公开(公告)号：KR100831877B1

公开(公告)日：2008-05-23

申请号：KR1020070019938

申请日：2007-02-27

Applicant: 한국에너지기술연구원

Inventor： 안영수 ,  여정구 ,  한문희 ,  조철희 ,  샤랏바가트 ,  김용하 ,  박호성

IPC: C01B33/14 ,  C01B33/157

CPC classification number: C01B33/1585 ,  B01J13/0091 ,  C01P2006/90

Abstract: A method for the preparation of a silica aerogel monolith in the atmosphere pressure is provided to prevent surface cracking frequently generated due to drying and contraction in ambient pressure drying by controlling the molar ratio of an organic precursor and methyl alcohol, thereby imparting flexibility to a wet gel of an intermediate step, and reduce the preparation cost by simplifying the preparation process. In a preparation method of a silica aerogel, a method for the preparation of a silica aerogel monolith comprises: a gelling process(S1) of diluting an organic precursor into methanol, adding oxalic acid as an acidic catalyst into the diluted solution in a concentration of 0.01 to 0.1M to hydrolyze the mixed solution for 24 hours, and adding a basic catalyst into the hydrolyzed material to gel the material at a temperature of 25 to 30 deg.C; and a drying process(S2) of drying the hydrophobic gel at a temperature of 50 to 300 deg.C in the atmosphere pressure. The organic precursor is one or more selected from the group consisting of methyltrimethoxysilane, trimethylchlorosilane, hexamethyldisilazane, trimethylethoxysilane, ethyltriethoxysilane, and phenyltriethoxysilane. The basic catalyst is one selected from the group consisting of ammonia water(NH4OH), potassium hydroxide(KOH), and sodium hydroxide(NaOH), and the basic catalyst is added after adding the acidic catalyst. Further, a mole rate(MeOH/MTMS) of the methyltrimethoxysilane and methanol is 30 to 40.

Abstract translation: 提供了一种在气氛压力下制备二氧化硅气凝胶整料的方法，以通过控制有机前体和甲醇的摩尔比来防止由于环境压力干燥中的干燥和收缩而频繁产生的表面开裂，从而赋予湿润的柔软性 凝胶，并通过简化制备过程降低制备成本。 在二氧化硅气凝胶的制备方法中，制备二氧化硅气凝胶整料的方法包括：将有机前体稀释成甲醇的胶凝方法（S1），将草酸作为酸性催化剂以浓度为 0.01〜0.1M水解该混合液24小时，在水解物中加入碱性催化剂，使其在25〜30℃的温度下凝胶化; 以及在大气压下在50〜300℃的温度下干燥疏水性凝胶的干燥工序（S2）。 有机前体是选自甲基三甲氧基硅烷，三甲基氯硅烷，六甲基二硅氮烷，三甲基乙氧基硅烷，乙基三乙氧基硅烷和苯基三乙氧基硅烷中的一种或多种。 碱性催化剂选自氨水（NH 4 OH），氢氧化钾（KOH）和氢氧化钠（NaOH），碱性催化剂加入酸性催化剂后加入。 此外，甲基三甲氧基硅烷和甲醇的摩尔比（MeOH / MTMS）为30〜40。