CN109574816A - A kind of dichloro pinacoline production technology - Google Patents
A kind of dichloro pinacoline production technology Download PDFInfo
- Publication number
- CN109574816A CN109574816A CN201811509427.9A CN201811509427A CN109574816A CN 109574816 A CN109574816 A CN 109574816A CN 201811509427 A CN201811509427 A CN 201811509427A CN 109574816 A CN109574816 A CN 109574816A
- Authority
- CN
- China
- Prior art keywords
- pinacoline
- chlorine
- dichloro
- hydrochloric acid
- reaction
- 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
-
- 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
- C07C45/63—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 introduction of halogen; by substitution of halogen atoms by other halogen atoms
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/07—Preparation of halogenated hydrocarbons by addition of hydrogen halides
- C07C17/08—Preparation of halogenated hydrocarbons by addition of hydrogen halides to unsaturated hydrocarbons
-
- 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
- C07C45/45—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by condensation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of dichloro pinacoline production technologies, it is characterised in that: specific production technology is as follows: the preparation of S1:2- chlorine isopentane；S2: the synthesis of pinacoline；S3: the rectifying of pinacoline；S4: the synthesis of dichloro pinacoline；S5: the processing of by-product；It carries out using excessive chlorine in chlorination reaction in pinacoline in the present invention, it ensure that pinacoline can react completely, furthermore, using formaldehyde addition in chlorination reaction, the generation of trichlorine pinacoline can be controlled, 3 times of reaction rate or more are also able to ascend simultaneously, general reaction needed between 70-75 hours, and the time can be made to complete reaction between 20-25 hours by the way of adding formaldehyde.
Description
Technical field
The present invention relates to dichloro pinacoline field more particularly to a kind of dichloro pinacoline production technologies.
Background technique
Dichloro pinacoline is a kind of important raw material, and dichloro pinacoline is mostly used for a variety of fine chemistry industries such as medicine, dyestuff
The intermediate of product；Iso-amylene is usually used as raw material in the production of dichloro pinacoline, during producing dichloro pinacoline, leads to
It crosses iso-amylene and generates pinacoline by the addition reaction with hydrochloric acid and with the condensation reaction of formaldehyde, the pinacoline of generation passes through excess
Chlorine carry out addition reaction generate dichloro pinacoline；
The general time in pinacoline production dichloro pinacoline reaction is especially long and is easy to produce trichlorine pinacoline, obtained production
Product purity is relatively low.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of dichloro pinacoline production technologies, are able to solve general dichloro
The production time is long in pinacoline production technology, the low problem of product purity.
In order to solve the above technical problems, the technical solution of the present invention is as follows: a kind of dichloro pinacoline production technology, innovative point
Be: specific production technology is as follows:
The preparation of S1:2- chlorine isopentane: technical hydrochloric acid is cooled to -5 DEG C~5 DEG C, 0 DEG C~3 DEG C are slowly added dropwise under stirring condition
Iso-amylene, be added dropwise, stir 1~3 hour, generate 2- chlorine isopentane；
S2: the synthesis of pinacoline: the 2- chlorine isopentane that step S1 is generated is pumped into condensation reaction kettle by front pump, then
Stirring is opened, while slowly heating, when gas phase temperature reaches 70 DEG C~80 DEG C, starts that first is slowly added dropwise into condensation reaction kettle
Aldehyde is added dropwise, and insulation reaction 1~2 hour, after reaction, cooling, stratification；
S3: the rectifying of pinacoline: upper layer crude product pinacoline carries out rectifying, lower layer's acid solution into 90 DEG C~100 DEG C of rectifier unit
Spent acid distillation still is evacuated to be fractionated；
S4: the synthesis of dichloro pinacoline: the pinacoline after rectifying is put into chlorinating container after metering, chlorine heating
Device is warming up to 75 DEG C, and chlorine is excessively passed into chlorinating container through surge tank, and formaldehyde is added in a kettle, in this temperature
Lower insulation reaction 25h；The dichloro pinacoline that reaction generates is subjected to room temperature cooling and obtains dichloro pinacoline finished product；
S5: the processing of by-product: the excessive chlorine and byproduct hydrogen chloride that the synthesis of dichloro pinacoline is passed through in S4 first pass through
After water is absorbed, dilute hydrochloric acid is obtained；Again excessive chlorine and byproduct hydrogen chloride absorb by liquid alkaline and be handled.
Further, it is being opened after 2- chlorine isopentane is pumped into condensation reaction kettle by front pump in the step S2
Before stirring, absorption by Hydrochloric Acid device is opened, the hydrogen chloride that reaction generates is absorbed into hydrochloric acid through water.
Further, lower layer's acid solution of the S3 step is evacuated to spent acid distillation still, and water, and the volume ratio of acid solution and water is added
For 1:7,80 DEG C~100 DEG C at a temperature of be fractionated, the dilute hydrochloric acid after fractionation is pumped into hydrochloric acid pans, the crude product obtained to fractionation
Pinacoline carries out rectifying into 70 DEG C~80 DEG C of rectifier unit, can obtain purity and reach >=98%, and colourless pinacoline product.
The present invention has the advantages that
1) it carries out using excessive chlorine in chlorination reaction in pinacoline in the present invention, ensure that pinacoline can react completely,
In addition, using formaldehyde addition the generation of trichlorine pinacoline can be controlled, while being also able to ascend reaction rate in chlorination reaction
3 times or more, general reaction needed between 70-75 hours, the time can be made at 20-25 hours by the way of adding formaldehyde
Between complete reaction.
Specific embodiment
The following examples can make professional and technical personnel that the present invention be more fully understood, but therefore not send out this
It is bright to be limited among the embodiment described range.
Embodiment 1:
A kind of dichloro pinacoline production technology, specific production technology are as follows:
The preparation of S1:2- chlorine isopentane: technical hydrochloric acid is cooled to -5 DEG C~5 DEG C, 0 DEG C~3 DEG C are slowly added dropwise under stirring condition
Iso-amylene, be added dropwise, stir 1~3 hour, generate 2- chlorine isopentane；
S2: the synthesis of pinacoline: the 2- chlorine isopentane that step S1 is generated is pumped into condensation reaction kettle by front pump, then
Stirring is opened, while slowly heating, when gas phase temperature reaches 70 DEG C~80 DEG C, starts that first is slowly added dropwise into condensation reaction kettle
Aldehyde is added dropwise, and insulation reaction 1~2 hour, after reaction, cooling, stratification；
S3: the rectifying of pinacoline: upper layer crude product pinacoline carries out rectifying, lower layer's acid solution into 90 DEG C~100 DEG C of rectifier unit
Spent acid distillation still is evacuated to be fractionated；
S4: the synthesis of dichloro pinacoline: the pinacoline after rectifying is put into chlorinating container after metering, chlorine heating
Device is warming up to 75 DEG C, and chlorine is excessively passed into chlorinating container through surge tank, and formaldehyde is added in a kettle, in this temperature
Lower insulation reaction 25h；The dichloro pinacoline that reaction generates is subjected to room temperature cooling and obtains dichloro pinacoline finished product；
S5: the processing of by-product: the excessive chlorine and byproduct hydrogen chloride that the synthesis of dichloro pinacoline is passed through in S4 first pass through
After water is absorbed, dilute hydrochloric acid is obtained；Again excessive chlorine and byproduct hydrogen chloride absorb by liquid alkaline and be handled.
In step S2 after 2- chlorine isopentane is pumped into condensation reaction kettle by front pump, before opening stirring, open
The hydrogen chloride that reaction generates is absorbed hydrochloric acid through water by absorption by Hydrochloric Acid device.
Lower layer's acid solution of S3 step is evacuated to spent acid distillation still, water is added, and acid solution and the volume ratio of water are 1:7, at 80 DEG C
It is fractionated at a temperature of~100 DEG C, the dilute hydrochloric acid after fractionation is pumped into hydrochloric acid pans, enters 70 to the crude product pinacoline that fractionation obtains
DEG C~80 DEG C of rectifier unit carries out rectifying, purity can be obtained up to >=98%, and colourless pinacoline product.
It should be understood by those skilled in the art that the present invention is not limited to the above embodiments, above-described embodiment and explanation
It is merely illustrated the principles of the invention described in book, without departing from the spirit and scope of the present invention, the present invention also has
Various changes and modifications, these changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention
It is defined by the appending claims and its equivalent thereof.
Claims (3)
1. a kind of dichloro pinacoline production technology, it is characterised in that: specific production technology is as follows:
The preparation of S1:2- chlorine isopentane: technical hydrochloric acid is cooled to -5 DEG C~5 DEG C, 0 DEG C~3 DEG C are slowly added dropwise under stirring condition
Iso-amylene, be added dropwise, stir 1~3 hour, generate 2- chlorine isopentane；
S2: the synthesis of pinacoline: the 2- chlorine isopentane that step S1 is generated is pumped into condensation reaction kettle by front pump, then
Stirring is opened, while slowly heating, when gas phase temperature reaches 70 DEG C~80 DEG C, starts that first is slowly added dropwise into condensation reaction kettle
Aldehyde is added dropwise, and insulation reaction 1~2 hour, after reaction, cooling, stratification；
S3: the rectifying of pinacoline: upper layer crude product pinacoline carries out rectifying, lower layer's acid solution into 90 DEG C~100 DEG C of rectifier unit
Spent acid distillation still is evacuated to be fractionated；
S4: the synthesis of dichloro pinacoline: the pinacoline after rectifying is put into chlorinating container after metering, chlorine heating
Device is warming up to 75 DEG C, and chlorine is excessively passed into chlorinating container through surge tank, and formaldehyde is added in a kettle, in this temperature
Lower insulation reaction 25h；The dichloro pinacoline that reaction generates is subjected to room temperature cooling and obtains dichloro pinacoline finished product；
S5: the processing of by-product: the excessive chlorine and byproduct hydrogen chloride that the synthesis of dichloro pinacoline is passed through in S4 first pass through
After water is absorbed, dilute hydrochloric acid is obtained；Again excessive chlorine and byproduct hydrogen chloride absorb by liquid alkaline and be handled.
2. a kind of dichloro pinacoline production technology according to claim 1, it is characterised in that: in 2- chlorine in the step S2
After isopentane is pumped into condensation reaction kettle by front pump, before opening stirring, absorption by Hydrochloric Acid device is opened, reaction is generated
Hydrogen chloride absorb hydrochloric acid through water.
3. a kind of dichloro pinacoline production technology according to claim 1, it is characterised in that: lower layer's acid of the S3 step
Liquid is evacuated to spent acid distillation still, water is added, and acid solution and the volume ratio of water are 1:7,80 DEG C~100 DEG C at a temperature of be fractionated, point
Dilute hydrochloric acid after evaporating is pumped into hydrochloric acid pans, carries out to the crude product pinacoline that fractionation obtains into 70 DEG C~80 DEG C of rectifier unit
Rectifying can obtain purity and reach >=98%, and colourless pinacoline product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811509427.9A CN109574816A (en) | 2018-12-11 | 2018-12-11 | A kind of dichloro pinacoline production technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811509427.9A CN109574816A (en) | 2018-12-11 | 2018-12-11 | A kind of dichloro pinacoline production technology |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109574816A true CN109574816A (en) | 2019-04-05 |
Family
ID=65928908
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811509427.9A Pending CN109574816A (en) | 2018-12-11 | 2018-12-11 | A kind of dichloro pinacoline production technology |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109574816A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110452108A (en) * | 2019-08-14 | 2019-11-15 | 南通鸿富达利化工有限公司 | A kind of pinacoline production product separating technique |
| CN111484401A (en) * | 2020-04-07 | 2020-08-04 | 南通利奥化工科技有限公司 | Production process for improving conversion rate of dichloropinacolone |
| CN111517935A (en) * | 2020-03-27 | 2020-08-11 | 南通利奥化工科技有限公司 | Refining process for increasing content of dichloropinacolone |
| CN116789537A (en) * | 2023-06-30 | 2023-09-22 | 江苏嘉晟化工科技有限公司 | Method for preparing 1, 1-dichloro pinacolone compound |
| CN116789538A (en) * | 2023-06-30 | 2023-09-22 | 江苏嘉晟化工科技有限公司 | Method for preparing 1, 1-dichloro pinacolone compound |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105503550A (en) * | 2015-12-29 | 2016-04-20 | 东南大学 | Green preparation method for compounding pinacolone |
| CN106397150A (en) * | 2016-08-26 | 2017-02-15 | 张家港市振方化工有限公司 | Preparation method of pinacolone |
| CN107628935A (en) * | 2017-09-27 | 2018-01-26 | 南通利奥化工科技有限公司 | A kind of production method of dichloro pinacoline |
| CN108191621A (en) * | 2018-02-01 | 2018-06-22 | 南通鸿富达利化工有限公司 | A kind of preparation process of pinacoline |
-
2018
- 2018-12-11 CN CN201811509427.9A patent/CN109574816A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105503550A (en) * | 2015-12-29 | 2016-04-20 | 东南大学 | Green preparation method for compounding pinacolone |
| CN106397150A (en) * | 2016-08-26 | 2017-02-15 | 张家港市振方化工有限公司 | Preparation method of pinacolone |
| CN107628935A (en) * | 2017-09-27 | 2018-01-26 | 南通利奥化工科技有限公司 | A kind of production method of dichloro pinacoline |
| CN108191621A (en) * | 2018-02-01 | 2018-06-22 | 南通鸿富达利化工有限公司 | A kind of preparation process of pinacoline |
Non-Patent Citations (2)
| Title |
|---|
| 道兴: "频哪酮的合成方法", 《农药译丛》 * |
| 顾先涛: "频哪酮绿色合成工艺研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110452108A (en) * | 2019-08-14 | 2019-11-15 | 南通鸿富达利化工有限公司 | A kind of pinacoline production product separating technique |
| CN111517935A (en) * | 2020-03-27 | 2020-08-11 | 南通利奥化工科技有限公司 | Refining process for increasing content of dichloropinacolone |
| CN111484401A (en) * | 2020-04-07 | 2020-08-04 | 南通利奥化工科技有限公司 | Production process for improving conversion rate of dichloropinacolone |
| CN116789537A (en) * | 2023-06-30 | 2023-09-22 | 江苏嘉晟化工科技有限公司 | Method for preparing 1, 1-dichloro pinacolone compound |
| CN116789538A (en) * | 2023-06-30 | 2023-09-22 | 江苏嘉晟化工科技有限公司 | Method for preparing 1, 1-dichloro pinacolone compound |
| CN116789538B (en) * | 2023-06-30 | 2024-01-30 | 江苏嘉晟化工科技有限公司 | Method for preparing 1, 1-dichloro pinacolone compound |
| CN116789537B (en) * | 2023-06-30 | 2024-01-30 | 江苏嘉晟化工科技有限公司 | Method for preparing 1, 1-dichloro pinacolone compound |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109574816A (en) | A kind of dichloro pinacoline production technology | |
| CN106278850B (en) | The synthetic method of the chloro- 1- acetylcyclopropanes of prothioconazoles intermediate 1- | |
| CN112047825A (en) | Production process of dichloro pinacolone | |
| CN104592116B (en) | 1,3,5-trisubstituted pyrazole compounds, and preparation method and application thereof | |
| CN108191621A (en) | A kind of preparation process of pinacoline | |
| CN105131028A (en) | Preparation method of methyl triethoxysilane | |
| CN106220629A (en) | A kind of preparation method of diquat dibromide two villaumite | |
| CN107473949A (en) | A kind of synthesis technique of the pentanone of 3,5 dichloro 2 | |
| CN102304024B (en) | Method for synthesizing difluoroethanol | |
| CN109678682A (en) | A kind of technique absorbing pinacoline production tail gas reproduction pinacoline using concentrated hydrochloric acid | |
| CN104892586A (en) | Novel method for preparing triglycidyl isocyanurate | |
| CN106380450B (en) | A kind of preparation method of low energy consumption glyoxaline ion liquid | |
| CN109180450A (en) | A kind of preparation method of methyl heptenone | |
| CN109369342A (en) | A kind of preparation method of high puring aluminium isopropoxide | |
| CN107311838A (en) | A kind of method of new synthesis Cyclopropyl Bromide | |
| CN105175218A (en) | Preparation method of dichloro-p-xylene cyclic dimer | |
| CN111484401A (en) | Production process for improving conversion rate of dichloropinacolone | |
| CN105801335B (en) | A kind of 1,2 2 fluoro- 1,2 dichloroethylene synthesis technologies | |
| CN104230662A (en) | Preparation method of high-purity 5N aluminum isopropoxide | |
| CN103204828B (en) | Preparation method of 1-cyclohexyl-1-phenyl-3-piperidinepropanol hydrochloride | |
| CN106866425A (en) | A kind of green synthesis method of bromo aromatic amine and α bromo aromatic ketones | |
| CN102206155A (en) | Method for synthesizing ethyl 4,4-difluoroacetoacetate | |
| CN106748628B (en) | A kind of method that low temperature continuous chlorination prepares mixed-chlorotoluene | |
| CN106008241A (en) | Synthesis method for N,N-dimethylaminoethyl acrylate | |
| CN111718366A (en) | Preparation method of tetravinylsilane |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190405 |