The past several decades have illustrated an enormous interest in noble metal nanoparticles for their superior catalytic activity, however, their industrial use is very restricted due to inefficient recovery leading to potential contamination of products and the environment. Immobilised nanoparticles illustrate promising results for scaling up processes, and can be successfully applied for various catalytic processes including waste industrial water treatment. The aim of the study was to design and study an easy and economically efficient green chemistry approach of preparation of macroporous material, with well distributed gold nanoparticles within the wall of cryogel. Ionic cryogels containing chitosan and tetrachloroaurate complex was reduced by 1.1.3.3-tetramethoxypropane, concurrently allowing chemical cross-linking of the polymer. A mechanism of reduction of noble gold complexes within the cryogel walls by tetramethoxypropane is also studied. Properties of the composite cryogels were evaluated using; differential scanning calorimetry, FT-IR, NMR, compression tests, SEM, TEM), Energy-dispersive X-ray spectroscopy and low temperature nitrogen adsorption. The catalytic activity of the in-situ synthesised gold nanoparticles was comprehensively studied using a model reduction reaction of 4-nitrophenol. Four different concentrations of gold nanoparticles within the cryogel structure were investigated. The turnover number and the turnover frequency parameters for cryogels containing four different concentrations of gold nanoparticles were calculated. The conversion degree of 4-nitrophenol to 4-aminophenol for cryogel containing the lowest of gold nanoparticles reached 96.8% at room temperature. The catalytic activity of incorporated gold nanoparticles for 4-nitrophenol conversion did not decline over 14 consequent testing cycles.