CN106944040B - 利用含钛矿渣和含锰矿渣制备氮氧化物净化催化剂的方法 - Google Patents
利用含钛矿渣和含锰矿渣制备氮氧化物净化催化剂的方法 Download PDFInfo
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- CN106944040B CN106944040B CN201710147782.5A CN201710147782A CN106944040B CN 106944040 B CN106944040 B CN 106944040B CN 201710147782 A CN201710147782 A CN 201710147782A CN 106944040 B CN106944040 B CN 106944040B
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- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitrogen oxide Substances 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O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 239000011572 manganese Substances 0.000 title claims abstract description 73
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 71
- 239000002893 slag Substances 0.000 title claims abstract description 66
- PWHULOQIROXLJO-UHFFFAOYSA-N manganese Chemical compound 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[Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 60
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- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 45
- 239000010936 titanium Substances 0.000 title claims abstract description 45
- 239000003054 catalyst Substances 0.000 title claims abstract description 41
- 229910052813 nitrogen oxide Inorganic materials 0.000 title claims abstract description 32
- 238000000746 purification Methods 0.000 title claims abstract description 30
- 238000000227 grinding Methods 0.000 claims abstract description 47
- 239000000843 powder Substances 0.000 claims abstract description 42
- 238000000498 ball milling Methods 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 26
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- BDAGIHXWWSANSR-UHFFFAOYSA-N formic acid Chemical compound 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- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 30
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Chemical group data:image/svg+xml;base64,PD94bWwgdmVyc2lvbj0nMS4wJyBlbmNvZGluZz0naXNvLTg4NTktMSc/Pgo8c3ZnIHZlcnNpb249JzEuMScgYmFzZVByb2ZpbGU9J2Z1bGwnCiAgICAgICAgICAgICAgeG1sbnM9J2h0dHA6Ly93d3cudzMub3JnLzIwMDAvc3ZnJwogICAgICAgICAgICAgICAgICAgICAgeG1sbnM6cmRraXQ9J2h0dHA6Ly93d3cucmRraXQub3JnL3htbCcKICAgICAgICAgICAgICAgICAgICAgIHhtbG5zOnhsaW5rPSdodHRwOi8vd3d3LnczLm9yZy8xOTk5L3hsaW5rJwogICAgICAgICAgICAgICAgICB4bWw6c3BhY2U9J3ByZXNlcnZlJwp3aWR0aD0nMzAwcHgnIGhlaWdodD0nMzAwcHgnIHZpZXdCb3g9JzAgMCAzMDAgMzAwJz4KPCEtLSBFTkQgT0YgSEVBREVSIC0tPgo8cmVjdCBzdHlsZT0nb3BhY2l0eToxLjA7ZmlsbDojRkZGRkZGO3N0cm9rZTpub25lJyB3aWR0aD0nMzAwLjAnIGhlaWdodD0nMzAwLjAnIHg9JzAuMCcgeT0nMC4wJz4gPC9yZWN0Pgo8dGV4dCB4PSczOC43JyB5PScxNzAuMCcgY2xhc3M9J2F0b20tMCcgc3R5bGU9J2ZvbnQtc2l6ZTo0MHB4O2ZvbnQtc3R5bGU6bm9ybWFsO2ZvbnQtd2VpZ2h0Om5vcm1hbDtmaWxsLW9wYWNpdHk6MTtzdHJva2U6bm9uZTtmb250LWZhbWlseTpzYW5zLXNlcmlmO3RleHQtYW5jaG9yOnN0YXJ0O2ZpbGw6I0U4NDIzNScgPkg8L3RleHQ+Cjx0ZXh0IHg9JzY0LjMnIHk9JzE3MC4wJyBjbGFzcz0nYXRvbS0wJyBzdHlsZT0nZm9udC1zaXplOjQwcHg7Zm9udC1zdHlsZTpub3JtYWw7Zm9udC13ZWlnaHQ6bm9ybWFsO2ZpbGwtb3BhY2l0eToxO3N0cm9rZTpub25lO2ZvbnQtZmFtaWx5OnNhbnMtc2VyaWY7dGV4dC1hbmNob3I6c3RhcnQ7ZmlsbDojRTg0MjM1JyA+TzwvdGV4dD4KPHRleHQgeD0nOTEuOScgeT0nMTU0LjAnIGNsYXNzPSdhdG9tLTAnIHN0eWxlPSdmb250LXNpemU6MjZweDtmb250LXN0eWxlOm5vcm1hbDtmb250LXdlaWdodDpub3JtYWw7ZmlsbC1vcGFjaXR5OjE7c3Ryb2tlOm5vbmU7Zm9udC1mYW1pbHk6c2Fucy1zZXJpZjt0ZXh0LWFuY2hvcjpzdGFydDtmaWxsOiNFODQyMzUnID4tPC90ZXh0Pgo8dGV4dCB4PScyMDAuNycgeT0nMTcwLjAnIGNsYXNzPSdhdG9tLTEnIHN0eWxlPSdmb250LXNpemU6NDBweDtmb250LXN0eWxlOm5vcm1hbDtmb250LXdlaWdodDpub3JtYWw7ZmlsbC1vcGFjaXR5OjE7c3Ryb2tlOm5vbmU7Zm9udC1mYW1pbHk6c2Fucy1zZXJpZjt0ZXh0LWFuY2hvcjpzdGFydDtmaWxsOiMzQjQxNDMnID5OPC90ZXh0Pgo8dGV4dCB4PScyMjguMycgeT0nMTcwLjAnIGNsYXNzPSdhdG9tLTEnIHN0eWxlPSdmb250LXNpemU6NDBweDtmb250LXN0eWxlOm5vcm1hbDtmb250LXdlaWdodDpub3JtYWw7ZmlsbC1vcGFjaXR5OjE7c3Ryb2tlOm5vbmU7Zm9udC1mYW1pbHk6c2Fucy1zZXJpZjt0ZXh0LWFuY2hvcjpzdGFydDtmaWxsOiMzQjQxNDMnID5hPC90ZXh0Pgo8dGV4dCB4PScyNDkuNicgeT0nMTU0LjAnIGNsYXNzPSdhdG9tLTEnIHN0eWxlPSdmb250LXNpemU6MjZweDtmb250LXN0eWxlOm5vcm1hbDtmb250LXdlaWdodDpub3JtYWw7ZmlsbC1vcGFjaXR5OjE7c3Ryb2tlOm5vbmU7Zm9udC1mYW1pbHk6c2Fucy1zZXJpZjt0ZXh0LWFuY2hvcjpzdGFydDtmaWxsOiMzQjQxNDMnID4rPC90ZXh0Pgo8L3N2Zz4K data:image/svg+xml;base64,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 [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- -1 polytetrafluoroethylene Polymers 0.000 claims description 17
- 239000004615 ingredient Substances 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 14
- 235000019441 ethanol Nutrition 0.000 claims description 12
- 235000019253 formic acid Nutrition 0.000 claims description 11
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound 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- VHUUQVKOLVNVRT-UHFFFAOYSA-N ammonium hydroxide Chemical compound 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[NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 239000000908 ammonium hydroxide Substances 0.000 claims description 2
- 239000003818 cinder Substances 0.000 claims description 2
- 239000000284 extract Substances 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 230000005611 electricity Effects 0.000 claims 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N magnesium Chemical compound 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[Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims 1
- 239000011777 magnesium Substances 0.000 claims 1
- 229910052749 magnesium Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000011812 mixed powder Substances 0.000 abstract description 4
- 239000002910 solid waste Substances 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials 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- 238000002360 preparation method Methods 0.000 description 8
- UGFAIRIUMAVXCW-UHFFFAOYSA-N carbon monoxide Chemical compound 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[O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 6
- 239000003546 flue gas Substances 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 239000007789 gas Substances 0.000 description 4
- 229910052689 Holmium Inorganic materials 0.000 description 3
- 210000002268 Wool Anatomy 0.000 description 3
- 239000003708 ampul Substances 0.000 description 3
- 230000003197 catalytic Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium Chemical compound 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[Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052904 quartz Inorganic materials 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- VTHJTEIRLNZDEV-UHFFFAOYSA-L Magnesium hydroxide Chemical compound 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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
本发明公开了一种利用含钛矿渣和含锰矿渣制备氮氧化物净化催化剂的方法,其步骤:(1)将含钛矿渣和含锰矿渣分别进行研磨,制成含钛矿渣粉末和含锰矿渣粉末;(2)将含钛矿渣粉末加入到酸性活化剂溶液中球磨混合,得到酸性混合料;(3)将含锰矿渣粉末加入到碱性活化剂中球磨混合,得到碱性混合料;(4)将步骤(2)所得含钛矿渣活化粉末与步骤(3)所得含锰矿渣活化粉末与醇类助磨剂球磨混合后,得到含钛‑锰矿渣混合粉末;(5)将含钛‑锰混合矿渣粉末,用离心机分离,得到的糊状固体物质,再冲洗,分离,得到固体物,再放入干燥箱干燥,用200目筛进行筛分,制得氮氧化物净化催化剂。该催化剂制备方法简便,周期短,成本低,能实现固体废弃物资源化利用。
Description
技术领域
本发明涉及固体废物处理资源化技术领域,具体涉及一种利用含钛矿渣和含锰矿渣制备氮氧化物净化催化剂的方法。
背景技术
目前我国含钛渣和含锰渣是较为常见的工业固体废弃物,没有充分资源化利用,处于堆弃处置的状态,或是集中在土地中作为软土固化剂,或是作为路基材料回填土, 或是作为硫酸盐水泥制作为硫酸盐水泥缓凝剂,并未将矿渣中钛和锰元素充分利用。含钛渣和含锰渣中一些毒重金属如铅、铬、锰等在自然环境中将慢慢溶出进入地下水体系中,引发严重的重金属污染,会造成环境危害。
在工业上,钛和锰可被应用于氮氧化物净化催化剂的制备。此类催化剂一般以锐钛矿结构的TiO2作为载体,再加入锰氧化物作为活性组分,例如,中国专利,专利号201610027417.6,名称为“一种钬改性的锰钛复合氧化物低温脱硝催化剂及其制备方法” ,该催化剂为钬改性的锰钛复合氧化物,钬的改性提高了催化剂的高温稳定性能,使催化剂的氮气选择性显著提高。但是,现有的催化剂主要是以纯物质组成,具有高成本,周期长,工艺过程复杂的问题。因此,利用含钛含锰渣制备氮氧化物净化催化剂是废物综合利用的新途径。
发明内容
针对现有技术的不足, 本发明的目的是提出一种利用含钛矿渣和含锰矿渣制备氮氧化物净化催化剂的方法,该净化催化剂制备方法简便,周期短,制备成本低,并能实现工业固体废弃物资源化利用。
为了实现上述目的,本发明提供如下技术方案:
一种利用含钛矿渣和含锰矿渣制备氮氧化物净化催化剂的方法,具体包括以下步骤:
(1). 将含钛矿渣和含锰矿渣分别放入球磨罐中进行研磨,分别制成含钛矿渣粉末和含锰矿渣粉末;
(2). 将步骤(1)中所得的含钛矿渣粉末加入到浓度1~4mol•L-1的酸性活化剂溶液中,调节pH值至1~2,按含钛矿渣粉末和酸性活化剂固液比为(1~4):20的比例混合,得到酸性混合料;然后,选取两种不同粒径的玛瑙球,将不同粒径的玛瑙球混合成混合磨球,将混合磨球与上述酸性混合料放入聚四氟乙烯球磨罐,再将球磨罐放入球磨机中,以100rpm~300rpm球磨1~10小时, 配料和玛瑙球以球料比为1:4,得到含钛矿渣活化粉末,所述的两种不同粒径的玛瑙球d1、玛瑙球d2质量比为1: (1~10),玛瑙球d1的体积占球磨机罐体积的0.045~0.065%,玛瑙球d2 的体积占球磨机罐体积的0.324~0.524%;
(3). 将步骤(1)中所得的含锰矿渣粉末加入到浓度4~9 mol•L-1的碱性活化剂溶液中,调节pH值至10~12,其中含锰矿渣粉末和碱性活化剂固液比为(1~4):10的比例混合,得到碱性混合料;然后,选取两种不同粒径的玛瑙球,将不同粒径的玛瑙球混合成混合磨球,将混合磨球与上述碱性混合料放入聚四氟乙烯球磨罐,再将球磨罐放入球磨机中,以100rpm~300rpm球磨1~10小时, 配料和玛瑙球以球料比为1:5,得到含锰矿渣活化粉末,所述的两种不同粒径的玛瑙球d1、玛瑙球d2质量比为1: (5~10),玛瑙球d1的体积占球磨机罐体积的0.065%,玛瑙球d2的体积占球磨机罐体积的0.524%;
(4). 将步骤(2)所得的含钛矿渣活化粉末与步骤(3)所得的含锰矿渣活化粉末与醇类助磨剂按照质量比为1:(1~4):(1~3)比例混合,再一起放入聚四氟乙烯球磨罐中,以200rpm~350rpm球磨1~4小时,配料和玛瑙球以球料比为1:6,得到球磨后含钛-锰矿渣混合粉末,所述的两种不同粒径的玛瑙球d1、玛瑙球d2质量比为1: (10~20);玛瑙球d1的体积占球磨机罐体积的0.045~0.065%,玛瑙球d2的体积占球磨机罐体积的0.424~0.524%
(5). 将步骤(4)中球磨后的含钛-锰混合矿渣粉末,从球磨罐取出,用离心机分离,得到的糊状固体物质,再用蒸馏水冲洗,然后离心机分离,得到固体物,再放入40~80℃的干燥箱中干燥15~20小时,烘干后;用200目筛进行筛分,制得氮氧化物净化催化剂。
上述步骤(1)所述的含钛矿渣为高炉矿渣提取钛后的废渣;含锰矿渣为电解含锰废渣。
上述步骤(2)所述的酸性活化剂为甲酸与盐酸的混合物或甲酸与硫酸的混合物,其中盐酸与甲酸体积比例为1:1~1:5,硫酸与甲酸体积比例为1:1~1:4。
上述步骤(3)所述的碱性活化剂是氢氧化钠、氢氧化镁、氨水中的一种。
上述步骤(4)所述的醇类助磨剂是甲醇与乙醇的混合物,其中混合物中甲醇与乙醇体积比例为1:1~1:4。
与现有技术相比,本发明方法有益效果是:
本发明制备氮氧化物净化催化剂的方法利用高能球磨、酸性活化剂和碱性活化剂去调整原有晶相,促进氮氧化物催化剂的形成。其比表面积会增大,同时,晶粒分散均匀,表面孔道增多;其酸性活化剂的浸出作用使得含钛矿渣中的钛组分,向锐钛矿型转变,使得含钛矿渣具有活性组分,能对其中的钙离子组分进行调整,降低碱性的阳离子对催化剂的毒性作用。而碱性活化剂将含锰矿渣中的锰,充分地暴露,使其再次获得活性,在碱性环境下,使锰渣中的硅铝组分和锰结合更好,制得的备氮氧化物净化催化剂方法简便,易操作,周期短,制备成本低,该氮氧化物净化催化剂有利于氮氧化物的催化还原。能实现以固体废弃物为原料,处理有害气体,能实现工业固体废弃物资源化利用。
附图说明
图1为本发明实施例1制备的氮氧化物净化催化剂对一氧化氮的催化效果曲线图;
图2为本发明实施例2制备的氮氧化物净化催化剂对一氧化氮的催化效果曲线图;
图3为本发明实施例3制备的氮氧化物净化催化剂对一氧化氮的催化效果曲线图。
具体实施方式
现将本发明的具体实施例详细叙述如下。
实施例1
一种利用含钛矿渣和含锰矿渣制备氮氧化物净化催化剂的方法,包括以下步骤:
(1). 将含钛矿渣和含锰矿渣分别放入研磨中进行研磨分别制成含钛矿渣粉末和含锰矿渣粉末;
(2). 将步骤(1)中所得的含钛矿渣加入到浓度为1mol·L-1的甲酸溶液中,调节pH值至1,按含钛矿渣粉末和甲酸固液比为1g:20ml比例混合,得到酸性混合料;然后,选取两种不同粒径的球,将不同粒径的磨球混合成混合磨球,将混合磨球与上述酸性混合料放入聚四氟乙烯球磨罐,再将球磨罐放入球磨机中,以100rpm转速球磨5小时, 配料和玛瑙球以球料比为1:4,得到含钛矿渣活化粉末,所述的两种不同粒径的玛瑙球d1、玛瑙球d2质量比为1:10,玛瑙球d1的体积占球磨机罐体积的0.065%,玛瑙球d2的体积占球磨机罐体积的0.524%;
(3). 将步骤(1)中所得的含锰矿渣加入到浓度为9mol·L-1的氢氧化钠溶液中,调节pH值至11,按含锰矿渣和氢氧化钠固液比为1g:10ml比例均匀混合,得到碱性混合料;然后,选取两种不同粒径的磨球,将不同粒径的玛瑙球混合成混合磨球, 将混合磨球与上述碱性混合料放入聚四氟乙烯球磨罐,再将球磨罐放入球磨机中,以100rpm转速球磨5小时,配料和玛瑙球以球料比为1:5,得到含锰矿渣活化粉末,所述的两种不同粒径的玛瑙球d1、玛瑙球d2质量比为1:5,玛瑙球d1的体积占球磨机罐体积的0.065%,玛瑙球d2的体积占球磨机罐体积的0.524%;
(4). 将步骤(2)所得的含钛矿渣活化粉末与步骤(3)所得的含锰矿渣活化粉末与醇类助磨剂按照质量比为1:1:1比例混合,再一起放入聚四氟乙烯球磨罐中,以100rpm转速球磨2小时,配料和玛瑙球以球料比为1:6,得到球磨后含钛-锰矿渣混合粉末,所述的两种不同粒径的玛瑙球d1、玛瑙球d2质量比为1:10;玛瑙球d1的体积占球磨机罐体积的0.065%,玛瑙球d2的体积占球磨机罐体积的0.524%;
(5). 将步骤(4)中球磨后的含钛-锰混合矿渣粉末,从球磨罐取出,用离心机分离,得到的糊状固体物质,再用蒸馏水冲洗,然后再用离心机分离,得到固体物,再放入60℃烘燥箱中干燥15个小时,烘干后;用200目筛进行筛分,制得氮氧化物净化催化剂。
采用下述试验验证本发明的有益效果,称取上述制得的0.1g氮氧化物净化催化剂放入石英管中,其两端放入石英棉固定,放入管式炉中,连接流量控制器;先通入30ml/min的N2清理管路,再通入30ml/min NO气体稳定;然后,再通入1.3ml/min O2和0.3 ml/min NH3进行催化剂活性实验,用烟气分析仪监测模拟烟气,测定100~300℃温度下一氧化氮(NO)的转化率;其测定结果如图1所示,当温度升至100℃时,一氧化氮(NO)的还原率出现明显提高,最终还原率能达97%。
实施例2
一种利用含钛矿渣和含锰矿渣制备氮氧化物净化催化剂的方法,包括以下步骤:
(1). 将含钛矿渣和含锰矿渣分别放入研磨中进行研磨分别制成含钛矿渣粉末和含锰矿渣粉末;
(2). 将步骤(1)中所得的含钛矿渣加入到浓度为4mol·L-1的甲酸溶液中,调节pH值至1,按含钛矿渣粉末和甲酸固液比为2g:20ml比例混合,得到酸性混合料;然后,选取两种不同粒径的玛瑙球,将不同粒径的玛瑙球混合成混合磨球,将混合磨球与上述酸性混合料放入聚四氟乙烯球磨罐,再将球磨罐放入球磨机中,以150rpm转速球磨2小时, 配料和玛瑙球以球料比为1:4,得到含钛矿渣活化粉末,所述的两种不同粒径的玛瑙球d1、玛瑙球d2质量比为1:10,玛瑙球d1的体积占球磨机罐体积的0.065%,玛瑙球d2的体积占球磨机罐体积的0.424%;
(3). 将步骤(1)中所得的含锰矿渣加入到浓度为4mol·L-1的氢氧化镁溶液中,调节pH值至11,按含锰矿渣和氢氧化钠固液比为2g :10ml比例均匀混合,得到碱性混合料;然后,选取两种不同粒径的玛瑙球,将不同粒径的玛瑙球混合成混合磨球, 将混合磨球与上述碱性混合料放入聚四氟乙烯球磨罐,再将球磨罐放入球磨机中,以150rpm转速球磨2小时,配料和玛瑙球以球料比为1:5,得到含锰矿渣活化粉末,所述的两种不同粒径的玛瑙球d1、玛瑙球d2质量比为1:10,玛瑙球d1的体积占球磨机罐体积的0.065%,玛瑙球d2的体积占球磨机罐体积的0.524%;
(4). 将步骤(2)所得的含钛矿渣活化粉末与步骤(3)所得的含锰矿渣活化粉末与醇类助磨剂按照质量比为1:4:3 比例混合,再一起放入聚四氟乙烯球磨罐中,以300rpm转速球磨4小时,配料和玛瑙球以球料比为1:6,得到球磨后含钛-锰矿渣混合粉末,所述的两种不同粒径的玛瑙球d1、玛瑙球d2质量比为1:10;玛瑙球d1的体积占球磨机罐体积的0.045%,玛瑙球d2的体积占球磨机罐体积的0.524%;
(5). 将步骤(4)中球磨后的含钛-锰混合矿渣粉末,从球磨罐取出,用离心机分离,得到的糊状固体物质,再用蒸馏水冲洗,然后再用离心机分离,得到固体物,再放入40℃烘燥箱中干燥20个小时,烘干后;用200目筛进行筛分,制得氮氧化物净化催化剂。
采用下述试验验证本发明的有益效果,称取上述制得的0.1g氮氧化物净化催化剂,称取上述制得的0.1g氮氧化物净化催化剂放入石英管中,其两端放入石英棉固定,放入管式炉中,连接流量控制器;先通入30ml/min的N2清理管路,再通入30ml/min NO气体稳定;然后,再通入1.3ml/min O2和0.3 ml/min NH3进行催化剂活性实验,用烟气分析仪监测模拟烟气,测定100~300℃温度下一氧化氮(NO)转化率;其测定结果如图2所示,当温度升至100℃时,一氧化氮(NO)的还原率出现明显提高,最终还原率能达92%。
实施例3
一种利用含钛矿渣和含锰矿渣制备氮氧化物净化催化剂的方法,具体包括以下步骤:
(1). 将含钛矿渣和含锰矿渣分别放入研磨中进行研磨分别制成含钛矿渣粉末和含锰矿渣粉末;
(2). 将步骤(1)中所得的含钛矿渣加入到浓度为4mol·L-1的混合酸(盐酸:甲酸=1:1)溶液中,调节pH值至1,按含钛矿渣粉末和混合酸固液比为1g:10ml比例混合,得到酸性混合料;然后,选取两种不同粒径的球,将不同粒径的磨球混合成混合磨球,将混合磨球与上述酸性混合料放入聚四氟乙烯球磨罐,再将球磨罐放入球磨机中,以200rpm转速球磨4小时, 配料和玛瑙球以球料比为1:4,得到含钛矿渣活化粉末,所述的两种不同粒径的玛瑙球d1、玛瑙球d2质量比为1:1,玛瑙球d1的体积占球磨机罐体积的0.065%,玛瑙球d2的体积占球磨机罐体积的0.324%;
(3). 将步骤(1)中所得的含锰矿渣加入到浓度为4mol·L-1的氨水溶液中,调节pH值至11,按含锰矿渣和氢氧化钠固液比为1g :10ml比例均匀混合,得到碱性混合料;然后,选取两种不同粒径的磨球,将不同粒径的玛瑙球混合成混合磨球, 将混合磨球与上述碱性混合料放入聚四氟乙烯球磨罐,再将球磨罐放入球磨机中,以200rpm转速球磨4小时, 配料和玛瑙球以球料比为1:5,得到含锰矿渣活化粉末,所述的两种不同粒径的玛瑙球d1、玛瑙球d2质量比为1:10,玛瑙球d1的体积占球磨机罐体积的0.065%,玛瑙球d2的体积占球磨机罐体积的0.524%;
(4). 将步骤(2)所得的含钛矿渣活化粉末与步骤(3)所得的含锰矿渣活化粉末与醇类助磨剂按照质量比为1:2:2 比例混合,再一起放入聚四氟乙烯球磨罐中,以200rpm转速球磨4小时,配料和玛瑙球以球料比为1:6,得到球磨后含钛-锰矿渣混合粉末,所述的两种不同粒径的玛瑙球d1、玛瑙球d2质量比为1:20;玛瑙球d1的体积占球磨机罐体积的0.055%,玛瑙球d2的体积占球磨机罐体积的0.424%;
(5). 将步骤(4)中球磨后的含钛-锰混合矿渣粉末,从球磨罐取出,用离心机分离,得到的糊状固体物质,再用蒸馏水冲洗,然后再用离心机分离,得到固体物,再放入50℃烘燥箱中干燥20个小时,烘干后;用200目筛进行筛分,制得氮氧化物净化催化剂。
采用下述试验验证本发明的有益效果,称取上述制得的0.1g氮氧化物净化催化剂,称取上述制得的0.1g氮氧化物净化催化剂放入石英管中,其两端放入石英棉固定,放入管式炉中,连接流量控制器;先通入30ml/min的N2清理管路,再通入30ml/min NO气体稳定;然后,再通入1.3ml/min O2和0.3 ml/min NH3进行催化剂活性实验,用烟气分析仪监测模拟烟气,测定100~300℃温度下一氧化氮(NO)的转化率;其测定结果如图3所示,当温度升至100℃时,一氧化氮(NO)的还原率出现明显提高,最终还原率能达96%。
Claims (3)
1.一种利用含钛矿渣和含锰矿渣制备氮氧化物净化催化剂的方法,其特征在于,该方法具体包括以下步骤:
(1).将含钛矿渣和含锰矿渣分别放入球磨罐中进行研磨,分别制成含钛矿渣粉末和含锰矿渣粉末;
(2).将步骤(1)中所得的含钛矿渣粉末加入到浓度1~4mol·L-1的酸性活化剂溶液中,调节pH值至1~2,按含钛矿渣粉末和酸性活化剂固液比为(1~4):20的比例混合,得到酸性混合料,所述固液比为所述含钛矿渣粉末的质量和所述酸性活化剂的体积比,单位为g:mL;然后,选取两种不同粒径的玛瑙球,将不同粒径的玛瑙球混合成混合磨球,将混合磨球与上述酸性混合料放入聚四氟乙烯球磨罐,再将球磨罐放入球磨机中,以100rpm~300rpm球磨1~10小时,配料和玛瑙球以球料比为1:4,得到含钛矿渣活化粉末,所述的两种不同粒径的玛瑙球d1、玛瑙球d2质量比为1:(1~10),玛瑙球d1的体积占球磨机罐体积的0.045~0.065%,玛瑙球d2的体积占球磨机罐体积的0.324~0.524%;所述的酸性活化剂为甲酸与盐酸的混合物或甲酸与硫酸的混合物,其中盐酸与甲酸体积比例为1:1~1:5,硫酸与甲酸体积比例为1:1~1:4;
(3).将步骤(1)中所得的含锰矿渣粉末加入到浓度4~9mol·L-1的碱性活化剂溶液中,调节pH值至10~12,其中含锰矿渣粉末和碱性活化剂固液比为(1~4):10的比例混合,得到碱性混合料,所述固液比为所述含锰矿渣粉末的质量和所述碱性活化剂的体积比,单位为g:mL ;然后,选取两种不同粒径的玛瑙球,将不同粒径的玛瑙球混合成混合磨球,将混合磨球与上述碱性混合料放入聚四氟乙烯球磨罐,再将球磨罐放入球磨机中,以100rpm~300rpm球磨1~10小时,配料和玛瑙球以球料比为1:5,得到含锰矿渣活化粉末,所述的两种不同粒径的玛瑙球d1、玛瑙球d2质量比为1:(5~10),玛瑙球d1的体积占球磨机罐体积的0.065%,玛瑙球d2的体积占球磨机罐体积的0.524%;所述的碱性活化剂是氢氧化钠、氢氧化镁、氨水中的一种;
(4).将步骤(2)所得的含钛矿渣活化粉末与步骤(3)所得的含锰矿渣活化粉末与醇类助磨剂按照质量比为1:(1~4):(1~3)比例混合,再一起放入聚四氟乙烯球磨罐中,以200rpm~350rpm球磨1~4小时,配料和玛瑙球以球料比为1:6,得到球磨后含钛-锰矿渣混合粉末,所述的两种不同粒径的玛瑙球d1、玛瑙球d2质量比为1:(10~20);玛瑙球d1的体积占球磨机罐体积的0.045~0.065%,玛瑙球d2的体积占球磨机罐体积的0.424~0.524%
(5).将步骤(4)中球磨后的含钛-锰混合矿渣粉末,从球磨罐取出,用离心机分离,得到的糊状固体物质,再用蒸馏水冲洗,然后离心机分离,得到固体物,再放入40~80℃的干燥箱中干燥15~20小时,烘干后;用200目筛进行筛分,制得氮氧化物净化催化剂。
2.根据权利要求1所述的一种利用含钛矿渣和含锰矿渣制备氮氧化物净化催化剂的方法,其特征在于,上述步骤(1)所述的含钛矿渣为高炉矿渣提取钛后的废渣;含锰矿渣为电解含锰废渣。
3.根据权利要求1所述的一种利用含钛矿渣和含锰矿渣制备氮氧化物净化催化剂的方法,其特征在于,上述步骤(4)所述的醇类助磨剂是甲醇与乙醇的混合物,其中混合物中甲醇与乙醇体积比例为1:1~1:4。
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