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Method for purifying behenyl polyoxyethylene ether methacrylate by extraction

A technology of polyoxyethylene ether methacrylate and behenyl alcohol, applied in chemical instruments and methods, solvent extraction, separation methods, etc., can solve the problem of undiscovered BEM pure product sale, unpurified BEM, etc. problem, to achieve the effect of low cost, easy realization and simple operation

Active Publication Date: 2015-02-04
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no report on the method of purifying BEM from SIPOMER BEM at home and abroad, and no pure BEM is found for sale.

Method used

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  • Method for purifying behenyl polyoxyethylene ether methacrylate by extraction
  • Method for purifying behenyl polyoxyethylene ether methacrylate by extraction
  • Method for purifying behenyl polyoxyethylene ether methacrylate by extraction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Use the following method to purify SIPOMER BEM, the steps are:

[0033] 1. Neutralization of methacrylic acid in SIPOMER BEM with alkaline saturated aqueous solution

[0034] Weigh 10g of SIPOMER BEM produced by Rhodia, which contains about 2.3g of methacrylic acid, add 250mL of saturated aqueous sodium bicarbonate solution to it, and mix well until the system no longer produces obvious bubbles. This system is called mixture I.

[0035] 2. BEM in mixture I was extracted with chloroform

[0036] Pour the mixture into a separatory funnel, add 100 mL of chloroform to the separatory funnel, extract the BEM in the mixture I, repeat 5 times, and collect the organic phase.

[0037] 3. Extraction of sodium methacrylate in the organic phase with a saturated aqueous solution of alkali

[0038] Add 100 mL of saturated aqueous sodium bicarbonate solution into the separatory funnel with the organic phase, repeat 3 times, and further remove the sodium methacrylate in the organic...

Embodiment 2

[0049]Adopt the method for embodiment 1 to purify SIPOMER BEM, difference is: the alkaline solution used in step 1 and 3 is saturated sodium carbonate aqueous solution, and the organic solvent used in step 2 is carbon tetrachloride, and the pure product purity of gained BEM is 98.4% , the yield is 93.8%.

Embodiment 3

[0051] Use the following method to purify SIPOMER BEM, the steps are:

[0052] 1. Neutralization of methacrylic acid in SIPOMER BEM with alkaline saturated aqueous solution

[0053] Weigh 10g of SIPOMER BEM produced by Rhodia, which contains about 2.3g of methacrylic acid, add 250mL of saturated aqueous solution of sodium bicarbonate to it, and mix well until the system no longer produces obvious bubbles. This system is called mixture I.

[0054] 2. BEM in mixture I was extracted with chloroform

[0055] Pour the mixture into a separatory funnel, add 75 mL of chloroform to the separatory funnel, extract the BEM in the mixture I, repeat 5 times, and collect the organic phase.

[0056] 3. Extraction of sodium methacrylate in the organic phase with a saturated aqueous solution of alkali

[0057] Add 25 mL of saturated aqueous sodium bicarbonate solution into the separatory funnel with the organic phase, repeat 5 times, and further remove the sodium methacrylate in the organi...

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PUM

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Abstract

The invention discloses a method for purifying behenyl polyoxyethylene ether methacrylate by extraction. The method includes steps of neutralizing methacrylic acid impurities contained in a raw material which is the commercially available behenyl polyoxyethylene ether methacrylate by alkaline aqueous solution into salt; extracting a mixture by organic solvents and collecting organic phases; extracting the organic phases by alkaline aqueous solution; further removing methacrylate remained in the organic phases; finally drying the organic phases; and removing the organic solvents by reduced pressure distillation to obtain a pure product. The pure BEM (behenyl polyoxyethylene ether methacrylate) product can be obtained via the conventional steps, and the method has the advantages that operation is simple, implementation is easy, the purification effect is good, cost is low, and environmental pollution is prevented.

Description

technical field [0001] The invention relates to a method for purifying BEM (i.e. behenyl alcohol polyoxyethylene ether methacrylate), in particular to purifying behenyl alcohol polyoxyethylene ether methyl methacrylate through simple neutralization and extraction steps. acrylate method. Background technique [0002] Behenyl alcohol polyoxyethylene ether methacrylate may be referred to as BEM for short, and its structural formula is shown in Formula 1. The compound contains a double bond, a polyoxyethylene long chain and a polyalkylene non-ionic group. Behenyl alcohol polyoxyethylene ether methacrylate trade name is SIPOMER BEM, which is currently produced by Rhodia Corporation of the United States. It is a compound of BEM, water and methacrylic acid, and the water content is about 25.0-27.0%. The base acrylic acid content is about 22.0-24.0%. [0003] [0004] Formula I: BEM structural formula and H in different chemical environments in the formula [0005] BEM can be...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D11/00
Inventor 关瑞芳周传健
Owner UNIV OF JINAN