CN108187610A - 一种用于污水处理的氮化碳-硅藻土的制备方法 - Google Patents
一种用于污水处理的氮化碳-硅藻土的制备方法 Download PDFInfo
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/14—Diatomaceous earth
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0259—Compounds of N, P, As, Sb, Bi
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/42—Materials comprising a mixture of inorganic materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
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- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Materials Engineering (AREA)
- Geochemistry & Mineralogy (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Physical Water Treatments (AREA)
Abstract
本发明公开了一种用于污水处理的氮化碳‑硅藻土的制备方法。a、将硅藻土加入硫酸溶液酸洗预处理后;b、加入水中分散,与巯丙基甲基二甲氧基硅烷混合,制得巯丙基甲基二甲氧基硅烷修饰的硅藻土;c、与三聚氰胺、水加入分散机,超声分散后得到三聚氰胺包覆的硅藻土;d、置于氮气氛围中,采用脉冲激光进行烧结,得到具有可见光响应的氮化碳硅藻土,即为用于污水处理的氮化碳‑硅藻土。所述方法具有以下有益效果:通过脉冲激光烧结形成的氮化碳均匀地负载于巯基修饰硅藻土上,结合力极强,性能稳定,并且具有高吸附性能,在可见光下具有良好的光催化效率,同时制备过程简单,成本低,可广泛用于污水处理领域。
Description
技术领域
本发明涉及污水处理领域,具体涉及污水处理硅藻土的制备,尤其是涉及一种用于污水处理的氮化碳-硅藻土的制备方法。
背景技术
工业废水和城市生活污水的排放,造成了严重的环境污染,因此,废水和污水的处理越来越受到人们的重视。当今污水处理的主要方法有两大类:一是物理化学法;二是生化法。普遍存在去除效果不理想,脱色效果差,而且会造成二次环境污染。因此,利用一些具有独特物理和化学性能的非金属矿,经过提纯、改性、活化、扩容等多种手段,使其具有优良的性能,用作污水处理剂,越来越受到关注和重视,例如对硅藻土、沸石、膨润土、海泡石、凹凸棒石等。尤其是硅藻土,已广泛用于污水处理、空气净化等各个领域。
硅藻土是由硅藻的壁壳组成,壁壳上有多级、大量、有序排列的微孔。这种独特的微孔结构,赋于它许多优良的性能。它性能稳定,耐酸、孔容大,孔径大,比表面积大,吸附性强,对污水有极好的净化效果。但硅藻土仅能吸附废水中的污染物,吸附量有限,且无法有效进行降解消除,因此需要与其他技术进行有效结合。其中光催化技术可以将有机污染物在较温和的条件下矿化降解为无毒无害的二氧化碳、水等产物,在污水处理、空气净化等方面的良好应用前景。目前常用的二氧化钛光催化剂只能响应波长较短的紫外光,其在可见光区域没有明显的吸收,相比而言,氮化碳因其层状结构,光能利用率高,受到越来越多地关注。将硅藻土和氮化碳等光催化剂进行结合,成为一项重要的研究课题。
专利申请号201710302610.0公开了一种高效污水处理剂及其制备方法,该污水处理剂由以下原料制备而成:玛雅蓝粉末、纳米水性粘合剂、石墨烯、聚乙二醇丙烯酸酯、阴离子聚丙烯酰胺、磷酸二氢钾、牡蛎壳粉、改性硅藻土、聚合硫酸铁、碳酸钙、苯扎氯铵、活性炭纤维、糠醛活性炭、锐钛矿型硫镧共掺杂纳米二氧化钛。此发明在污水处理的过程中实现了吸附与降解的同时进行,具有很强的吸附和降解能力,出水清澈,水质稳定;且吸附降解剂能够实现再生回用,再生方便,节约污水的处理成本。
专利申请号201710708221.8公开了一种利用硅藻土作为载体的组合物及其制备方法和应用,该组合物由硅藻土、氢氧化钙、纳米二氧化钛、纳米氧化锌、贝壳粉、电气石粉、蛭石粉、葡萄糖甙、赖氨酸、醚化淀粉、海藻胶、聚乙二醇、甘露醇、丙三醇、葡萄糖、二氧化锰和水组成。此组合物既可用于装修装饰材料以吸附室内的甲醛、氨气以及其他有刺激性异味的气体,也可用于污水处理,以降低其重金属离子、磷、低分子醛等有害物质的含量。
专利申请号201410234668.2公开了一种硅藻土球负载铌酸盐类可见光光催化剂的制备方法,以廉价的Nb2O5替代昂贵的有机铌源,制备可溶性氢氧化铌,并与碳酸钾同时加到柠檬酸溶液中,加热搅拌得到铌酸钾溶胶。将制备好的硅藻土球浸渍在溶胶中,经浸渍、烘干、煅烧,即得硅藻土球负载铌酸盐类可见光光催化剂。该光催化剂制备工艺简单,制备成本低,并可直接利用可见光。采用可见光源,经3h可降解89%的罗丹明B溶液;在太阳光下照射1h即可彻底杀灭大肠杆菌;以普通日光灯照射3h,可降解85%的甲醛,表明该负载型光催化剂在污水处理、抗菌杀菌、空气净化等方面具有良好的应用前景,且利于回收再利用,光催化性能及稳定性优异。
专利申请号201710098145.3公开了一种可见光响应型光催化剂的制备方法,该催化剂是一种少层氮化碳/氧化锌复合物。该复合光催化剂由一定质量的少层氮化碳和氧化锌复合而成,其具体制备步骤如下:将制备的花状氧化锌材料置于去离子水中超声至均匀分散,然后加入一定质量的少层氮化碳并继续超声分散、搅拌一定时间后,再将混合液转移至油浴锅中加热搅拌直至蒸干,即可得到少层氮化碳/氧化锌复合光催化剂。光催化性能实验表明该复合光催化剂相对于宽禁带的非可见光响应型氧化锌材料,既有较宽的可见光响应范围,又有较高的光催化活性,在太阳能转化和污水处理等方面具有良好的应用前景和经济效益。
由此可见,现有技术中硅藻土进行污水处理时吸附量有限,无法降解污染物,限制其在污水处理中的应用,而光催化氧化技术在光能利用率和光催化活性方面较差,将硅藻土与光催化剂结合的技术中,材料结合性差,并且需要长时间的煅烧,存在能耗高且生产效率低等问题。
发明内容
为有效解决上述技术问题,本发明提出了一种用于污水处理的氮化碳-硅藻土的制备方法,可有效提高氮化碳和硅藻土的结合力,所得氮化碳硅藻土吸附性能强,并且具有良好的催化降解能力。
本发明的具体技术方案如下:
一种用于污水处理的氮化碳-硅藻土的制备方法,具体的制备步骤为:
a、将硅藻土加入质量浓度为60~70%的硫酸溶液中,搅拌均匀后煮沸2~3h,使硅藻土中的杂质与硫酸反应生成可溶性盐类,经压滤、洗涤、干燥,得到预处理的硅藻土;
b、将步骤a中预处理的硅藻土加入水中,分散均匀,再加入巯丙基甲基二甲氧基硅烷,混合搅拌分散,得到巯丙基甲基二甲氧基硅烷修饰的硅藻土;
c、将步骤b制得的巯丙基甲基二甲氧基硅烷修饰的硅藻土加入水中,置于分散机中,然后加入三聚氰胺,进行超声辅助分散,干燥后制得三聚氰胺包覆的硅藻土;
d、将步骤c制得的三聚氰胺包覆的硅藻土置入氮气气氛中,采用脉冲激光器缓慢升高能量,对硅藻土表面进行脉冲激光烧结,三聚氰胺的分子链断裂后,在硅藻土表面和微孔中形成一层氮化碳,洗涤,干燥,得到具有可见光响应的氮化碳硅藻土,即为用于污水处理的氮化碳-硅藻土。
优选的,所述硅藻土的比表面积为40~60m2/g,孔隙率为80~85%,孔体积0.5~0.9m3/g。
优选的,步骤b所述各组分的重量份为:预处理的硅藻土35~40份、巯丙基甲基二甲氧基硅烷硫酸溶液1~2份、水58~64份。
优选的,步骤c所述各组分的重量份为:巯丙基甲基二甲氧基硅烷修饰的硅藻土30~35份、三聚氰胺14~18份,水47~56份。
优选的,步骤c所述分散机为升降式分散机,可采用液压升降分散机、气动升降分散机或手摇升降分散机中的一种。
优选的,步骤c所述超声辅助分散的超声波频率为20~30kHz,分散时间为40~60min。
优选的,步骤d所述脉冲激光器采用钇铝石榴石激光器、红宝石激光器、钕玻璃激光器、氮分子激光器或准分子激光器中的一种。
优选的,步骤d所述脉冲激光烧结的初始能量为10~20J,终止能量为80~90J,脉冲能量升高速度为0.5~1J/s,升高到终止能量后继续反应10~15min。
本发明上述内容还提出一种用于污水处理的氮化碳-硅藻土的制备方法,主要是将硅藻土加入硫酸溶液预处理,除去硅藻土微孔中的杂质;将处理过的硅藻土加入到水中,分散均匀,用巯丙基甲基二甲氧基硅烷进行修饰,得到巯丙基甲基二甲氧基硅烷修饰的硅藻土;将巯丙基甲基二甲氧基硅烷修饰的硅藻土分散到水中,然后加入三聚氰胺,超声分散均匀后,得三聚氰胺包覆的硅藻土;将三聚氰胺包覆的硅藻土在氮气气氛中采用脉冲激光进行烧结,三聚氰胺的分子链断裂后,在硅藻土表面和微孔中形成一层氮化碳,得到一种具有可见光响应的氮化碳硅藻土。通过脉冲激光烧结,三聚氰胺能够快速转变为氮化碳,并且均匀的负载在硅藻土微孔及表面上,巯基修饰硅藻土可以加大氮化碳和硅藻土的结合力,能够更容易驻留在硅藻土中,制得的氮化碳硅藻土具有高吸附性能,并且在可见光下具有良好的光催化效率。
本发明的有益效果为:
1.提供了一种用于污水处理的氮化碳-硅藻土的制备方法。
2.本发明制备中通过脉冲激光烧结,三聚氰胺能够快速转变为氮化碳,并且均匀的负载在硅藻土微孔及表面上,巯基修饰硅藻土使得氮化碳和硅藻土的结合力极强,性能稳定。
3.本发明制得的氮化碳硅藻土具有高吸附性能,并且在可见光下具有良好的光催化效率,可高效达到污水处理的。
4.本发明制备过程简单,成本低,适合工业化生产。
具体实施方式
以下通过具体实施方式对本发明作进一步的详细说明,但不应将此理解为本发明的范围仅限于以下的实例。在不脱离本发明上述方法思想的情况下,根据本领域普通技术知识和惯用手段做出的各种替换或变更,均应包含在本发明的范围内。
实施例1
a、将硅藻土加入质量浓度为65%的硫酸溶液中,搅拌均匀后煮沸2.5h,使硅藻土中的杂质与硫酸反应生成可溶性盐类,经压滤、洗涤、干燥,得到预处理的硅藻土;
b、将步骤a中预处理的硅藻土加入水中,分散均匀,再加入巯丙基甲基二甲氧基硅烷,混合搅拌分散,得到巯丙基甲基二甲氧基硅烷修饰的硅藻土;
c、将步骤b制得的巯丙基甲基二甲氧基硅烷修饰的硅藻土加入水中,置于分散机中,然后加入三聚氰胺,进行超声辅助分散,干燥后制得三聚氰胺包覆的硅藻土;
d、将步骤c制得的三聚氰胺包覆的硅藻土置入氮气气氛中,采用脉冲激光器缓慢升高能量,对硅藻土表面进行脉冲激光烧结,洗涤,干燥,得到具有可见光响应的氮化碳硅藻土,即为用于污水处理的氮化碳-硅藻土。
预处理的硅藻土各组分的重量份为:硅藻土53份、硫酸溶液47份;巯丙基甲基二甲氧基硅烷修饰的硅藻土各组分的重量份为:预处理的硅藻土38份、巯丙基甲基二甲氧基硅烷硫酸溶液1份、水61份;三聚氰胺包覆的硅藻土各组分的重量份为:巯丙基甲基二甲氧基硅烷修饰的硅藻土33份、三聚氰胺16份,水51份。
分散机为液压升降分散机;超声辅助分散的超声波频率为25kHz,分散时间为50min;脉冲激光器采用钇铝石榴石激光器;脉冲激光烧结的初始能量为15J,终止能量为85J,脉冲能量升高速度为0.8J/s,升高到终止能量后继续反应13min。
实施例2
a、将硅藻土加入质量浓度为60%的硫酸溶液中,搅拌均匀后煮沸3h,使硅藻土中的杂质与硫酸反应生成可溶性盐类,经压滤、洗涤、干燥,得到预处理的硅藻土;
b、将步骤a中预处理的硅藻土加入水中,分散均匀,再加入巯丙基甲基二甲氧基硅烷,混合搅拌分散,得到巯丙基甲基二甲氧基硅烷修饰的硅藻土;
c、将步骤b制得的巯丙基甲基二甲氧基硅烷修饰的硅藻土加入水中,置于分散机中,然后加入三聚氰胺,进行超声辅助分散,干燥后制得三聚氰胺包覆的硅藻土;
d、将步骤c制得的三聚氰胺包覆的硅藻土置入氮气气氛中,采用脉冲激光器缓慢升高能量,对硅藻土表面进行脉冲激光烧结,洗涤,干燥,得到具有可见光响应的氮化碳硅藻土,即为用于污水处理的氮化碳-硅藻土。
预处理的硅藻土各组分的重量份为:硅藻土50份、硫酸溶液50份;巯丙基甲基二甲氧基硅烷修饰的硅藻土各组分的重量份为:预处理的硅藻土35份、巯丙基甲基二甲氧基硅烷硫酸溶液1份、水64份;三聚氰胺包覆的硅藻土各组分的重量份为:巯丙基甲基二甲氧基硅烷修饰的硅藻土30份、三聚氰胺14份,水56份。
分散机为气动升降分散机;超声辅助分散的超声波频率为20kHz,分散时间为60min;脉冲激光器采用红宝石激光器;脉冲激光烧结的初始能量为10J,终止能量为80J,脉冲能量升高速度为0.5J/s,升高到终止能量后继续反应15min。
实施例3
a、将硅藻土加入质量浓度为70%的硫酸溶液中,搅拌均匀后煮沸2h,使硅藻土中的杂质与硫酸反应生成可溶性盐类,经压滤、洗涤、干燥,得到预处理的硅藻土;
b、将步骤a中预处理的硅藻土加入水中,分散均匀,再加入巯丙基甲基二甲氧基硅烷,混合搅拌分散,得到巯丙基甲基二甲氧基硅烷修饰的硅藻土;
c、将步骤b制得的巯丙基甲基二甲氧基硅烷修饰的硅藻土加入水中,置于分散机中,然后加入三聚氰胺,进行超声辅助分散,干燥后制得三聚氰胺包覆的硅藻土;
d、将步骤c制得的三聚氰胺包覆的硅藻土置入氮气气氛中,采用脉冲激光器缓慢升高能量,对硅藻土表面进行脉冲激光烧结,洗涤,干燥,得到具有可见光响应的氮化碳硅藻土,即为用于污水处理的氮化碳-硅藻土。
预处理的硅藻土各组分的重量份为:硅藻土55份、硫酸溶液45份;巯丙基甲基二甲氧基硅烷修饰的硅藻土各组分的重量份为:预处理的硅藻土40份、巯丙基甲基二甲氧基硅烷硫酸溶液2份、水58份;三聚氰胺包覆的硅藻土各组分的重量份为:巯丙基甲基二甲氧基硅烷修饰的硅藻土35份、三聚氰胺18份,水47份。
分散机为手摇升降分散机;超声辅助分散的超声波频率为30kHz,分散时间为40min;脉冲激光器采用钕玻璃激光器;脉冲激光烧结的初始能量为20J,终止能量为90J,脉冲能量升高速度为1J/s,升高到终止能量后继续反应10min。
实施例4
a、将硅藻土加入质量浓度为63%的硫酸溶液中,搅拌均匀后煮沸2.5h,使硅藻土中的杂质与硫酸反应生成可溶性盐类,经压滤、洗涤、干燥,得到预处理的硅藻土;
b、将步骤a中预处理的硅藻土加入水中,分散均匀,再加入巯丙基甲基二甲氧基硅烷,混合搅拌分散,得到巯丙基甲基二甲氧基硅烷修饰的硅藻土;
c、将步骤b制得的巯丙基甲基二甲氧基硅烷修饰的硅藻土加入水中,置于分散机中,然后加入三聚氰胺,进行超声辅助分散,干燥后制得三聚氰胺包覆的硅藻土;
d、将步骤c制得的三聚氰胺包覆的硅藻土置入氮气气氛中,采用脉冲激光器缓慢升高能量,对硅藻土表面进行脉冲激光烧结,洗涤,干燥,得到具有可见光响应的氮化碳硅藻土,即为用于污水处理的氮化碳-硅藻土。
预处理的硅藻土各组分的重量份为:硅藻土52份、硫酸溶液48份;巯丙基甲基二甲氧基硅烷修饰的硅藻土各组分的重量份为:预处理的硅藻土36份、巯丙基甲基二甲氧基硅烷硫酸溶液1份、水63份;三聚氰胺包覆的硅藻土各组分的重量份为:巯丙基甲基二甲氧基硅烷修饰的硅藻土32份、三聚氰胺15份,水53份。
分散机为压升降分散机;超声辅助分散的超声波频率为22kHz,分散时间为55min;脉冲激光器采用氮分子激光器;脉冲激光烧结的初始能量为12J,终止能量为82J,脉冲能量升高速度为0.6J/s,升高到终止能量后继续反应14min。
实施例5
a、将硅藻土加入质量浓度为66%的硫酸溶液中,搅拌均匀后煮沸3h,使硅藻土中的杂质与硫酸反应生成可溶性盐类,经压滤、洗涤、干燥,得到预处理的硅藻土;
b、将步骤a中预处理的硅藻土加入水中,分散均匀,再加入巯丙基甲基二甲氧基硅烷,混合搅拌分散,得到巯丙基甲基二甲氧基硅烷修饰的硅藻土;
c、将步骤b制得的巯丙基甲基二甲氧基硅烷修饰的硅藻土加入水中,置于分散机中,然后加入三聚氰胺,进行超声辅助分散,干燥后制得三聚氰胺包覆的硅藻土;
d、将步骤c制得的三聚氰胺包覆的硅藻土置入氮气气氛中,采用脉冲激光器缓慢升高能量,对硅藻土表面进行脉冲激光烧结,洗涤,干燥,得到具有可见光响应的氮化碳硅藻土,即为用于污水处理的氮化碳-硅藻土。
预处理的硅藻土各组分的重量份为:硅藻土54份、硫酸溶液46份;巯丙基甲基二甲氧基硅烷修饰的硅藻土各组分的重量份为:预处理的硅藻土38份、巯丙基甲基二甲氧基硅烷硫酸溶液2份、水60份;三聚氰胺包覆的硅藻土各组分的重量份为:巯丙基甲基二甲氧基硅烷修饰的硅藻土34份、三聚氰胺17份,水49份。
分散机为气动升降分散机;超声辅助分散的超声波频率为26kHz,分散时间为46min;脉冲激光器采用准分子激光器;脉冲激光烧结的初始能量为16J,终止能量为88J,脉冲能量升高速度为0.8J/s,升高到终止能量后继续反应13min。
对比例1
a、将硅藻土加入质量浓度为65%的硫酸溶液中,搅拌均匀后煮沸2.5h,使硅藻土中的杂质与硫酸反应生成可溶性盐类,经压滤、洗涤、干燥,得到预处理的硅藻土;
b、将步骤a制得的预处理的硅藻土加入水中,置于分散机中,然后加入三聚氰胺,进行超声辅助分散,干燥后制得三聚氰胺包覆的硅藻土;
c、将步骤b制得的三聚氰胺包覆的硅藻土置入氮气气氛中,采用脉冲激光器缓慢升高能量,对硅藻土表面进行脉冲激光烧结,洗涤,干燥,得到具有可见光响应的氮化碳硅藻土,即为用于污水处理的氮化碳-硅藻土。
预处理的硅藻土各组分的重量份为:硅藻土53份、硫酸溶液47份;三聚氰胺包覆的硅藻土各组分的重量份为:预处理的硅藻土33份、三聚氰胺16份,水51份。
分散机为液压升降分散机;超声辅助分散的超声波频率为25kHz,分散时间为50min;脉冲激光器采用钇铝石榴石激光器;脉冲激光烧结的初始能量为15J,终止能量为85J,脉冲能量升高速度为0.8J/s,升高到终止能量后继续反应13min。
上述实施例1~5及对比例1制得的氮化碳硅藻土,测试其催化剂残留率、重金属吸附率及有机物降解率,测试表征的方法或条件如下:
催化剂残留率:采用超声清洗机对氮化碳硅藻土进行超声清洗,测定清洗试验前后催化剂的质量比,计算催化剂残留率,表征氮化碳与硅藻土的结合力。
重金属吸附率:采用重金属检测仪,测试本发明产品对污水中铅、镉及铜的吸附量,计算重金属吸附率,表征吸附性能。
有机物降解率:可见光强度为20000lux,照射时间为2h,光催化剂的使用量为3%,测试降解有机物的质量百分比,即为有机物降解率,表征其光催化性能。
结果如表1所示。
表1:
Claims (7)
1.一种用于污水处理的氮化碳-硅藻土的制备方法,其特征在于:所述氮化碳-硅藻土经酸洗处理后,由巯丙基甲基二甲氧基硅烷进行修饰,再由三聚氰胺包覆后采用脉冲激光烧结,制得可见光响应的氮化碳-硅藻土,具体的制备步骤为:
a、将硅藻土加入质量浓度为60~70%的硫酸溶液中,搅拌均匀后煮沸2~3h,使硅藻土中的杂质与硫酸反应生成可溶性盐类,经压滤、洗涤、干燥,得到预处理的硅藻土;
b、将步骤a中预处理的硅藻土加入水中,分散均匀,再加入巯丙基甲基二甲氧基硅烷,混合搅拌分散,得到巯丙基甲基二甲氧基硅烷修饰的硅藻土;
c、将步骤b制得的巯丙基甲基二甲氧基硅烷修饰的硅藻土加入水中,置于分散机中,然后加入三聚氰胺,进行超声辅助分散,干燥后制得三聚氰胺包覆的硅藻土;
d、将步骤c制得的三聚氰胺包覆的硅藻土置入氮气气氛中,采用脉冲激光器缓慢升高能量,对硅藻土表面进行脉冲激光烧结,三聚氰胺的分子链断裂后,在硅藻土表面和微孔中形成一层氮化碳,洗涤,干燥,得到具有可见光响应的氮化碳硅藻土,即为用于污水处理的氮化碳-硅藻土。
2.根据权利要求1所述一种用于污水处理的氮化碳-硅藻土的制备方法,其特征在于:所述硅藻土的比表面积为40~60m2/g,孔隙率为80~85%,孔体积0.5~0.9m3/g。
3.根据权利要求1所述一种用于污水处理的氮化碳-硅藻土的制备方法,其特征在于:步骤b中,按重量份计:预处理的硅藻土35~40份、巯丙基甲基二甲氧基硅烷硫酸溶液1~2份、水58~64份。
4.根据权利要求1所述一种用于污水处理的氮化碳-硅藻土的制备方法,其特征在于:步骤c中,按重量份计:巯丙基甲基二甲氧基硅烷修饰的硅藻土30~35份、三聚氰胺14~18份,水47~56份。
5.根据权利要求1所述一种用于污水处理的氮化碳-硅藻土的制备方法,其特征在于:步骤c所述超声辅助分散的超声波频率为20~30kHz,分散时间为40~60min。
6.根据权利要求1所述一种用于污水处理的氮化碳-硅藻土的制备方法,其特征在于:步骤d所述脉冲激光器采用钇铝石榴石激光器、红宝石激光器、钕玻璃激光器、氮分子激光器或准分子激光器中的一种。
7.根据权利要求1所述一种用于污水处理的氮化碳-硅藻土的制备方法,其特征在于:步骤d所述脉冲激光烧结的初始能量为10~20J,终止能量为80~90J,脉冲能量升高速度为0.5~1J/s,升高到终止能量后继续反应10~15min。
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CN112756008A (zh) * | 2021-01-13 | 2021-05-07 | 合肥工业大学 | 一种铁掺杂氮化碳硅藻土复合材料及其制备方法、应用 |
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CN112756008A (zh) * | 2021-01-13 | 2021-05-07 | 合肥工业大学 | 一种铁掺杂氮化碳硅藻土复合材料及其制备方法、应用 |
CN114717118A (zh) * | 2022-05-19 | 2022-07-08 | 中南大学 | 一种载银硅藻材料及其制备方法和应用 |
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