CN102020529A - Method for preparing diiodomethane - Google Patents
Method for preparing diiodomethane Download PDFInfo
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- CN102020529A CN102020529A CN200910070536XA CN200910070536A CN102020529A CN 102020529 A CN102020529 A CN 102020529A CN 200910070536X A CN200910070536X A CN 200910070536XA CN 200910070536 A CN200910070536 A CN 200910070536A CN 102020529 A CN102020529 A CN 102020529A
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- stir
- iodide
- methylene
- water layer
- standing demix
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Abstract
The invention relates to a method for preparing diiodomethane, which is characterized by comprising the following steps of: (1) reacting for synthesizing the diiodomethane; (2) washing with water; and (3) refining. The method improves product yield, meets market requirement and improves economic and social benefits of enterprises.
Description
Technical field
The present invention relates to organic compound preparation method field, particularly a kind of preparation method of methylene iodide.
Background technology
Methylene iodide is one of domestic and international bulk article, the analysis that is widely used in organic synthesis, mineral with separate, the evaluation of pyridine and the mensuration of specific refraction, be used for synthetic cyclopropane especially in a large number.At present, do not increasing sophisticated equipment and do not strengthening under the situation of operator's technical requirements, the product yield that synthesizes is not high.
Summary of the invention
The objective of the invention is to provides a kind of preparation method of methylene iodide in order to overcome the deficiencies in the prior art.
The present invention for achieving the above object, by the following technical solutions:
(1) methylene iodide building-up reactions
Sodium iodide, methylene dichloride and solvent dimethyl formamide are mixed, and the ratio of weight and number of sodium iodide and methylene dichloride is 4: 1, and sodium iodide and dimethyl formamide ratio of weight and number are 1: 1.25-1.5, stir and be heated to 100 ℃, isothermal reaction 6-8 hour;
(2) washing
A, add hypo solution in post reaction mixture, stir, standing demix discards water layer;
B, adding buck stir, and standing demix discards water layer;
C, adding clear water stir, and standing demix discards water layer;
(3) refining
Underpressure distillation gets the methylene iodide finished product.
Among the present invention, described sodium iodide, methylene dichloride, solvent dimethyl formamide are the general industry product.
Among the present invention, described reactor has heating unit, electric stirring, thermometer, water circulation condenser and water-and-oil separator.
The beneficial effect that the present invention had:
The present invention has improved product yield, has satisfied the demand in market, has improved economic benefit of enterprises and social benefit.
Embodiment
The present invention is further illustrated below in conjunction with specific embodiment.
Embodiment one:
(1) methylene iodide building-up reactions
In a reactor of 2000 milliliters that has heating unit, electric stirring, thermometer, water circulation condenser and a water-and-oil separator, drop into 800 gram sodium iodides, 200 gram methylene dichloride, 1000 gram solvent dimethyl formamides successively, stirring also is heated to 100 ℃, isothermal reaction 6-8 hour;
(2) washing
Adding concentration is 10% hypo solution 1000 grams in the mixture of reaction, stirs, and standing demix discards water layer;
Adding concentration is 5% sodium carbonate solution 1000 grams, stirs, and standing demix discards water layer;
Add clear water 1000 grams, stir, standing demix discards water layer then;
(3) refining
The reactant of washing after the neutralization is moved in the still kettle, and vacuum degree control is at the 30mmHg post, and temperature is controlled at 80 ℃, underpressure distillation, the methylene iodide finished product.
Embodiment two:
(1) methylene iodide building-up reactions
In a reactor of 2000 milliliters that has heating unit, electric stirring, thermometer, water circulation condenser and a water-and-oil separator, drop into 800 gram sodium iodides, 200 gram methylene dichloride, 1100 gram solvent dimethyl formamides successively, stirring also is heated to 100 ℃, isothermal reaction 6-8 hour.
(2) washing
Adding concentration is 10% hypo solution 1000 grams in the mixture of reaction, stirs, and standing demix discards water layer;
Adding concentration is 5% sodium carbonate solution 1000 grams, stirs, and standing demix discards water layer;
Add clear water 1000 grams, stir, standing demix discards water layer then;
(3) refining
The reactant of washing after the neutralization is moved in the still kettle, and vacuum degree control is at the 30mmHg post, and temperature is controlled at 80 ℃, underpressure distillation, the methylene iodide finished product.
Embodiment three:
(1) methylene iodide building-up reactions
In a reactor of 2000 milliliters that has heating unit, electric stirring, thermometer, water circulation condenser and a water-and-oil separator, drop into 800 gram sodium iodides, 200 gram methylene dichloride, 1200 gram solvent dimethyl formamides successively, stirring also is heated to 100 ℃, isothermal reaction 6-8 hour.
(2) washing
Adding concentration is 10% hypo solution 1000 grams in the mixture of reaction, stirs, and standing demix discards water layer;
Adding concentration is 5% sodium carbonate solution 1000 grams, stirs, and standing demix discards water layer;
Add clear water 1000 grams, stir, standing demix discards water layer then;
(3) refining
The reactant of washing after the neutralization is moved in the still kettle, and vacuum degree control is at the 30mmHg post, and temperature is controlled at 80 ℃, underpressure distillation, the methylene iodide finished product.
The above only is preferred embodiment of the present invention, is not technical scheme of the present invention is done any pro forma restriction.Every foundation technical spirit of the present invention all still belongs in the scope of technical scheme of the present invention any simple modification, equivalent variations and modification that above embodiment did.
Claims (1)
1. the preparation method of a methylene iodide is characterized in that comprising:
(1) methylene iodide building-up reactions
Sodium iodide, methylene dichloride and solvent dimethyl formamide are mixed, and the ratio of weight and number of sodium iodide and methylene dichloride is 4: 1, and sodium iodide and dimethyl formamide ratio of weight and number are 1: 1.25-1.5, stir and be heated to 100 ℃, isothermal reaction 6-8 hour;
(2) washing
A, add hypo solution in post reaction mixture, stir, standing demix discards water layer;
B, adding buck stir, and standing demix discards water layer;
C, adding clear water stir, and standing demix discards water layer;
(3) refining
Underpressure distillation gets the methylene iodide finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910070536XA CN102020529A (en) | 2009-09-23 | 2009-09-23 | Method for preparing diiodomethane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910070536XA CN102020529A (en) | 2009-09-23 | 2009-09-23 | Method for preparing diiodomethane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102020529A true CN102020529A (en) | 2011-04-20 |
Family
ID=43862352
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910070536XA Pending CN102020529A (en) | 2009-09-23 | 2009-09-23 | Method for preparing diiodomethane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102020529A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107501037A (en) * | 2017-09-08 | 2017-12-22 | 南通意特化工有限公司 | A kind of preparation method of diiodomethane |
| CN112961029A (en) * | 2021-02-02 | 2021-06-15 | 浙江肯特催化材料科技有限公司 | Preparation method of diiodomethane |
-
2009
- 2009-09-23 CN CN200910070536XA patent/CN102020529A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107501037A (en) * | 2017-09-08 | 2017-12-22 | 南通意特化工有限公司 | A kind of preparation method of diiodomethane |
| CN112961029A (en) * | 2021-02-02 | 2021-06-15 | 浙江肯特催化材料科技有限公司 | Preparation method of diiodomethane |
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| Date | Code | Title | Description |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20110420 |