CN102295519A - Preparation method for iodomethane - Google Patents
Preparation method for iodomethane Download PDFInfo
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- CN102295519A CN102295519A CN2011102107635A CN201110210763A CN102295519A CN 102295519 A CN102295519 A CN 102295519A CN 2011102107635 A CN2011102107635 A CN 2011102107635A CN 201110210763 A CN201110210763 A CN 201110210763A CN 102295519 A CN102295519 A CN 102295519A
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- Prior art keywords
- phosphoric acid
- iodomethane
- solid phosphoric
- acid catalyst
- methyl alcohol
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- 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
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Abstract
The invention discloses a preparation method for iodomethane. According to the invention, methanol and potassium iodide are used as raw materials and are subjected to an exchange reaction in the presence of a solid phosphoric acid catalyst, and the object product, iodomethane, is collected from an organic phase. The purity of iodomethane obtained by the method provided in the invention is more than 98%, and yield of iodomethane is more than 80%. Compared to the prior art, solid phosphoric acid is used as a catalyst to substitute strong acid in the invention, which enables reaction yield to be effectively improved, and the solid phosphoric acid catalyst can be recycled for cyclic utilization, thereby reducing production cost; potassium iodide is used as a raw material to substitute iodine or dimethyl sulphate used in the prior art, which is beneficial for environmental protection; the preparation method in the invention has the characteristics of simple operation, stable product quality and high purity, and is applicable to continuous production.
Description
Technical field
The present invention relates to a kind of preparation method of methyl iodide, particularly a kind of method for preparing methyl iodide with solid phosphoric acid catalyst.
Background technology
Methyl iodide is an iodine substituent of methane, in organic synthesis, be commonly used for methylating reagent, the intermediate of organic synthesis, because iodide ion is good leavings group, can be used as the good initiator of grignard reaction, be used to cause inactive halides such as chlorinated aromatic hydrocarbons, also can be used as sterilant, weedicide, agrochemical, be widely used industrial.
In the prior art, be raw material, under lead tetraacetate catalysis, react that prepare methyl iodide, this method yield is higher, but catalyzer costs an arm and a leg with acetate and iodine, and very big to the influence of environment.Zhejiang Polytechnical University's journal 2008,36 (6): disclosed among the 619-621 and a kind ofly obtained the method for methyl iodide, this method convenient post-treatment, good product purity with methyl-sulfate and potassiumiodide prepared in reaction, but the reactant methyl-sulfate is highly toxic product, easily operator is damaged.The document has reported that simultaneously with methyl alcohol and potassiumiodide be raw material, adds the acid catalyst reaction and obtains methyl iodide, and this method yield is low, and the acid that is added can't be reclaimed, and environment is also had very big influence.
Summary of the invention
The technical problem that the present invention solves is to provide a kind of preparation method of methyl iodide, and to overcome catalyzer valency height in the prior art, reactant toxicity is big, and reaction yield is low, difficult solvent recovery, the irretrievable deficiency of acid catalyst.
Technical conceive of the present invention is such: with methyl alcohol, potassiumiodide is a raw material, carries out permutoid reaction in the presence of solid phosphoric acid catalyst, collects target product then from reaction solution.
Method of the present invention comprises the steps:
Methyl alcohol in the presence of solid phosphoric acid catalyst, 50-60 ℃, add potassiumiodide in 0.5 hour in batches, reaction is 3-5 hour under nitrogen pressure 0.1-0.5MPa, reaction solution is cooled to room temperature, filters, and adds sherwood oil, collects target product from the organic phase of telling.
According to the present invention, the mass ratio of said methyl alcohol and solid acid is 1: 0.1-0.3, g/g, the mol ratio of said methyl alcohol and potassiumiodide is 1: 0.5-1, and mol/mol, the mass ratio of said methyl alcohol and sherwood oil are 1: 3-5, g/g, the present invention collects target product and comprises the steps: that the Calcium Chloride Powder Anhydrous drying obtains methyl iodide after the underpressure distillation through washing from the organic phase of telling.
The methyl iodide purity that obtains with preparation method of the present invention reaches more than 98%, and yield reaches more than 80%.
The said solid phosphoric acid catalyst of the present invention can be according to " chemical intermediate " 2006, and the method for (2): 1-4 prepares, and the present invention repeats no more.
The present invention's beneficial effect compared with prior art:
The present invention uses solid phosphoric acid to replace traditional strong acid as catalyzer, effectively raises reaction yield, and solid phosphoric acid catalyst can reclaiming, drops into and reuses, and has reduced production cost; Adopting potassiumiodide is that raw material replaces used iodine or methyl-sulfate in the traditional mode of production, is beneficial to environmental protection; The present invention is simple to operate, constant product quality, and the purity height is suitable for serialization production.
Embodiment
The invention will be further described below by embodiment, but embodiment does not limit protection scope of the present invention.
Embodiment 1
In the reactor that has heating, stirring, thermometer, add 320g methyl alcohol successively, the 32g solid phosphoric acid catalyst, heat temperature raising to 50 under stirring ± 2 ℃ added potassiumiodide 830g in batches in 0.5 hour, uniform temp is pushed down into nitrogen to 0.1Mpa, reacts 3 hours.Reaction solution is cooled to room temperature, removes by filter catalyzer (reclaim and concentrate, reuse); Add the 960g sherwood oil, tell petroleum ether layer, with the 1000mL washing, after the Calcium Chloride Powder Anhydrous drying, underpressure distillation obtains light yellow liquid product iodine methane 616.7g, and yield is 86.86%, purity 98.1% (chemical analysis).
Embodiment 2
In the reactor that has heating, stirring, thermometer, add 320g methyl alcohol successively, the 64g solid phosphoric acid catalyst, heat temperature raising to 55 under stirring ± 2 ℃ added potassiumiodide 1162g in batches in 0.5 hour, uniform temp is pushed down into nitrogen to 0.3Mpa, reacts 4 hours.Reaction solution is cooled to room temperature, removes by filter catalyzer (reclaim and concentrate, reuse); Add the 1280g sherwood oil, tell petroleum ether layer, with the 1000ml washing, after the Calcium Chloride Powder Anhydrous drying, underpressure distillation obtains light yellow liquid product iodine methane 884.56g, and yield is 88.99%, purity 98.7% (chemical analysis).
Embodiment 3
In the reactor that has heating, stirring, thermometer, add 320g methyl alcohol successively, the 96g solid phosphoric acid catalyst, heat temperature raising to 60 under stirring ± 2 ℃ added potassiumiodide 1660g in batches in 0.5 hour, uniform temp is pushed down into nitrogen to 0.5Mpa, reacts 5 hours.Reaction solution is cooled to room temperature, removes by filter catalyzer (reclaim and concentrate, reuse); Add the 960g sherwood oil, tell petroleum ether layer, with the 1000ml washing, after the Calcium Chloride Powder Anhydrous drying, underpressure distillation obtains light yellow liquid product iodine methane 1178.94g, and yield is 83.02%, purity 99.1% (chemical analysis).
Need to prove that above embodiment is only unrestricted in order to technical scheme of the present invention to be described.Although the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can make amendment or be equal to replacement the technical scheme of invention, and not break away from the scope of technical solution of the present invention, it all should be encompassed in the claim scope of the present invention.
Claims (5)
1. the preparation method of a methyl iodide is characterized in that, comprises the steps:
Methyl alcohol in the presence of solid phosphoric acid catalyst, 50-60 ℃, add potassiumiodide in 0.5 hour in batches, reaction is 3-5 hour under nitrogen pressure 0.1-0.5MPa, reaction solution is cooled to room temperature, filters, and adds sherwood oil, collects target product from the organic phase of telling.
2. method according to claim 1 is characterized in that, the mass ratio of said methyl alcohol and solid phosphoric acid catalyst is 1:0.1-0.3, g/g.
3. method according to claim 1 is characterized in that, the mol ratio of said methyl alcohol and potassiumiodide is 1:0.5-1, mol/mol.
4. method according to claim 1 is characterized in that, the mass ratio of said methyl alcohol and sherwood oil is 1:3-5, g/g.
5. method according to claim 1 is characterized in that, collects target product and comprise the steps: that the Calcium Chloride Powder Anhydrous drying obtains methyl iodide after the underpressure distillation through washing from the organic phase of telling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102107635A CN102295519A (en) | 2011-07-26 | 2011-07-26 | Preparation method for iodomethane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102107635A CN102295519A (en) | 2011-07-26 | 2011-07-26 | Preparation method for iodomethane |
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| Publication Number | Publication Date |
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| CN102295519A true CN102295519A (en) | 2011-12-28 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011102107635A Pending CN102295519A (en) | 2011-07-26 | 2011-07-26 | Preparation method for iodomethane |
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| CN (1) | CN102295519A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104326864A (en) * | 2014-10-15 | 2015-02-04 | 太仓沪试试剂有限公司 | High-purity grade diiodomethane purifying method used for photovoltaic material |
| CN104370689A (en) * | 2014-10-20 | 2015-02-25 | 太仓沪试试剂有限公司 | Purification method of high-purity iodomethane for LED (light-emitting diode) materials |
| CN108586210A (en) * | 2018-04-11 | 2018-09-28 | 深圳市前海博扬研究院有限公司 | A kind of preparation method of dimethyl ether |
| CN113831213A (en) * | 2021-10-18 | 2021-12-24 | 安徽亚格盛电子新材料有限公司 | Method for preparing ethyl iodide by recycling iodine ion-containing solution |
| CN114195616A (en) * | 2021-12-23 | 2022-03-18 | 广东先导微电子科技有限公司 | Preparation method of methyl iodide |
| CN115583957A (en) * | 2022-11-02 | 2023-01-10 | 上海上药新亚药业有限公司 | Methylation synthesis method of ceftaroline fosamil intermediate |
| CN114195616B (en) * | 2021-12-23 | 2024-04-12 | 广东先导微电子科技有限公司 | Preparation method of methyl iodide |
-
2011
- 2011-07-26 CN CN2011102107635A patent/CN102295519A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 仉霞，等: "绿色固体磷酸催化剂的研究进展", 《化工中间体》 * |
| 杨振平,等: "制备碘甲烷不同方法比较", 《浙江工业大学学报》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104326864A (en) * | 2014-10-15 | 2015-02-04 | 太仓沪试试剂有限公司 | High-purity grade diiodomethane purifying method used for photovoltaic material |
| CN104326864B (en) * | 2014-10-15 | 2016-07-06 | 太仓沪试试剂有限公司 | A kind of photovoltaic material purification process of high-purity grade of diiodomethane |
| CN104370689A (en) * | 2014-10-20 | 2015-02-25 | 太仓沪试试剂有限公司 | Purification method of high-purity iodomethane for LED (light-emitting diode) materials |
| CN104370689B (en) * | 2014-10-20 | 2016-03-30 | 太仓沪试试剂有限公司 | A kind of LED material purification process of high-purity grade of methyl iodide |
| CN108586210A (en) * | 2018-04-11 | 2018-09-28 | 深圳市前海博扬研究院有限公司 | A kind of preparation method of dimethyl ether |
| CN113831213A (en) * | 2021-10-18 | 2021-12-24 | 安徽亚格盛电子新材料有限公司 | Method for preparing ethyl iodide by recycling iodine ion-containing solution |
| CN114195616A (en) * | 2021-12-23 | 2022-03-18 | 广东先导微电子科技有限公司 | Preparation method of methyl iodide |
| CN114195616B (en) * | 2021-12-23 | 2024-04-12 | 广东先导微电子科技有限公司 | Preparation method of methyl iodide |
| CN115583957A (en) * | 2022-11-02 | 2023-01-10 | 上海上药新亚药业有限公司 | Methylation synthesis method of ceftaroline fosamil intermediate |
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Application publication date: 20111228 |