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de - Beste verfügbare Techniken (BVT) - Umweltbundesamt

de - Beste verfügbare Techniken (BVT) - Umweltbundesamt de - Beste verfügbare Techniken (BVT) - Umweltbundesamt

bvt.umweltbundesamt.de
von bvt.umweltbundesamt.de Mehr von diesem Publisher
05.01.2013 Aufrufe

Chapter 2 Organic feed solvent SO 3 Water H 2 SO 4 Water Sulphonation with SO 3 Precipitation Product washing SO 3, SO 2, VOC Phase separation Organic phase Filtration Product Figure 2.28: Sulphonation with SO3 in liquid phase Organic feed SO 3 Water Sulphonation with SO 3 Product washing Product Figure 2.29: Sulphonation with SO3 in gas-liquid reaction Mother liquor Wash-water SO 3 , SO 2 , VOC Wash-water 62 Dezember 2005 OFC_BREF

2.5.14 Sulphochlorination with chlorosulphonic acid [15, Köppke, 2000] Chapter 2 Sulphochlorination leads to organic sulphochlorides, which act as intermediates for a variety of fine chemicals, e.g. sulphonamides, sulphono hydrazides, sulphonic esters, sulphinic acids, sulphones, and thiophenols. Chemical reaction Sulphochlorination takes place in a two step reaction as shown: R HSO 3Cl SO 3H R (1) (2a) Figure 2.30: Sulphochlorination with chlorosulphonic acid HSO 3Cl - H 2SO 4 OFC_BREF Dezember 2005 63 R SO 2Cl Step (1) represents a sulphonation similar to that described in Section 2.5.13. The reversible second step is a chlorination and is usually carried out with excess chlorosulphonic acid. Alternatively, thionyl chloride may be used for the second step as shown in the following equation: (2b) R – SO3H + SOCl2 � R – SO2Cl + SO2 + HCl Side reactions: • formation of sulphones (e.g. 35 % in the case of chloro benzene) • formation of isomers • formation of other halogenation products. Operations Figure 2.31 shows a typical sequence of operations in sulphochlorination. The chlorosulphonic acid is introduced into a cast-steel or enamelled-steel vessel and 10 - 25 mol % of the aromatic compound is stirred in at 25 – 30 °C, whereupon sulphonation of the aromatic compound and HCl formation occur. The exothermic formation of sulphonyl chloride is initiated by heating the reactants to 50 – 80 °C. In the case of aromatic compounds that easily take up two sulphochloride groups, e.g. anisole, monochlorosulphonation is carried out with only a little more than the calculated amount of chlorosulphonic acid at a low temperature (0 °C) and in the presence of a diluent such as dichloromethane. The temperature has to be controlled accurately to ensure the uniform release of HCl gas. Restarting the agitator after an interruption of the electricity supply is hazardous and may cause the contents of the vessel to foam over.

Chapter 2<br />

Organic feed<br />

solvent<br />

SO 3<br />

Water<br />

H 2 SO 4<br />

Water<br />

Sulphonation with SO 3<br />

Precipitation<br />

Product washing<br />

SO 3, SO 2, VOC<br />

Phase separation Organic phase<br />

Filtration<br />

Product<br />

Figure 2.28: Sulphonation with SO3 in liquid phase<br />

Organic feed<br />

SO 3<br />

Water<br />

Sulphonation with SO 3<br />

Product washing<br />

Product<br />

Figure 2.29: Sulphonation with SO3 in gas-liquid reaction<br />

Mother liquor<br />

Wash-water<br />

SO 3 , SO 2 , VOC<br />

Wash-water<br />

62 Dezember 2005 OFC_BREF

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