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Separation method of water-soluble polymer with tetrahydrofuran as extracting agent

A water-soluble polymer and tetrahydrofuran technology, applied in the direction of liquid solution solvent extraction, etc., can solve the problems of complicated operation and high cost, and achieve the effect of good solubility and easy removal

Inactive Publication Date: 2014-09-24
SHANGHAI UNIVERSITY OF ELECTRIC POWER
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to propose a separation and purification method for extracting water-soluble polymers in order to solve the technical problems of high cost and complicated operation in the separation and purification process of the above-mentioned water-soluble polymer products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Extraction of Polycitric Acid from Mother Liquor of Sulfuric Acid Catalyzed Polymerization of Citric Acid

[0027] In addition to polycitric acid, the citric acid polymerization reaction mother liquor also contains small molecular impurities such as tetrahydrofuran, citric acid, and sulfuric acid.

[0028] At 20~30°C, use 10mL of citric acid polymerization reaction mother liquor with 45mL of 10% sodium hydroxide aqueous solution to adjust the pH to be neutral, then add 5mL of water and 5 grams of sodium sulfate solid to the solution to form sodium sulfate Solution, wherein the mass percent concentration of sodium sulfate is 20%;

[0029] Then, add 40mL tetrahydrofuran to the sodium sulfate solution obtained above, shake and let it stand for 5min, the solution is divided into two layers, the upper layer is an organic phase-tetrahydrofuran phase, and the lower layer is an aqueous phase-a sodium sulfate aqueous solution;

[0030] The amount of tetrahydrofuran added above ...

Embodiment ２

[0034] Extraction of Polycitric Acid from Mother Liquor of Sulfuric Acid Catalyzed Polymerization of Citric Acid

[0035] At 20~30°C, use 10mL of citric acid polymerization reaction mother liquor with 45mL of 10% sodium hydroxide aqueous solution to adjust the pH to be neutral, then add 35mL of water and 1 gram of sodium sulfate to the solution to form a sodium sulfate solution , wherein the mass percent concentration of sodium sulfate is 10%.

[0036] Then, add 10mL tetrahydrofuran to the sodium sulfate solution obtained above, shake and let it stand for 10min, the solution is divided into two layers, the upper layer is an organic phase-tetrahydrofuran phase, and the lower layer is an aqueous phase-a sodium sulfate aqueous solution;

[0037] The amount of tetrahydrofuran added above is calculated by volume ratio, that is, sodium sulfate solution: tetrahydrofuran is 1:0.25;

[0038] Finally, the tetrahydrofuran phase obtained above is separated by a separatory funnel, and the...

Embodiment 3

[0041] Extraction of Polycitric Acid from Mother Liquor of Sulfuric Acid Catalyzed Polymerization of Citric Acid

[0042] At 20~30°C, adjust 10mL of citric acid polymerization reaction mother liquor with 45mL of 10% sodium hydroxide aqueous solution to adjust the pH value to be neutral, and then add 16 grams of sodium sulfate to the solution to form a sodium sulfate solution. The mass percentage concentration of sodium is 35%.

[0043] Then, add 80mL tetrahydrofuran to the sodium sulfate solution obtained above, shake and let it stand for 10min, the solution is divided into two layers, the upper layer is an organic phase-tetrahydrofuran phase, and the lower layer is an aqueous phase-a sodium sulfate aqueous solution;

[0044] The amount of tetrahydrofuran added above is calculated by volume ratio, that is, sodium sulfate solution: tetrahydrofuran is 1:2;

[0045] Finally, the tetrahydrofuran phase obtained above is separated by a separatory funnel, and then the separated tetr...

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Abstract

The invention discloses a separation method of a water-soluble polymer with tetrahydrofuran as an extracting agent. The preparation method comprises the following steps: firstly, at temperature of 20-30 DEG C, adjusting a pH value of a reaction solution containing a water-soluble polymer, obtained through a polymerization reaction, to be neutral, adding sulfate to the reaction solution to form a sulfate solution; adding tetrahydrofuran to the obtained sulfate solution, calculating according to a volume ratio, i.e. a ratio of the sulfate solution to the tetrahydrofuran of 1:(0.25-2); standing and demixing after oscillating, wherein the upper layer is an organic-phase tetrahydrofuran phase, the lower layer is a water phase-phase sulfate solution; then separating the obtained tetrahydrofuran by using a separating funnel to obtain a tetrahydrofuran solution rich in water-soluble polymer, performing reduced pressure distillation in a water bath with temperature of 50-70 DEG C by using a rotary evaporator, and evaporating a tetrahydrofuran solvent to obtain the water-soluble polymer, thus realizing the separation of the water-soluble polymer with the tetrahydrofuran as the extracting agent.

Description

technical field [0001] The invention belongs to the technical field of separation and purification of water-soluble polymers, in particular to a method for separating water-soluble polymers using tetrahydrofuran as an extraction agent. Background technique [0002] Water-soluble polymers usually use water as a solvent during the preparation process, and small molecular substances such as initiators, stabilizers, and molecular weight modifiers added during the reaction are also mostly soluble in water. In addition, adjusting the pH value before and after polymerization will also introduce water-soluble small molecular substances such as salts. Therefore, after the end of the polymerization reaction, in addition to macromolecular products, small molecular impurities such as initiator or catalyst residues, surfactants, stabilizers, and unreacted monomers will also exist in the reaction solution. [0003] Both macromolecular products and small molecular impurities are water-sol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D11/04C08G63/06C08G63/90C08G65/00
Inventor 赵玉增刘快迎马利纳葛红花朱雁萍胡信雅
Owner SHANGHAI UNIVERSITY OF ELECTRIC POWER
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