CN111939974A - 一种净化室内甲醛的钛硅分子筛复合材料的制备方法 - Google Patents
一种净化室内甲醛的钛硅分子筛复合材料的制备方法 Download PDFInfo
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- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 title claims abstract description 123
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- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 52
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- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical group CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 3
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- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical group [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 3
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Abstract
本发明公开了一种净化室内甲醛的钛硅分子筛催化剂及制备方法,包括以下步骤:S1:溶液的配制;S2:水热法合成钛硅分子筛;S3:钛硅分子筛上负载Ag。本发明方法制备的钛硅分子筛催化剂具有较高的疏水性及特殊的孔道结构,可以将室内低浓度的甲醛吸附富集到负载了Ag的钛硅分子筛上,可以在室温条件下实现对甲醛的高效降解。同时,该催化剂因较大的比表面积、良好的热稳定性可以实现长时间稳定操作。
Description
技术领域
本发明设计室内气体净化领域,尤其是涉及一种净化室内甲醛的分子筛复合材料的制备方法。
背景技术
甲醛是一种原生毒质,也是室内VOCs的主要污染物,它对人体的危害主要体现在刺激作用、致敏作用以及致畸作用,严重危害人类的身体健康,国际癌症研究机构将甲醛列为一类致癌物质,我国的《室内空气质量标准》规定室内空气中甲醛的含量不得高于0.08mg/m3,但是刚装修的房子的甲醛浓度远远超过这个标准,因此为了保证人们的身体健康,研发高效的甲醛净化技术对提高室内空气质量意义重大。
针对净化室内甲醛,国内外采用较多的处理技术主要有以下几种:物理吸附法、等离子体技术、光催化技术等。其中物理吸附虽然操作相对简单,但是当吸附剂吸附的甲醛达到吸附平衡时,就不会再对甲醛进行去除,而对吸附剂进行脱附过程比较繁琐;等离子体技术利用介质放电产生的电子,经过物理化学反应后可将甲醛分解,但是该技术设备成本过高,运行能耗较大,且产生的CO副产物会造成二次污染;光催化技术利用光照产生的空穴可将甲醛进行高效分解,但是该方法一般必须要有紫外光照才能将催化剂激发出空穴,而太阳光中大部分为可见光和红外光,紫外光线仅为5%,因此光催化技术去除甲醛的技术仍需改进。
发明内容
为了克服背景技术的不足,本发明公开了一种净化室内甲醛的钛硅分子筛催化剂的制备方法。所提供的钛硅分子筛中Ti起到主要的催化作用,而且该分子筛的疏水性以及特殊的孔道结构,对甲醛有很好的吸附能力,可以将较低浓度的甲醛吸附并富集到催化剂上,该催化剂负载Ag后可作为催化剂将甲醛高效降解。同时,该催化剂因较大的比表面积、良好的热稳定性可以实现长时间稳定操作。
技术方案:本发明的净化室内甲醛的钛硅分子筛催化剂及制备方法,其特征在于,包括以下步骤:
S1:溶液的配制
将硅源加入到模板剂溶液中,搅拌10-30分钟,使硅源均匀分散在模板剂溶液中,得到溶液A,将钛源溶于异丙醇溶液中,搅拌10-30分钟,得到溶液B,在搅拌下将溶液B逐滴滴加到溶液A中,充分搅拌后得到溶液C,将溶液C于70-90℃下进行水浴加热以除去异丙醇;
S2:水热法合成钛硅分子筛
将S1除醇后的溶液转移至反应釜中进行水热反应,于170-200℃反应24-48小时得到钛硅分子筛前驱体,用去离子水洗至中性,于70-90℃下干燥2-6小时,然后在550-750℃下煅烧6-8小时,钛硅分子筛催化剂;
S3:钛硅分子筛上负载Ag
将S2制备的钛硅分子筛加入到浓硝酸溶液中,进行搅拌15-30min,使分子筛均匀地分散在溶液中,用去离子水洗涤至pH=7,得到溶液D;将硝酸银加入去离子水中搅拌溶解,而后加入硝酸溶液,得到溶液E;将溶液E中加入溶液D,于70-9080℃下搅拌2-4小时后,静置12-24小时后蒸发、干燥、并于氢气氛围中还原2-8小时,得到Ag负载的钛硅分子筛催化剂。
进一步的,S1中所述硅源为正硅酸四乙酯,所述模板剂为20wt%的四丁基氢氧化铵,所述的钛源为钛酸四丁酯。
进一步的,S1除醇步骤中要适时添加去离子水,确保溶液体积不变。
进一步的,S3所述的硝酸浓度为0.1-6mol/L。
进一步的,S3所述的钛硅分子筛和硝酸溶液的固液比为1:(5-25)。
进一步的,S3所述的硝酸银负载量为钛硅分子筛质量的0.5-2wt%。
进一步的,S3所述的蒸发温度为50-100℃,干燥温度为100-150℃,H2氛围还原温度为300-500℃。
本发明的有益效果:当室内甲醛浓度较低时能够将其吸附富集到负载了Ag的钛硅分子筛上,并可以在室温条件下实现对甲醛的高效降解。相较于普通的甲醛吸附剂,本发明方法制备的分子筛可以利用其特殊的孔道结构对甲醛进行吸附,而且分子筛的活性最分Ti以及负载的Ag可以直接将吸附的甲醛降解,避免了普通甲醛吸附剂达到吸附平衡后再生活化的过程。而且该催化剂的制备方法工艺简单,原料低廉,适合在工业上推广。
附图说明
图1为Ag的不同负载量下甲醛的去除率。
具体实施方式
下面结合实施例对本发明的技术方案作进一步的说明。
实施例1
S1:溶液的配制
将15g正硅酸四乙酯加入到30mL 20wt%的四丁基氢氧化铵溶液中,搅拌30分钟,使硅源均匀分散在模板剂溶液中,得到溶液A,将0.6g钛酸四丁酯溶于12mL异丙醇溶液中,搅拌30分钟,得到溶液B,在搅拌下将溶液B逐滴滴加到溶液A中,充分搅拌后得到溶液C;将溶液C于80℃下进行水浴加热以除去异丙醇,该步骤要适时添加去离子水,确保溶液体积不变;
S2:水热法合成钛硅分子筛
将S1除醇后的溶液转移至反应釜中进行水热反应,于170℃反应48小时得到钛硅分子筛前驱体,用去离子水洗至中性,于80℃下干燥6小时,然后在550℃下煅烧8小时,钛硅分子筛催化剂;
S3:钛硅分子筛上负载Ag
将S2制备的钛硅分子筛加入到浓度为1mol/L的硝酸溶液中,进行搅拌30min,使钛硅分子筛均匀地分散在溶液中,用去离子水洗涤至pH=7,得到溶液D,将0.5wt%硝酸银加入去离子水中搅拌溶解,而后加入1mol/L的硝酸溶液,得到溶液E,将溶液E中加入溶液D,于80℃下搅拌3小时后,静置12小时后于60℃下蒸发掉水分,而后在120℃下干燥8小时,并于氢气氛围中400℃还原4小时,得到0.5wt%Ag负载的钛硅分子筛催化剂。
实施例2
Ag的负载量变为1.0wt%,其他原料组分分与工艺参数不变,得到1.0wt%Ag负载的钛硅分子筛催化剂。
实施例3
Ag的负载量变为1.5wt%,其他原料组与工艺参数不变,得到1.5wt%Ag负载的钛硅分子筛催化剂。
实施例4
Ag的负载量变为2.0wt%,其他原料组分与工艺参数不变,得到2.0wt%Ag负载的钛硅分子筛催化剂。
实施例1-4制备的催化剂去除甲醛的应用结果如图1所示,房间面积15m2,甲醛初始浓度为0.8mg/m3。选用普通甲醛吸附剂150g,30小时后,房间内甲醛浓度为0.12mg/m3,甲醛去除率为85%;使用本发明中Ag负载的钛硅分子筛催化剂150g,其中Ag负载量为1.5wt%时,房间内甲醛浓度为0.072mg/m3,甲醛去除率达到91%。
Claims (7)
1.一种净化室内甲醛的钛硅分子筛催化剂的制备方法,其特征在于,包括以下步骤:
S1:溶液的配制
将硅源加入到模板剂溶液中,搅拌10-30分钟,使硅源均匀分散在模板剂溶液中,得到溶液A;将钛源溶于异丙醇溶液中,搅拌10-30分钟,得到溶液B;在搅拌下将溶液B逐滴滴加到溶液A中,充分搅拌后得到溶液C;将溶液C于70-90℃下进行水浴加热以除去异丙醇;
S2:水热法合成钛硅分子筛
将S1除醇后的溶液转移至反应釜中进行水热反应,于170-200℃反应24-48小时得到钛硅分子筛前驱体;用去离子水洗至中性,于70-90℃下干燥2-6小时,然后在550-750℃下煅烧6-8小时,钛硅分子筛催化剂;
S3:钛硅分子筛上负载Ag
将S2制备的钛硅分子筛加入到浓硝酸溶液中,进行搅拌15-30min,使分子筛均匀地分散在溶液中,用去离子水洗涤至pH=7,得到溶液D;将硝酸银加入去离子水中搅拌溶解,而后加入硝酸溶液,得到溶液E;将溶液E中加入溶液D,于70-90℃下搅拌2-4小时后,静置12-24小时后蒸发、干燥、并于氢气氛围中还原2-8小时,得到Ag负载的钛硅分子筛催化剂。
2.根据权利要求1所述的净化室内甲醛的钛硅分子筛催化剂的制备方法,其特征在于:S1中所述硅源为正硅酸四乙酯,所述模板剂为20wt%的四丁基氢氧化铵,所述的钛源为钛酸四丁酯。
3.根据权利要求1所述的净化室内甲醛的钛硅分子筛催化剂的制备方法,其特征在于:S1除醇步骤中要适时添加去离子水,确保溶液体积不变。
4.根据权利要求1所述的净化室内甲醛的钛硅分子筛催化剂的制备方法,其特征在于:S3所述的硝酸浓度为0.1-6mol/L。
5.根据权利要求1所述的净化室内甲醛的钛硅分子筛催化剂的制备方法,其特征在于:S3所述的分子筛和硝酸溶液的固液比为1:5-25。
6.根据权利要求1所述的净化室内甲醛的钛硅分子筛催化剂的制备方法,其特征在于:S3所述的硝酸银负载量为分子筛质量的0.5-2wt%。
7.根据权利要求1所述的净化室内甲醛的钛硅分子筛催化剂的制备方法,其特征在于:S3所述的蒸发温度为50-100℃,干燥温度为100-150℃,H2氛围还原温度为300-500℃。
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