Free sample Diiodomethane CAS 75-11-6

Free sample Diiodomethane CAS 75-11-6

Diiodomethane or methylene iodide, commonly abbreviated “MI”, is an organoiodine compound. Diiodomethane is a colorless liquid; however, it decomposes upon exposure to light liberating iodine, which colours samples brownish. It is slightly soluble in water, but soluble in organic solvents. It has a relatively high refractive index of 1.741, and a surface tension of 0.0508 N·m−1.

Physicochemical properties

Appearance and traits: light yellow or gold liquid, with a smell like chloroform
Density: 3.325 g/mL at 25 °C (lit.)
Melting point: 6 °C
Boiling point: 67-69 °C 11 mm Hg (lit.)
Flash point: 181°C
Refractive index: 1.737
Water solubility: 14 g/L (20 oC)
Stability: Stable. Incompatible with strong oxidizing agents, strong bases. Reacts violently with alkali metal salts. May discolour on exposure to light.
Storage conditions: warehouse ventilated low temperature drying, separate storage with oxidants, food additives
Steam density: 9.25 (vs air)

production method
1. Obtained from the bromination of hexanediol: In a 500 mL flask with a reflux condenser, 58 g of 1,6-hexanediol and 6.84 g of red phosphorus were added. The mixture was heated to 100-150°C with stirring, and 80 g of bromine was added dropwise. After the addition was complete, stirring was continued at this room temperature for 1 h. The reaction was cooled to room temperature and diluted with water. Add 100 mL of ether and filter off excess red phosphorus. The dibromide solution in diethyl ether was separated and washed sequentially with 10% sodium sulfate solution and water. Dry with anhydrous calcium chloride. Distilling off the ether, vacuum distillation, collecting 114 ~ 115 ° C (1.6kPa) fractions, to obtain the finished product 85g, the yield was 71%.1. Prepare bromoacetic acid by reacting bromine with acetic acid and acetic anhydride in pyridine, and then react with bromoacetic acid and ethanol in the presence of sulfuric acid to form ethyl bromoacetate. It is generally prepared in two steps. 1 Preparation of bromoacetic acid: 3L glacial acetic acid and 100mL acetic anhydride were added to the flask, and 15g of red phosphorus or 70g of phosphorus tribromide was added, heated to 100°C with stirring, and 300mL (900g, 5.6mol) was slowly dropped from the separating funnel. ) Bromide, the reaction has an induction process, do not add too fast, so as to avoid sudden reactions. After the start of the reaction (with HBr released), maintain a temperature between 90°C and 100°C, and slowly add 2.0L of bromine (2.3L in total, 41 mol). After the addition, continue stirring and heating to turn the brown-red liquid into orange red. Since then, it has rarely been released. Unreacted acetic acid was recovered to a distillation temperature of 140°C and approximately 1L was recovered for the next synthesis. 2Esterification: The crude bromoacetic acid was poured into another 10L flask, 5L of industrial ethanol and 200 mL of sulfuric acid were added, refluxed on a boiling water bath for 12 hours, ethanol was recovered, washed with saturated brine three times, and dried after drying over anhydrous sodium sulfate. , collect 154 ~ 158 ° C distillate, get 2.4 ~ 2.6kg.1. Iodoform, sodium arsenite method first with arsenic trioxide and liquid base reaction, preparation of sodium arsenite, and then mixed with iodoform, sodium arsenite solution, heated to 60 ~ 65 °C under stirring, and then added Sodium reacted in one step to produce diiodomethane. The reaction product is washed, distilled, decolorized, crystallized, separated and dried to obtain a finished product.
2. Iodoform method Obtained by the action of sodium acetate, the reaction formula is as follows: After the above reaction is completed, the finished product is obtained through distillation.
3. Phase transfer catalyst synthesis method Triethyl benzyl ammonium chloride as a catalyst, derived from the reaction of dichloromethane and sodium iodide, the reaction formula is as follows:
use
Mainly used for organic synthesis and the separation of mixed minerals.
(2) 220 g (1.58 mol), 155 mL of anhydrous ethanol (2.66 mol), 240 mL of toluene and 1 mL of concentrated sulfuric acid, and zeolite was further added. Heat reflux, water, toluene, ethanol layered in the water separator, toluene back to the reaction flask, the lower layer, about collected 75mL. Ethanol 20 mL was added and reflux reaction was continued for 0.5 h. Evaporate ethanol and toluene as much as possible. The reaction was poured into water and allowed to stand for delamination. Separate the aqueous layer, and then washed with 5% sodium bicarbonate and water, dried over anhydrous sodium sulfate, fractionally distilled, and collect the distillate from 164 to 168°C to obtain ethyl bromoacetate.

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Product expansion

1> Cosmetic Raw Materials: Cosmetics is a variety of raw materials through a reasonable deployment of processing from the compound mixture. Cosmetics with a wide range of raw materials, different performance. According to the raw material properties and uses of cosmetics, can be divided into matrix materials and auxiliary raw materials in two categories. The former is a class of cosmetics in the main raw materials, cosmetics in the possession of a large proportion of the cosmetics play a major role in the role of the material. The latter is the formation of cosmetics, stability or to give color, smell and other characteristics of the role of these substances in the cosmetic formula is not used, but it is extremely important. Cosmetics are natural, synthetic or extracted from the role of different substances as raw materials, by heating, mixing and emulsification and other production processes processed from the chemical mixture.

2> Active Pharmaceutical Ingredients(API): API refers to the raw materials in the production of various types of preparations, which is the active ingredient in powder,crystal and paste for medicine use through chemical synthesis,plant extract, and preparations of biotechnology institute.It is one substance or mixture during the medicine making period, it can not be taken directly by patients.

3> Fragrance And Spices: Spice is a substance that can be scented by smelling or scented by taste, and is the raw material for the preparation of the fragrance. Spices are an important part of fine chemicals, it is composed of natural spices, synthetic spices and single fragrance.

4> Organic Raw Material: Intermediates are also known as organic intermediates. The use of coal tar or petroleum products as raw materials to produce dyes, pesticides, pharmaceuticals, resins, additives, and other intermediates.

5> Chemicals Used In Paints: Paint, the traditional Chinese name is paint. So-called coating is coated on the surface of the object that be protected or be adornment, and with the continuous film coating to form strong adhesion, usually in resin, or oil, or emulsion is given priority to, add or not add pigment, filler, add the corresponding additives, organic solvents or water preparation of viscous liquid.