, the repeatable utilization of sulphuric acid used, clean environment firendly, the preparation technology of safe and reliable difluoro chlroacetone.
Technical scheme: the preparation technology of a kind of difluoro chlroacetone of the present invention, comprises the steps:
(1) difluoro chloroacetyl acetacetic ester and diluted acid are joined in the glass reaction bottle with stirring and rectifying column and condensing unit；
(2) slowly carry out warming temperature, then react distillation operation；
(3) collecting the fraction finished product of tower top certain temperature range, fraction receiving bottle is followed by tail gas water absorption plant, to reduce the CO2 product taken away；
(4) the absorption liquid that tail gas water absorption plant absorbs and concentrated acid are mixed to get and need concentration；
(5) concentrated acid obtains diluted acid with absorbing after liquid is diluted, it is provided that reuse to step (1).
Further, step (1) described difluoro chloroacetyl acetacetic ester is 1:0.5～10 with the weight ratio of described diluted acid.
Further, step (1) and the described diluted acid of step (5) adopt dilute sulfuric acid or dilute hydrochloric acid.
Further, the Solute mass fraction of step (1) and step (5) described diluted acid is 5%-70%.
Further, step (2) described intensification refers to be warmed up to 30-120 DEG C.
Further, the certain temperature range of the described collection tower top of step (3) refers to the temperature range of 45-47 DEG C.
Beneficial effect: the present invention adopts reaction and rectification device to produce and draws difluoro chlroacetone, selectivity is high, conversion ratio is high, production capacity is high, product purity is high, easy and simple to handle, energy consumption is low, and reagent is easy to get, the repeatable utilization of sulphuric acid used, clean environment firendly, safe and reliable.
Accompanying drawing explanation
Fig. 1 is the overall flow schematic diagram of the present invention.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, present disclosure is described in further detail:
Embodiment 1
The preparation technology of a kind of difluoro chlroacetone as shown in Figure 1, comprises the steps:
(1) by 500g difluoro chloroacetyl acetacetic ester and etc. 20% dilute sulfuric acid of weight join in the glass reaction bottle with stirring and rectifying column and condensing unit；
(2) slowly carry out being warmed up to 30 DEG C, then react distillation operation；
(3) collecting the fraction finished product of tower top 45 DEG C, fraction receiving bottle is followed by tail gas water absorption plant, to reduce the CO2 product taken away；
(4) the absorption liquid that tail gas water absorption plant absorbs mixes with concentrated sulphuric acid；
(5) concentrated sulphuric acid obtains needing the dilute sulfuric acid of concentration after being diluted, it is provided that reuse to step (1).
Embodiment 2
The preparation technology of a kind of difluoro chlroacetone as shown in Figure 1, comprises the steps:
(1) 30% dilute hydrochloric acid of 600g difluoro chloroacetyl acetacetic ester and 1200g is joined in the glass reaction bottle with stirring and rectifying column and condensing unit；
(2) slowly carry out being warmed up to 100 DEG C, then react distillation operation；
(3) collecting the fraction finished product of tower top 47 DEG C, fraction receiving bottle is followed by tail gas water absorption plant, to reduce the CO2 product taken away；
(4) the absorption liquid that tail gas water absorption plant absorbs mixes with concentrated hydrochloric acid；
(5) concentrated hydrochloric acid obtains needing the dilute hydrochloric acid of concentration after being diluted, it is provided that reuse to step (1).
Embodiment 3
The preparation technology of a kind of difluoro chlroacetone as shown in Figure 1, comprises the steps:
(1) 70% dilute sulfuric acid of 550g difluoro chloroacetyl acetacetic ester and 5500g is joined in the glass reaction bottle with stirring and rectifying column and condensing unit；
(2) slowly carry out being warmed up to 65 DEG C, then react distillation operation；
(3) collecting the fraction finished product of tower top 46 DEG C, fraction receiving bottle is followed by tail gas water absorption plant, to reduce the CO2 product taken away；
(4) the absorption liquid that tail gas water absorption plant absorbs mixes with concentrated sulphuric acid；
(5) concentrated sulphuric acid obtains needing the dilute sulfuric acid of concentration after being diluted, it is provided that reuse to step (1).
The present invention adopts reaction and rectification device to produce and draws difluoro chlroacetone, and selectivity is high, conversion ratio is high, production capacity is high, product purity is high, easy and simple to handle, energy consumption is low, and reagent is easy to get, the repeatable utilization of sulphuric acid used, clean environment firendly, safe and reliable.
The above, it it is only presently preferred embodiments of the present invention, not the present invention is done any pro forma restriction, although the present invention is disclosed above with preferred embodiment, but it is not limited to the present invention, any those skilled in the art, without departing within the scope of technical solution of the present invention, when the technology contents of available the disclosure above makes a little change or is modified to the Equivalent embodiments of equivalent variations, in every case it is the content without departing from technical solution of the present invention, according to any simple modification that above example is made by the technical spirit of the present invention, equivalent variations and modification, all still fall within the scope of technical solution of the present invention.
Claims (6)
1. the preparation technology of a difluoro chlroacetone, it is characterised in that: comprise the steps:
(1) difluoro chloroacetyl acetacetic ester and diluted acid are joined in the glass reaction bottle with stirring and rectifying column and condensing unit；
(2) slowly carry out warming temperature, then react distillation operation；
(3) collecting the fraction finished product of tower top certain temperature range, fraction receiving bottle is followed by tail gas water absorption plant, to reduce the CO2 product taken away；
(4) the absorption liquid that tail gas water absorption plant absorbs and concentrated acid are mixed to get and need concentration；
(5) concentrated acid obtains diluted acid with absorbing after liquid is diluted, it is provided that reuse to step (1).
2. the preparation technology of a kind of difluoro chlroacetone according to claim 1, it is characterised in that: the weight ratio of step (1) described difluoro chloroacetyl acetacetic ester and described diluted acid is 1:0.5～10.
3. the preparation technology of a kind of difluoro chlroacetone according to claim 1, it is characterised in that: step (1) and the described diluted acid of step (5) adopt dilute sulfuric acid or dilute hydrochloric acid.
4. the preparation technology of a kind of difluoro chlroacetone according to claim 1 or 3, it is characterised in that: the Solute mass fraction of step (1) and step (5) described diluted acid is 5%-70%.
5. the preparation technology of a kind of difluoro chlroacetone according to claim 1, it is characterised in that: step (2) described intensification refers to be warmed up to 30-120 DEG C.
6. the preparation technology of a kind of difluoro chlroacetone according to claim 1, it is characterised in that: the certain temperature range of the described collection tower top of step (3) refers to the temperature range of 45-47 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610263106.XA CN105753678A (en) | 2016-04-26 | 2016-04-26 | Process for preparing difluoro chloroacetone |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610263106.XA CN105753678A (en) | 2016-04-26 | 2016-04-26 | Process for preparing difluoro chloroacetone |
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| CN105753678A true CN105753678A (en) | 2016-07-13 |
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| CN201610263106.XA Pending CN105753678A (en) | 2016-04-26 | 2016-04-26 | Process for preparing difluoro chloroacetone |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19725802A1 (en) * | 1996-07-10 | 1998-01-15 | Lonza Ag | Preparation of 3,3,3-tri:fluoro-2-hydroxy-2-methyl propionic acid, |
| CN102336640A (en) * | 2011-07-20 | 2012-02-01 | 南通宝凯化工有限公司 | Synthesis method of halogen acetone |
-
2016
- 2016-04-26 CN CN201610263106.XA patent/CN105753678A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19725802A1 (en) * | 1996-07-10 | 1998-01-15 | Lonza Ag | Preparation of 3,3,3-tri:fluoro-2-hydroxy-2-methyl propionic acid, |
| CN102336640A (en) * | 2011-07-20 | 2012-02-01 | 南通宝凯化工有限公司 | Synthesis method of halogen acetone |
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Application publication date: 20160713 |
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