The synthesis of zeolite beta has been studied using the following templating agents: (i) tetraethylammonium hydroxide (TEA;)(ii) tetraethylammonium bromide–diethanolamine; and (iii) tetraethylammonium hydroxide–tetraethylammonium bromide–triethanolamine. TEA⁺ ions and TEAOH molecules only have a structure-directing effect. The ratio (Si + Al)/TEA⁺ in the gel was varied from 2 to 10, the Si/Al ratio from 12 to 1000. The temperature of crystallization was chosen in the range 368–443 K. The samples were characterized using X-ray diffraction, micrographs, chemical analysis, thermal analysis, IR spectroscopy and nitrogen adsorption. Zeolite beta of good crystallinity (micropore volume = 0.28 cm³ g^–1) was obtained with Si/Al ratios from 14 to 72. The acid strength and number of acid sites were determined from the calorimetrically measured heat of NH₃ sorption and from the TPD of NH₃. The initial acid strengths of zeolite beta (up to 185 kJ mol^–1) are higher than those of other high-silica zeolites.

Polycrystalline agglomerates are formed instead of small single crystals on the addition of diethanolamine to the synthesis gel. The agglomerates are characterized by a high intercrystalline volume (> 0.47 cm³ g^–1), which can be influenced in a definite manner by variation of the TEABr/diethanolamine ratio. The presence of triethanolamine initiates the transformation of zeolite beta into a SiO₂ layer structure at 368 K.