The method of obtaining the ion exchange sorbent

 

(57) Abstract:

Use: production of ion exchangers for the removal of coloured organic substances from water and mud. The inventive condensation of phenol, formaldehyde and hexamethylenetetramine in sulfuric acid medium in the presence of the transducer of ethylene glycol at 60 - 75C, at a molar ratio of phenol: formaldehyde: hexamethylenetetramine: sulfuric acid: ethylene glycol, equal 1 : (0,6 - 2,0) : (0,06 - 0,24) : (0,4 - 1,9) : (2,4 - 5,7) of cured polycondensate extracted with water, ethylene glycol and sulfuric acid. After evaporation of the solution the last return in the process. Formaldehyde is used in the form of paraformaldehyde or trioxane. 2 C.p. f-crystals, 1 table.

The invention relates to the field of chemical technology and can be used in the production of anion exchange resins, which are used to remove colored organic compounds from natural water (humic acid), from various hydrolysates chemical and microbiological origin.

A known method of producing ionosorbed by condensation of metaphenylenediamine, resorcinol and formaldehyde in hydrochloric acid medium in the presence of large amounts of water. Ionosorbed Oblonsky strength, there is no true porosity, moisture reduction during storage leads to deterioration of quality.

To impart porosity, increase the mechanical strength of the sorbent and its capacity for colored organic compounds, a method for sorbent condensation of phenol and formaldehyde in the environment of ethylene glycol at pH 7-8. In the second stage of the process is administered aliphatic amine containing a primary amino group. Having good porosity (0.4 to 1.2 cm3/g), the sorbent provides a high sorption capacity in static conditions (0.7 to 1.5 mg/ml). When testing in dynamic conditions, the sorbent shows a lack of implementation capacity specified in static conditions.

Closest to the claimed is a method of producing anion exchange resins, which are co-condensation of phenol and hexamethylenetetramine, an aqueous solution of formaldehyde at 90-95aboutWith sulfate in the environment in two stages. In the first stage, carry out the condensation at a molar ratio of phenol:formaldehyde: hexamethylenetetramine: sulfuric acid: mineral salt: water= 0,095-1: (1,75-1,8):(0,37-0,38):(0,60-0,63):(0,35-0,65): (8,0-8,5) within 2 h, at the second stage, increasing the molar content of the acid up to 1,90-1,95. As mineral and the organic layers) is used to increase acidity in three times.

Obtained in this way anion exchange resin has a low porosity of 0.2-0.3 cm3/g, which is a specified way to improve it is not possible. Insufficient capacity of the anion on humus gamestm (0.6 mg/ml) in case of insufficient chemical resistance. When using water commodity resins obtained solution containing sulfuric acid, sodium chloride or potassium, formaldehyde, ammonium sulfate. This solution is almost impossible to return to the process cycle. Regeneration is the process of evaporation allows to obtain a solution containing sulfuric acid, sodium sulfate or potassium, ammonium sulfate. Such a solution cannot be reused. In addition, receive the condensate water containing hydrochloric acid, methylamine. This condensate reuse can only 1-2 times.

The aim of the invention is to increase the porosity of the sorbent, chemical stability in contact with the solutions, and the capacity of organic matter humus nature, and other colored compounds). Additionally achieves the important goal of creating zero waste.

This goal is achieved by the fact that expose cocondensate phenol and hexamethylenetetramine, formaldehyde in sulfuric acid medium at Navo, the condensation is carried out at a temperature of 60-75aboutAnd formaldehyde is used in the form of low molecular weight polymers of formaldehyde is paraformaldehyde or trioxane. The condensation is carried out at a lower relative pH of the medium in one stage, with the following molar ratio of phenol: formaldehyde: hexamethylenetetramine:sulfuric acid:ethylene glycol= 1: (0,6-2,0): (0,06-0,24):(0,6-1,9):(3,8-5,7), moreover, to ensure the waste products of the technological process glycol and sulfuric acid is extracted from the finished resin with water, and after evaporation of the resulting solution back into the process.

The invention is illustrated by the following examples.

P R I m e R 1. In a reactor equipped with a jacket for heating and cooling, a stirrer, a thermocouple, load of 4.7 mol (291,4 wt.h.) of ethylene glycol, 0.15 mol (21 wt.h.) hexamethylenetetramine (urotropine), 1 mol (94 wt.h.) phenol, 1.3 mol (137 wt.h.) 93% sulfuric acid, 1.3 mol in terms of formaldehyde (39 wt.h.) trioxane or paraformaldehyde. The temperature of the reaction mass was raised to 67aboutC. At this temperature and stirring maintain the reaction mass 90 minutes, then poured into a pan and placed in a heat chamber, magneticone resin. Spend the extraction of water from the resin of ethylene glycol and sulfuric acid. The yield of tar 376 g with a humidity of 70%. A solution of ethylene glycol and sulfuric acid evaporated and return to the stage of condensation, taking into account when calculating the amount of the glycol and acid.

Information on examples 2-3 are summarized in the table that presents the test results of the properties of the obtained sorbent. Examples 4-13 tably serve as a control.

The proposed method, the sorbent can be the porosity of the product is 0.5-1.2 cm3/g, the minimum content of organic matter in the treated water, which indicates a high chemical stability and selectivity of sorption, the number purified from organic substances water 800-1000 about/about.the resin. You can create a waste-free manufacturing process through the use of one stripped off the solution after extraction from the pores of the resin of ethylene glycol and sulfuric acid.

In receipt of sorbent used products:

the synthetic phenol, GOST 23519-79,

ethylene glycol, GOST 19710-83,

trioxane symmetric, THE 6-05-211-1420-86,

paraformaldehyde, THE 6-05-930-78,

urotropine (hexamethylenetetramine technical), GOST 1381-73,

acid is ncacii by heating phenol, formaldehyde, hexamethylenetetramine in the presence of sulfuric acid and pore-forming with subsequent thermotherapies of the polycondensation product, characterized in that, to increase porosity, chemical resistance and capacity of the sorbent for organic substances as blowing agent used ethylene glycol, the condensation is carried out at 60 - 75oC and a molar ratio of phenol: formaldehyde : hexamethylenetetramine: sulfuric acid: ethylene glycol 1 : 0,6 - 2,0 : 0,06 - 0,24 : 0,4 - 1,9 : 2,4 - 5,7, then from the fully cured polycondensate extracted with water, ethylene glycol and sulfuric acid.

2. The method according to p. 1, characterized in that use formaldehyde as paraformaldehyde or trioxane.

3. The method according to p. 1, characterized in that the extracted water solution of ethylene glycol and sulfuric acid is evaporated and returned to the process.

 

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Abstract // 2293061

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