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High-purity grade diiodomethane purifying method used for photovoltaic material

A diiodomethane and purification method technology, applied in chemical instruments and methods, disproportionation separation/purification of halogenated hydrocarbons, organic chemistry, etc., can solve problems such as unworthy promotion, large environmental impact, cumbersome operation, etc., and achieve stable product quality , Yield improvement, simple operation

Active Publication Date: 2015-02-04
TAICANG HUSHI REAGENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In the prior art, the usual purification method of high-purity diiodomethane is to stir with dilute sodium thiosulfate solution or sodium bisulfate solution, then wash with water, dilute sodium carbonate solution and more water respectively, and finally dry with calcium chloride And distill to obtain the final product, the disadvantage is that the operation is cumbersome, and the washing process has a great impact on the environment, so it is not worth promoting

Method used

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  • High-purity grade diiodomethane purifying method used for photovoltaic material

Examples

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Effect test

Embodiment 1

[0023] (1) Preparation of modified 2-acrylamide-2-methylpropanesulfonic acid copolymer adsorption column:

[0024] Take 100g of sodium carbonate, add 1750ml of pure water, 150ml of diisooctyl phthalate, and 500ml of ethyl acetate, add 500g of 2-acrylamide-2-methylpropanesulfonic acid to the dipping solution at room temperature, and then immerse for 15h After filtering, washing twice with 500ml of 18.2MΩ·cm ultrapure water, drying at 105°C for 12h, 553g of modified 2-acrylamide-2-methylpropanesulfonic acid copolymer is obtained, which is packed in a column and ready for use.

[0025] (2) Purification of diiodomethane:

[0026] 1000g of industrial grade diiodomethane raw material with a content of 95.0wt% is adsorbed through an adsorption column containing a modified 2-acrylamide-2-methylpropanesulfonic acid copolymer medium at a temperature of 0.22MPa and 20°C, and the filtrate is purified by quartz The rectification device removes the front distillate under the vacuum condition of -...

Embodiment 2

[0028] (1) Preparation of modified 2-acrylamide-2-methylpropanesulfonic acid copolymer adsorption column: Take 150g of sodium carbonate, add 2000ml of pure water, 200ml of diisooctyl phthalate, and 750ml of ethyl acetate. Add 500g of 2-acrylamide-2-methylpropanesulfonic acid to the dipping solution at room temperature, immerse for 17.5h, filter, wash twice with 600ml of 18.2MΩ·cm ultrapure water, and dry at 105°C for 12h, that is 561 g of modified 2-acrylamide-2-methylpropanesulfonic acid copolymer was obtained, which was packed in a column for use.

[0029] (2) Purification of diiodomethane:

[0030] 1000g of industrial grade diiodomethane raw material with a content of 95.0wt% is adsorbed through an adsorption column containing a modified 2-acrylamide-2-methylpropanesulfonic acid copolymer medium at a temperature of 0.17MPa and 23°C, and the filtrate is purified by quartz The distillation device removes the front distillate under the vacuum condition of -0.085MPa, and collects t...

Embodiment 3

[0032] (1) Preparation of modified 2-acrylamide-2-methylpropanesulfonic acid copolymer adsorption column:

[0033] Take 200g of potassium carbonate, add 2250ml of pure water, 250ml of diisooctyl phthalate, and 1000ml of ethyl acetate, add 500g of 2-acrylamide-2-methylpropanesulfonic acid to the dipping solution at room temperature. After immersing for 20 hours After filtering, washing twice with 700ml of 18.2MΩ·cm ultrapure water, drying at 105°C for 12h, 583g of modified 2-acrylamide-2-methylpropanesulfonic acid copolymer is obtained, which is packed in column and ready for use.

[0034] (2) Purification of methyl iodide:

[0035] 1000g of industrial grade diiodomethane raw material with a content of 95.0wt% is adsorbed through an adsorption column containing a modified 2-acrylamide-2-methylpropanesulfonic acid copolymer medium at a temperature of 0.12MPa and 20°C, and the filtrate is purified by quartz The rectification device removes the front fraction under the vacuum condition ...

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Abstract

The invention discloses a high-purity grade diiodomethane purifying method used for photovoltaic material used for a photovoltaic material. The method comprises the following steps: 1)an industrial grade diiodomethane raw material is absorbed by passing through an adsorption column equipped with modified 2-acrylamide-2-methul propanesulfonic acid copolymer medium to obtain a filtrate; 2)passing a filtrate through a quartz purification and rectification apparatus, under vacuum condition, removing preceding fraction, collecting a distillation fluid; and 3)filtering and processing the distillation fluid to obtain the high-purity grade diiodomethane used for photovoltaic material. According to the invention, the modified 2-acrylamide-2-methul propanesulfonic acid copolymer medium is employed for column adsorption, and has strong adsorption capability to impurity ions in a solution, and has strong adsorption capability to hydroxy impurity, free iodine, moisture, and metal ions in industrial grade diiodomethane, and impurity can be effectively removed. According to the invention, the purifying process operation is simple, cost is reduced, yield is increased, and the obtained product quality is stable.

Description

Technical field [0001] The invention relates to the technical field of diiodomethane, in particular to a method for purifying high-purity diiodomethane for photovoltaic materials. Background technique [0002] Diiodomethane, also known as methylene iodide, is colorless and clear to light yellow heavy liquid, molecular weight 267.87, flash point 110℃, melting point 6℃, boiling point 181℃, decomposes, insoluble in water, soluble in ethanol, ether, benzene, Most organic solvents such as chloroform have relative density (water = 1) 3.32; relative density (air = 1) 9.25, stable, and are mainly used for organic synthesis and separation of mixed minerals. [0003] In the prior art, the usual purification method of high-purity diiodomethane is to stir with dilute sodium thiosulfate solution or sodium bisulfate solution, then wash with water, dilute sodium carbonate solution and more water, and finally dry with calcium chloride The final product is obtained by distillation. The disadvantag...

Claims

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Application Information

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IPC IPC(8): C07C19/07C07C17/38C07C17/389
Inventor 王永旗郑琦王伟吕明
Owner TAICANG HUSHI REAGENT
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