WO2017117861A1 - 空气杀菌消毒净化用催化剂及其制备方法 - Google Patents

空气杀菌消毒净化用催化剂及其制备方法 Download PDF

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WO2017117861A1
WO2017117861A1 PCT/CN2016/075854 CN2016075854W WO2017117861A1 WO 2017117861 A1 WO2017117861 A1 WO 2017117861A1 CN 2016075854 W CN2016075854 W CN 2016075854W WO 2017117861 A1 WO2017117861 A1 WO 2017117861A1
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catalyst
chlorite
chlorine dioxide
solution
air
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French (fr)
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李国培
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深圳市康风环境科技发展有限公司
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Priority to US15/554,020 priority Critical patent/US10183187B2/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8678—Removing components of undefined structure
    • B01D53/8687—Organic components
    • A—HUMAN NECESSITIES
    • A62—LIFE-SAVING; FIRE-FIGHTING
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    • A62D3/17—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by subjecting to electric or wave energy or particle or ionizing radiation to electromagnetic radiation, e.g. emitted by a laser
    • A62D3/176—Ultraviolet radiations, i.e. radiation having a wavelength of about 3nm to 400nm
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/06—Halogens; Compounds thereof
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    • B01D—SEPARATION
    • B01D2251/00—Reactants
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    • B01D—SEPARATION
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    • B01D2255/70—Non-metallic catalysts, additives or dopants
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/80—Type of catalytic reaction
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D2257/91—Bacteria; Microorganisms
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    • B01D2258/00—Sources of waste gases
    • B01D2258/06—Polluted air

Definitions

  • the invention belongs to the field of green chemistry advanced oxidation technology and environmental engineering application, and relates to preparing active particles such as gas phase radicals OH, ⁇ ClO 2 , ⁇ HO 2 , ⁇ O in a gaseous condition and inducing a chain reaction.
  • Microbial pollutants and chemical pollutants in air pollution are usually purified by adsorption, photocatalysis, negative ions, plasma, ozone, and the like.
  • the high-concentration ozone purification method is most effective.
  • the standard electrode potential of ozone is 2.07 volts, and the chemical reaction rate constant is 10 1 to 10 2 L/(mol ⁇ s).
  • the ozone kills mold in the gas phase (microbial contamination)
  • One of the more difficult to kill) time needs 100min
  • ozone purification still has shortcomings, and ozone is harmful to the human body, and indoor air sterilization and purification can not coexist.
  • OH has a stronger oxidizing power (standard electrode potential 2.80 volts), which is almost equivalent to the oxidizing ability of elemental fluorine (2.87 volts) and is a strong oxidizing substance.
  • the reaction of ⁇ OH is a radical reaction with a very high chemical reaction rate of 10 7 to 10 9 L/(mol ⁇ s), which is 7 orders of magnitude higher than ozone.
  • the chemical reaction time is less than 1 s, and the biochemical reaction time is 1 to 10 s.
  • the surface of the silica has a strong affinity for water, and the water molecules can be irreversibly or reversibly adsorbed on the surface, so the surface of the silica is usually covered by a layer of OH (hydroxyl) and water.
  • the former is a hydroxyl group bonded to the surface Si atom, that is, chemisorbed water; the latter is water adsorbed on the surface molecule, that is, physically adsorbed water.
  • ClO 2 causes ionized hydrolysis of the physical water (small amount) on the surface of the silica by H 2 O in the absence of light or heat.
  • H + + OH - in addition to the slow hydrolysis of ClO 2 + H 2 O ⁇ HClO 2 + HClO 3 , there is also non-ionic hydrolysis of chemisorbed water:
  • non-ionized hydrolysis (radical type) is not remarkable in general, but is greatly accelerated when a substrate is reacted with it or physically or chemically catalyzed, so that a large amount of ⁇ OH is formed.
  • the surface of the active alumina has a surface hydroxyl group which is generated by adsorbing water, the properties of the above silica are also present.
  • the object of the present invention is to solve the prior art deficiencies in the application of advanced oxidation technology in the treatment of pollutants under gaseous conditions, and to provide an air pollution capable of preparing gas phase free radicals OH, ⁇ ClO 2 , ⁇ HO 2 , ⁇ O on a scale.
  • the new method of treatment improves the removal efficiency, has no secondary pollution, has a long service life, is simple and reliable, can be co-located, and has been applied in practice.
  • the catalyst carrier may be silica, zeolite, sepiolite, diatomaceous earth, montmorillonite, alumina trioxide inorganic porous material (particle size ⁇ 100 mesh), preferably 2-3 mm, 3- 5mm, which may be any one of them, or a mixture or composite of various kinds, impregnated stable chlorine dioxide solution or stable chlorite solution, dried at 85 ° C or lower, and the water content is ⁇ 8%.
  • the catalyst carrier can also be passed through a structured carrier, cordierite honeycomb ceramic or mullite honeycomb ceramic (pore density 50 mesh - 900 mesh), preferably 400 mesh, size 150 x 150 mm, thickness can be arbitrarily set as needed Preferably, it is 25 mm, 50 mm, 100 mm, and 150 mm.
  • the impregnated stable chlorine dioxide solution or the stabilized sodium chlorite solution is dried at 85 ° C or lower to a moisture content of ⁇ 8%.
  • UV lamp irradiation After UV lamp irradiation, it produces active particles such as ⁇ OH, ⁇ ClO 2 , ⁇ HO 2 , ⁇ O, induce chain reaction, and quickly kill viruses, bacteria, mold and chemical pollution. The substance eventually becomes carbon dioxide, water and trace mineral salts. 2.
  • active particles such as ⁇ OH, ⁇ ClO 2 , ⁇ HO 2 , ⁇ O
  • UV lamp irradiation After UV lamp irradiation, it produces active particles such as ⁇ OH, ⁇ ClO 2 , ⁇ HO 2 , ⁇ O, induce chain reaction, and quickly kill viruses, bacteria, mold and chemical pollution. The substance eventually becomes carbon dioxide, water and trace mineral salts.
  • it can be directly used as a catalytic oxidation material without ultraviolet light irradiation. It can also degrade chemical pollutants and kill viruses, bacteria, molds and other microorganisms, but the purification efficiency is slightly lower than the first method. To achieve the same purification effect, the amount of catalyst used is
  • the first scheme preparing a stable chlorine dioxide solution, using a high-purity chlorine dioxide generator to obtain chlorine dioxide gas with a purity of ⁇ 98%, and sodium peroxyhydrate hydrate (chemical formula Na 2 CO 3 ⁇ mH 2 O 2 ⁇ nH 2 O) As a stabilizer, a certain proportion of the absorption liquid is prepared, and finally a solution having a chlorine dioxide content of 2% to 5% is prepared.
  • the second scheme preparing a stable sodium chlorite solution, the content of each component in the solution is as follows: chlorite 0.1-10, stabilizer 0.1-5, buffer 0.05-15, absorbent 0.1-75.
  • Chlorite refers to a salt containing chlorite ion ClO 2 — for example, sodium chlorite, potassium chlorite, lithium chlorite.
  • Stabilizers are also strong oxidizing agents such as potassium permanganate, H 2 O 2 , perchlorates, nitrates, and the like.
  • Buffering agent refers to a substance which can maintain a substantially constant pH value of a solution within a certain range, generally a salt.
  • a salt of a weak base such as sodium carbonate or borate or citrate can be used.
  • Absorbent refers to chemical absorbent, and there is a chemical reaction between it and solute.
  • the solubility of solute is not only related to the law of gas-liquid equilibrium, but also related to the chemical equilibrium law.
  • Chemical absorbent Most are solutions of certain active components, such as aqueous solutions of potassium carbonate, sodium carbonate, sodium hydroxide, potassium hydroxide, and the like.
  • the three bands of wavelengths A, B, and C can excite the catalytic material to produce active particles such as gas phase radicals OH, ⁇ ClO 2 , ⁇ HO 2 , ⁇ O, as long as the irradiation intensity is the same.
  • LED lights or mercury UV lamps have basically the same effect.
  • the central air supply filter system uses a catalyst with a peak of ceramics as a carrier (small wind resistance) to be irradiated by a C-band (185 nm) ultraviolet lamp generated by ozone, and the purification effect is particularly good.
  • the existing photocatalytic oxidation technology or the normal temperature multi-phase catalytic oxidation technology will greatly reduce the purification efficiency of the pollutants, but the catalyst of the present invention will not be affected by the humidity. This kind of meteorological conditions will often appear in life.
  • Figure 1 is a particle catalyst installed test prototype KF-501A of the present invention.
  • Figure 2 shows the above-mentioned sample sterilization rate detection data.
  • Figure 3 shows the sample detection data in addition to formaldehyde.
  • Figure 4 shows the comparison of the formaldehyde removal curve of the above prototype with the well-known brand purifier and high concentration ozone.
  • Figure 5 shows the minimum power removal formaldehyde curve of the above-mentioned sample in addition to the formaldehyde curve and the maximum power of the famous Swiss brand I.
  • a stable sodium chlorite stabilizing solution is prepared, and 5000 ml of purified water is weighed, 400 g of 80% sodium chlorite is weighed, and after dissolving in water, 100 g of sodium chloride is weighed and continuously stirred and dissolved in water, and then Add 20 g of sodium borate tetrahydrate, and finally add 20 ml of 30% hydrogen peroxide, stir, filter, and finally adjust the pH between 8.0-9.5 with sodium carbonate.

Abstract

一种空气中杀菌消毒净化用催化剂的使用方法，催化剂是以二氧化硅、沸石、硅藻土、海泡石、蒙脱石及三氧化二铝等无机多孔材料或堇青石、莫来石蜂窝陶瓷作为载体，浸渍亚氯酸钠稳定液或二氧化氯稳定液，干燥而成，在室温条件下经紫外线灯照射，产生气相自由基·OH、·ClO 2、·HO 2、·O等活性粒子，杀灭空气中的病毒、细菌和霉菌等微生物性污染物，去除甲醛等化学性污染物。

Description

空气杀菌消毒净化用催化剂及其制备方法 技术领域
本发明属于绿色化学高级氧化技术和环境工程应用领域,涉及在气态条件,规模制备气相自由基·OH、·ClO2、·HO2、·O等活性粒子,并诱发链式反应。
背景技术
空气污染中的微生物性污染物和化学性污染物,通常采用吸附、光催化、负离子、等离子、臭氧等方法进行净化。这些方法中,以高浓度臭氧净化方法最有效，臭氧的标准电极电位2.07伏,化学反应速率常数101～102L/(mol·s)，臭氧在气相中杀灭霉菌(微生物性污染中较难杀灭的一种)时间需要100min，臭氧净化仍有不足之处,而且臭氧对人体有害,在室内空气杀菌消毒净化不能人机共处。然而·OH有更强的氧化能力(标准电极电位2.80伏),它与单质氟(2.87伏)的氧化能力几乎相当，是一种强氧化物质。同时·OH的反应属于游离基反应,具有非常高的化学反应速率107～109L/(mol·s)，比臭氧高7个数量级。其化学反应时间小于1s,生化反应时间1～10s。但由于·OH寿命极短(10ns左右),所以·OH制备及污染治理需在同一时间进行,即一边产生·OH一边进行治理,也就是说必须实现原位再生高浓度气相自由基,或规模制备气相自由基·OH、·ClO2、·HO2、·O等活性粒子。
二氧化硅表面对水有极强的亲和力,水分子可以不可逆地或可逆地吸附在表面上,所以二氧化硅表面通常是由一层OH(羟基)和吸 时水复盖着的。前者是键合到表面Si原子上的羟基,也就是化学吸附水；后者是吸附在表面分子的水,也就是物理吸附的水。在大量实验事实基础上,经过我们长期观察和深入的理论思考,二氧化硅这一特性帮助我们实现了规模制备羟基自由基等气相自由基的梦想。当二氧化硅负载了二氧化氯稳定液,并经85℃以下干燥后,在无光照、无加热情况下,ClO2使二氧化硅表面物理水(小量)有离子化水解H2O→H++OH-,从而有ClO2+H2O→HClO2+HClO3的缓慢水解外,还存在化学吸附水的非离子水解:
Figure PCTCN2016075854-appb-000001
从而有ClO2+·H→HClO2
总反应为ClO2+H2O→HClO2+·OH
此外，还有2·OH→H2O2
和·OH+H2O2→·HO2+H2O
上述非离子化水解(自由基型式)在一般情况下不显著，但在有底物与之反应或有物理或化学催化时会大大加速，从而有大量·OH生成。
Figure PCTCN2016075854-appb-000002
·O+H2O→2·OH
·ClO+H2O+O2→HClO2+·HO2
3·O→O3
O3+·HO2→·OH+2O2
O3+H2O→2·OH+O2
由于活性三氧化二铝表面也有因吸附水而产生的表面羟基，所以也有上述二氧化硅的特性。
高级氧化技术是以产生·OH为标志的,然而目前气态产生·OH的方法,如专利201010567135.8和201310700249.9都需要庞大的附加设备而且成本高,很难大规模工业应用。
发明内容
本发明的目的是解决高级氧化技术应用在气态条件下,污染物治理方面已有技术的不足,提供一种能规模制备气相自由基·OH、·ClO2、·HO2、·O的空气污染治理新方法,提高了去除效率,无二次污染、使用寿命长、简单可靠、可以人机共处并已在实际中取得了应用。
本发明的特征：1.催化剂载体可以是二氧化硅、沸石、海泡石、硅藻土、蒙脱石、三氧化二铝无机多孔材料(粒度≥100目)，优选2-3mm、3-5mm,可以是其中任意一种,也可以是多种的混合物或复合物,浸渍稳定性二氧化氯溶液或稳定性亚氯酸盐溶液,85℃以下干燥,至含水率≤8％而成。
本发明的特征:2.催化剂载体也可以通过规整载体,堇青石蜂窝陶瓷或莫来石蜂窝陶瓷(孔密度50目‐900目),优选400目,规格150×150mm,厚度可以根据需要任意设定,优选25mm、50mm、100mm、150mm。浸渍稳定性二氧化氯溶液或稳定性亚氯酸钠溶液,85℃以下干燥,至含水率≤8％而成。
该材料有两种使用方法:1.经紫外线灯照射,产 生·OH、·ClO2、·HO2、·O等活性粒子,诱发链式反应,迅速杀灭病毒、细菌、霉菌和降解化学污染物,最终成为二氧化碳、水和微量矿盐。2.根据治理环境和治理对象的不同,可不经紫外线灯照射,直接作为催化氧化材料,同样可以降解化学污染物和杀灭病毒、细菌、霉菌等微生物,只是净化效率稍逊于第一种方法,要达到同样净化效果,所用催化剂量比用紫外线灯照射时要增加30％左右。
本发明所采用的浸渍溶液有两种方案
第一方案:配制稳定性二氧化氯溶液,用高纯度二氧化氯发生器得到纯度≥98％的二氧化氯气体,以过氧水合碳酸钠(化学通式为Na2CO3·mH2O2·nH2O)作为稳定剂,配成一定比例的吸收液,最后制备成二氧化氯含量为2％-5％的溶液。
第二方案:配制稳定性亚氯酸钠溶液,该溶液中各组分含量如下:亚氯酸盐0.1-10,稳定剂0.1-5,缓冲剂0.05-15,吸收剂0.1-75。
亚氯酸盐指含亚氯酸根离子ClO2 —的盐,例如:亚氯酸钠、亚氯酸钾、亚氯酸锂。
稳定剂也是强氧化剂,例如:高锰酸钾、H2O2、高氯酸盐、硝酸盐等。
缓冲剂是指能使溶液PH值在一定范围内维持基本恒定的物质,一般是盐类,在这里只能用强碱弱酸的盐,如碳酸钠或硼酸盐、柠檬酸盐等。
吸收剂是指化学吸收剂,与溶质之间有化学反应,溶质的溶解度不仅与气液平衡规律有关,而且与化学平衡规律有关。化学吸收剂 大多是某种活性组分的溶液,例如碳酸钾、碳酸钠、氢氧化钠、氢氧化钾的水溶液等。
上述两种方案中一种作为浸渍液,浸渍上述任何一种无机多孔载体,经85℃以下温度干燥直至含水率≤8％,得到我们所需要的催化材料。
紫外线灯中A、B、C三个波段(波长400-180nm)照射均可以激发该催化材料规模产生气相自由基·OH、·ClO2、·HO2、·O等活性粒子,只要照射强度相同,LED灯或汞紫外灯效果基本相同。中央送风过滤系统,以峰窝陶瓷作为载体的催化剂(风阻小)经有臭氧产生的C波段(185nm)紫外线灯照射,净化效果尤佳。
空气湿度大时(如大于80％),已有的光催化氧化技术或常温多相催化氧化技术对污染物净化效率,都会大幅度下降,而本发明催化剂,却不会因湿度大而受影响,在生活中这种气象条件会经常出现。
附图说明
附图1本发明颗粒催化剂装机试验样机KF-501A。
附图2上述样机除菌率检测数据。
附图3上述样机除甲醛检测数据。
附图4上述样机除甲醛曲线与知名品牌净化器及高浓度臭氧对比。
附图5上述样机除甲醛曲线最小功率除甲醛曲线与瑞士知名品牌I最大功率对比。
具体实施方式
实例,首先制取稳定性亚氯酸钠稳定溶液,量取5000ml纯净水,称取400g含量80％的亚氯酸钠,在水中溶解后,称取氯化钠100g继续在水中搅拌溶化,然后加入20g四合水硼酸钠,最后加20ml含量30％过氧化氢,搅拌后过滤,最后用碳酸钠调整PH值8.0-9.5之间。然后加入3000g粒度为3～5mm的二氧化硅全部浸渍在液体中,不停搅拌,1～2小时后,沥尽余液,风扇吹干并放在65℃真空加热炉干燥,至含水率≤8％即可出炉冷却备用。用此材料制成两个滤网装配在一台双面进风的家用消毒净化器KF-501A中,该净化器没有装UV灯,与H13HEPA网配合对室内空气进行净化。附图1
30立方米试验舱,第三方检测,除菌率数据。附图2
30立方米试验舱第三方检测除甲醛数据。附图3
10立方米试验舱KF-501A除甲醛曲线图与高浓度臭氧机及国外知名品牌净化器除甲醛曲线图。附图4
10立方米试验舱KF-501A最小功率除甲醛曲线与瑞士知名品牌I最大功率除甲醛曲线图。附图5

Claims (8)

  1. 一种空气中杀菌消毒净化用催化剂及使用方法,其特征:该催化剂在室温条件下经紫外线灯照射,规模产生气相自由基·OH、·ClO2、·HO2、·O等活性粒子,吸附并氧化杀灭空气中的病毒、细菌和霉菌等微生物,同时氧化清除空气中的甲醛等化学污染物。
  2. 根据权利要求书1所述催化剂,其特征在于,无机多孔性催化剂载体,浸渍稳定性二氧化氯溶液或稳定性亚氯酸盐溶液,经85℃以下温度干燥而成。
  3. 根据权利要求1所述的催化剂,其特征在于,权利要求2所述的无机多孔性载体,可以是孔密度30目至900目的规整载体,如堇青石、莫来石蜂窝陶瓷,设计成某一种便于生产的尺寸,然后根据需要作不同的串并联组合,满足不同净化过滤风量及风阻的使用要求,优选的规格,如孔密度400目,尺寸150×150mm(长×宽),根据需要切成不同厚度,优选厚度25mm、50mm、100mm、150mm。
  4. 根据权利要求书1所述的催化剂,其特征在于,权利要求2所述的无机多孔性载体,也可以是粒度≥100目的三氧化二铝、二氧化硅、沸石、海泡石、蒙脱石、硅藻土其中一种或多种混合物或复合物,这些无机多孔性物质应有10平方米/克或更大的比表面积,优选100立方米/克以上的比表面积,粒度优选2-3mm、3-5mm。
  5. 根据权利要求书2所述的稳定性二氧化氯溶液,其特征在于,用高纯度二氧化氯发生器得到纯度≥98％的二氧化氯气体,以过氧水合碳酸钠(化学通式为Na2CO3·mH2O2·nH2O)作为稳定剂,配成一定比例的吸收液,最后制备成二氧化氯含量为2％-5％的溶液。
  6. 根据权利要求书2所述的稳定性亚氯酸盐溶液,其特征在于,该溶液中各组分含量如下:亚氯酸盐0.1-10,稳定剂0.1-5,缓冲剂0.05-15,吸收剂0.1-75,亚氯酸盐可以是亚氯酸的碱金属盐或亚氯酸的碱土金属盐,如亚氯酸钠、亚氯酸钾、亚氯酸锂。
  7. 根据权利要求书1所述的消毒净化方法,其特征在于,该催化剂可以按照不同的使用要求预先加工成任何形状,放置于微环境空气过滤系统或移动式空气消毒净化设备上,只要经过≥30微瓦/平方厘米照射强度的紫外线,就能高效去除微生物性污染物和化学性污染物。
  8. 根据权利要求书1所述的消毒净化方法,其特征在于,权利书7所述的紫外线可以由汞紫外线灯或LED紫外线灯提供,紫外线中的A、B、C三波段均可以激发催化剂规模产生气相自由基活性粒子。
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