SU503843A1 - The method of obtaining polybenzylchloride - Google Patents

Description

at 60-, 16Q С, Catalysts can be chemically pure substances or contain trace impurities of other elements.

Example 1, To a round-bottom box, with a capacity of 2OO ml, equipped with a reflux condenser, 66 g of benzyl chloride are loaded with 30 g of a ball-type aluminosilicate catalyst (MPTU 38-.1-189-b5). The mixture is heated in a water bath at a temperature of the reaction mass C for 5 hours. The released hydrogen chloride is absorbed by 10% caustic soda. After completion of the reaction, the contents of the flask are cooled to 2 ° C and filtered. Get 55,2 g of polybenzyl chloride with a refractive index And, p 1,5990 and chlorine content,%; 14.11; 13.93. By dakna: l NMR spectroscopy average; the degree of polycondensation (P) is 2.45; the average molecular weight (M) is 269.3; the ratio of steam to ortho-substitution (i) is 5.16.

Example 2. A mixture of 66 g of benzyl chloride and 30 g of aluminosilicate catalysis is carried out on a glycerin bath at 135 ° C for 1.5 hours, and 3 g of the substance is taken

§О 15780, chlorine content,%: 18,

74, 18, 78, R 1.75V M- 196.9, 75: The residue is heated for another 3 hours. 5Og polybenzyl chloride, H 1.6130; chlorine content,%: 1O, 88; 1O, 65; P - 3.25, M 330.6, p: p 4.54.

Example 3.10Og benzyl chloride and 1 g of CaA brand zeolite are heated on a boiling water bath for about 1.5 hours. After cooling and filtration, 81 g of polybenzlchloride are obtained, having

Oh oh

j H 35 1.602; chlorine content,%: 16,

li; 98; R 2.55, M 268.2, p: o 8.4. Example 4. 100 g of benzyl chloride and 50 g of mixed catalyst C With aluminosilicate with zeolite C-3) are heated at 116-118 C for 3 h. After cooling the filtration, 73.4 g of olibenanlhporide are obtained. Investigate 3i samples (for Sr), selected during the reaction and KOMe4Hb5 product .; The results are shown in Table. one.

Example 5. 100 g of benzyl chloride and booster of KSK brand are heated at 155-16 ° C. The flow of 18 hours. Obtain 83 g of polybenzyl chloride 5 I. 1,584; chlorine content,%: 16.30; 16.05; P 1.90; M 210.2; p: about 5.33.

Example 6. 15Og benzyl chloride and 75 g of calcined river; sand) is heated to 80 ° C. At this temperature, an energetic reaction starts, which continues after cooling the reaction mass at 60-65 ° C for 35 minutes. After filtration, 116 g of polybenzoyl chloride are obtained. Examine 2 samples (3 g) and the final product. The results are shown in table. 2

Example 7. 110g of chloride

benzyl and 5 g of anhydrous alumina (TU No. 2O63-49) are heated at 160 ° C for 7 hours, then 3g of substance is collected that has an AND 2 1.566, chlorine content,%: 21.32, 21.0; P 1.51; M 175; n: about 3.25.

The residue is heated for another 6 hours. 85.1 g of polybenzyl chloride are obtained, having

20

 у- - 1,604, chlorine content,%:

l2, ol; 11.80; P 2.73; M 285, O; n: about 8.6.

Example 8. 5Og benzyl chloride and 0.5 g of HM-TK-.46 brand zeolite are heated at 100-105 C for 3.75 hours. 40.1 g of polybenzyl chloride are obtained, and, 2p 1.607; chlorine content,%:

11.73; 11.60; P 3.30; M 335.1; n: o 4,5.

} t) Sand contains impurities of cations,%: 0.01, A3, A 3.0, 0.001, 0.1, 0.3, 0.003, M / 0.001, N OOZ,

Ag -O, UOl. The amount of these impurities does not change after the experiment, despite the loss of the catalytic activity of the sand.

Table 1

Claims (2)

Formula of simplifying the manufacturing process, in The method for producing polybenzyl chlorides is oxides of silicon, aluminum, aluminosilicates, Formulas (® - -®40 | them. -firms, zeolites, or mixtures thereof.  by polycondensation; chloro) benzyl 2. The method according to p. 1, distinguishing : in the presence of a catalyst, when heated, so that the process is carried out in a liquid phase, in that with a view at 50-180 ° C ... as a catalyst, the process is used