RU1455654C - Method of obtaining sorbent - Google Patents

Abstract

The invention relates to the synthesis of high molecular weight polymer sorbents of the Polysorb type. The invention allows to increase the specific surface area of the sorbent and the sorption capacity for the absorption of organic substances from aqueous solutions by copolymerizing ethyl styrene with divinylbenzene in the presence of glycidyl methacrylate or its mixture with triethylene glycol dimethacrylic ether in the amount of 16.1-34.6% of the polymerization mass and in the presence of modifying solvents (85-87% gasoline or 100-200% toluene in relation to the weight of monomers). Post-polymerization conditioning with methanol and water with heating is possible to increase the specific surface area. 1 s.p. crystals, 4 tab.

Description

The invention relates to the synthesis of polysorb type high-porous polymer sorbents that can be used to isolate antibiotics and other biologically active compounds from fermentation solutions, as well as in chromatographic analysis as column fillers.

The aim of the invention is to increase the sorption capacity of highly porous sorbents for organic compounds from aqueous solutions by increasing the specific surface of the sorbent

Example 1 A 400-liter 1% starch aqueous solution is charged to a flask equipped with a thermometer J and a reflux condenser, then a polymerization mixture is added, consisting of 18.9 g glycidyl methacrylate, 50 g divsptbenzene, 28, 1 ethyl styrene, 3 g azobisisobutyric acid dinitrile and 85 tons of BR-L gasoline After reaching the desired degree of dispersion over. The reaction temperature is increased for 10–15 min. Up to 70 ° C and kept at this temperature for 6 hours. A semi-saturated sorbent is washed with water.

Further conditioning is carried out according to the scheme:

-exposure in an aqueous medium at a temperature of Tu1Ge 90-95 ° С for 1 4j

-two-, three-fold treatment of the sorbent with methanol at a temperature

50 s for 2 4j

-two-, three-fold treatment of the sorbent with water for 1 h at a temperature of 90-95 C.

1 ate ate

C5 O1

Yield 98.5%,

Up to 5, 333.5 m / g (specific surface area),

P

After conditioning 1, S, ..

p g g l / ° and

355.3 m / g.

Example ..2, V. d-rad goryugo flask equipped with a stirrer, thermometer and refrigerator, load a 0.5 L aqueous solution of krata (al) and add a mixture of 275 g glycidide methyl crylate 5% g divinylbenzo a. 19 | 9 g of ethyl styrene, 3 g of diptril azobis-oil knotslotts 200 g of toluene. Further, copolymerization and intronanye 1 lead .t is the same as in example 1S

Yield 98.3%,

Contains butyl acetate, acetic acid K1 slot5 methyl methacrylic acid in the amount of 300 to 800 ig / l,

Solution 3.

Contains organophosphorus co-Q dinenes, in particular trnbutyl phosphate, in an amount of from 30 to 150 mg / l,

The experiments were carried out under static conditions. Contact time 2-3 hours

Claims (1)

Desorption is carried out with methanol at a temperature of 40-45 ° C. Claims fifteen 1 a Method for the preparation of cop6eii7 a by 2 tmerization of divinylbeneol and ethyl DOI to 1HI1 SQ ionization. lOjSH / it.jQ styrene in the presence of modifying Gy.Piagrilamide in col - up to 2 g / l. 55654 formalin lives, honestly from Oh :) Solution 2 ( Contains butyl acetate, acetic acid K1 slot5 methyl methacrylic acid in the amount of 300 to 800 ig / l, Solution 3. Contains organophosphorus co-Q dinenes, in particular trnbutyl phosphate, in an amount of from 30 to 150 mg / l, The experiments were carried out under static conditions. Contact time 2-3 hours Desorption is carried out with methanol at a temperature of 40-45 ° C. Claims fifteen  az After air conditioning, -0 bfVr, The dependence of the specific surface area on the amount and Bi-based codification solvent is illustrated by the distant tables, 1.-3. -. Table 1 shows data on the specific surface of sorbentoa depending on the amount of glycidyl methacrylate introduced and its mixture with triethenlengpi ™ col dimethacrylate. The results of the sorption capacity test for organic compounds from aqueous solutions 1–3 in comparison with the gphototype and the base object are given in Table It solution Contains a mixture of amines: 255-methyl vipnylpyridine. pyridine j, .trga ethyl-anine dimethylamine, and also contains a solvent and a catalyst, especially with a view to increasing the sorption capacity of organic compounds in aqueous pacTHopaXt polymerization mass, glidyl methyl methacrylate or its mixture with trieth1-tenglycol dimethacrylate is additionally introduced in an amount relative to the polymerization mass, and gasoline in an amount of 85-87% or toluene in an amount of 100-200% relative to the polymerization mass is used as a modifying solvent; 2, The method according to claim 1, with h and o-ED and with the fact that the obtained sorbent is subjected to post-heat-conditioning conditioning by sequential treatment with water, methanol and water when heated to a temperature below the boiling point. water and methanol. Table 1 196.4 212.0 218.0 2 1 2 ,. 2 Prototype (example 1) Also (example 2) Polysorb 10 (prototype) CAD-iodine (base object) U5565A10 Table u 49.3 45.8 29.5 13.8