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CN106186249B - A kind of micro-nano iron sulfide/porous carbon composite material and its preparation and application of seaweed biomass - Google Patents

A kind of micro-nano iron sulfide/porous carbon composite material and its preparation and application of seaweed biomass Download PDF

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CN106186249B
CN106186249B CN201610498854.6A CN201610498854A CN106186249B CN 106186249 B CN106186249 B CN 106186249B CN 201610498854 A CN201610498854 A CN 201610498854A CN 106186249 B CN106186249 B CN 106186249B
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seaweed
iron sulfide
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porous carbon
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CN106186249A (en
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吕剑
武君
骆永明
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Yantai Institute of Coastal Zone Research of CAS
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/58Treatment of water, waste water, or sewage by removing specified dissolved compounds
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    • C01G49/00Compounds of iron
    • C01G49/12Sulfides
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    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
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    • C09K17/02Soil-conditioning materials or soil-stabilising materials containing inorganic compounds only
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    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer

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Abstract

The present invention relates to a kind of method of environmental technology field, specifically a kind of micro-nano iron sulfide/porous carbon composite and its preparation and seaweed biomass application.Promote biological sulphate reduction to generate iron sulfide using seaweed biomass and be covered on seaweed biomass surface, then pass through mild hydro-thermal reaction, seaweed biomass carbonization is made to generate the porous carbon material that load has micro-nano biological iron sulfide.The multiple technologies problem that the present invention effectively overcomes seaweed biomass higher value application to be faced, initial investment capital cost is cheap, can salvage the time according to the harvest place and concentration harvest of seaweed, quickly emergency sets up reactor, prepares micro-nano iron sulfide/porous carbon composite.Prepared micro-nano iron sulfide/seaweed base biology carbon composite can be applied in water pollution control, soil (deposit) improvement or pollution law.

Description

一种微纳米硫化铁/多孔碳复合材料及其制备和海藻生物质 应用A kind of micro-nano iron sulfide/porous carbon composite material and its preparation and seaweed biomass application

技术领域technical field

本发明涉及的是一种环保技术领域的方法,具体地说是一种微纳米硫化铁/多孔碳复合材料及其制备和海藻生物质应用。The invention relates to a method in the technical field of environmental protection, in particular to a micro-nano iron sulfide/porous carbon composite material and its preparation and seaweed biomass application.

背景技术Background technique

我国海藻生物质资源十分丰富,海藻产量居世界第一位,但国内对海藻的利用却很少。以海带为例,海带的年产量约占世界产量95%。海藻生物质相较于陆地生物质有优势。海藻生长在海里,不占用土地资源,生长速度快,生长过程捕获大量二氧化碳,并吸收去除大量氮磷。绿潮是海洋大型藻爆发性生长聚集形成的藻华现象。绿潮藻漂移至近岸水域或堆积在沙滩上,如果处理不及时就会很快腐烂,关于绿潮藻生物质的资源化也是一个困扰海岸带地区的难题。因此,如能将我国近海海藻生物质加以充分利用,具有重要的现实意义。my country is very rich in seaweed biomass resources, and seaweed production ranks first in the world, but domestic utilization of seaweed is very small. Take kelp as an example, the annual output of kelp accounts for about 95% of the world's output. Algal biomass has advantages over terrestrial biomass. Seaweed grows in the sea, does not occupy land resources, grows fast, captures a large amount of carbon dioxide during the growth process, and absorbs and removes a large amount of nitrogen and phosphorus. Green tide is an algal bloom phenomenon formed by the explosive growth and aggregation of marine macroalgae. Green tide algae drift to the nearshore waters or accumulate on the beach. If they are not treated in time, they will quickly rot. The resource utilization of green tide algae is also a problem that plagues coastal areas. Therefore, it is of great practical significance to make full use of my country's offshore algal biomass.

目前海藻生物质的主要利用方式包括开发生物质能源、提炼海藻胶、生产饲料、制备海藻肥等。海藻生物质的开发利用多限于初级生产加工阶段,海藻生物质的利用率不高。以干物质计,目前海带工业利用率仅达30%左右。在提取完海藻胶等物质后的残渣被作为废弃物直接排放到自然界中,不但造成生物质资源的浪费,也造成的一系列的环境污染问题。如能将这类海藻废弃物加以利用,具有重要的现实意义。当前我国的海洋藻类可利用的范围广、资源多,但缺乏系统性研究和高端技术。因此,需要开发新型高附加值的海藻生物质利用技术。本专利在大量的实验基础上发明了一种应用海藻生物质制备微纳米硫化铁/多孔碳复合材料的方法。At present, the main utilization methods of seaweed biomass include the development of biomass energy, the extraction of seaweed gum, the production of feed, and the preparation of seaweed fertilizer. The development and utilization of seaweed biomass is mostly limited to the primary production and processing stage, and the utilization rate of seaweed biomass is not high. In terms of dry matter, the current industrial utilization rate of kelp is only about 30%. The residue after the extraction of alginate and other substances is directly discharged into the nature as waste, which not only causes waste of biomass resources, but also causes a series of environmental pollution problems. If this kind of seaweed waste can be utilized, it has important practical significance. At present, my country's marine algae have a wide range of available resources and many resources, but lack of systematic research and high-end technology. Therefore, it is necessary to develop new high value-added seaweed biomass utilization technologies. This patent invents a method for preparing micro-nano iron sulfide/porous carbon composite material by using seaweed biomass on the basis of a large number of experiments.

经过对现有技术文献的检索发现,罗丽卉等发表在《中国环境科学》,2012,32(2):249-253的文章中,通过有机酸促进硫酸还原菌还原硫酸根合成了纳米硫化铁材料。曾淦宁等在《环境科学学报》,2014,34(2):392-397上发表的“铜藻基生物炭的水热制备及性能表征”一文中,提到通过水热反应利用铜藻生物质制备了多孔碳。到目前为止,尚未有应用海藻生物质促进硫酸菌生长合成生物微纳米硫铁材料,然后再通过水热反应碳化过程制备海藻多孔碳基微纳米硫化铁复合材料的报道。After searching the prior art literature, it was found that Luo Lihui et al. published an article in "China Environmental Science", 2012, 32(2): 249-253, and synthesized nano-iron sulfide materials by promoting sulfuric acid-reducing bacteria to reduce sulfate radicals by organic acids. . Zeng Ganning et al. in the "Journal of Environmental Science", 2014, 34(2): 392-397, in the article "Hydrothermal Preparation and Performance Characterization of Copper Algae-Based Biochar", mentioned the utilization of copper algae biomass by hydrothermal reaction. Porous carbon was prepared. So far, there is no report on the application of seaweed biomass to promote the growth of sulfuric acid bacteria to synthesize biological micro-nano ferric sulfide materials, and then prepare seaweed porous carbon-based micro-nano ferric sulfide composites through a hydrothermal reaction carbonization process.

发明内容SUMMARY OF THE INVENTION

本发明的目的在于针对现有技术的不足,提供一种微纳米硫化铁/多孔碳复合材料及其制备和海藻生物质应用。The purpose of the present invention is to provide a micro-nano iron sulfide/porous carbon composite material and its preparation and seaweed biomass application in view of the deficiencies of the prior art.

为实现上述目的,本发明采用技术方案为:To achieve the above object, the present invention adopts the technical scheme as follows:

一种微纳米硫化铁/多孔碳复合材料,利用海藻生物质促进硫酸盐生物还原生成硫化铁并覆盖在海藻生物质表面,然后经过温和水热反应,使海藻生物质碳化生成负载有微纳米生物硫化铁的多孔炭材料。A micro-nano iron sulfide/porous carbon composite material uses seaweed biomass to promote sulfate biological reduction to generate iron sulfide and covers the surface of seaweed biomass. Porous carbon material of iron sulfide.

所述海藻生物质为近岸海域直接打捞海藻、收集上岸堆积晾晒的海藻或海藻加工废弃物。The seaweed biomass is directly salvaged seaweed in the near-shore sea area, and collected seaweed or seaweed processing waste that is accumulated and dried on the shore.

一种微纳米硫化铁/多孔碳复合材料的制备方法,利用海藻生物质促进硫酸盐生物还原生成硫化铁并覆盖在海藻生物质表面,然后经过温和水热反应,使海藻生物质碳化生成负载有微纳米生物硫化铁的多孔炭材料。A preparation method of micro-nano iron sulfide/porous carbon composite material, which utilizes seaweed biomass to promote sulfate biological reduction to generate iron sulfide and covers the surface of seaweed biomass, and then undergoes mild hydrothermal reaction to carbonize seaweed biomass to form loaded iron sulfide. Porous carbon materials of micro-nano bio-iron sulfide.

具体为:Specifically:

1)将海藻经粉碎获得海藻浆,待用;1) The seaweed is pulverized to obtain seaweed pulp, which is set aside for use;

2)将含有硫酸还原菌的物料和硫酸亚铁各按照1-5%(质量比)的比例加入到上述海藻浆中匀浆混合,于15-35℃下将匀浆中硫酸盐生物还原反应72-240h,使海藻生物质颗粒表面布满硫化铁,生成硫化铁/海藻生物质混合物;2) material containing sulfate-reducing bacteria and ferrous sulfate are respectively added in the above-mentioned seaweed slurry according to the ratio of 1-5% (mass ratio) and mixed, and the sulfate biological reduction reaction is carried out in the homogenate at 15-35 ° C. 72-240h, make the surface of seaweed biomass particles covered with iron sulfide to generate iron sulfide/seaweed biomass mixture;

3)将步骤2)中获得微纳米硫化铁/海藻生物质混合物投入水热反应釜,170-220℃水热反应2-24h,收集残存于反应釜底部的黑色固体,即为微纳米硫化铁/海藻基生物炭复合材料,经扫描电镜检验负载在多孔炭上的硫化铁颗粒为微纳米级颗粒。3) Put the micro-nano iron sulfide/algal biomass mixture obtained in step 2) into the hydrothermal reaction kettle, conduct hydrothermal reaction at 170-220 ° C for 2-24 hours, and collect the black solid remaining at the bottom of the reaction kettle, which is the micro-nano iron sulfide /Seaweed-based biochar composite material, the iron sulfide particles loaded on porous carbon are micro-nano-sized particles by scanning electron microscopy.

所述海藻为直接打捞、直接打捞收集上岸堆积或直接打捞收集晾晒的海藻经洗涤后粉碎,待用。Said seaweed is directly salvaged, directly salvaged, collected and stacked on the shore, or directly salvaged and collected to dry the seaweed, washed and then pulverized and set aside for use.

所述物料为发酵用含有硫酸还原菌的基质;基质为污泥、牛粪、沼渣或其它富含硫酸盐还原菌的基质(所含硫酸盐还原菌数量>1×107MPN/g)。The material is a substrate containing sulfate-reducing bacteria for fermentation; the substrate is sludge, cow dung, biogas residue or other substrates rich in sulfate-reducing bacteria (the number of sulfate-reducing bacteria contained is >1×10 7 MPN/g) .

所述水热反应后收集残存于反应釜底部的黑色固体,进行后续干燥处置,即为微纳米硫化铁/海藻基生物炭复合材料。After the hydrothermal reaction, the black solid remaining at the bottom of the reactor is collected and subjected to subsequent drying treatment, which is the micro-nano iron sulfide/algae-based biochar composite material.

一种微纳米硫化铁/多孔碳复合材料的应用,所述上述制备获得微纳米硫化铁/海藻基生物炭复合材料可在水污染控制、土壤沉积物改良或污染环境修复中的应用。An application of a micro-nano iron sulfide/porous carbon composite material, the micro-nano iron sulfide/algae-based biochar composite material obtained by the above preparation can be used in water pollution control, soil sediment improvement or polluted environment remediation.

一种海藻生物质的应用,海藻生物质在制备微纳米硫化铁/多孔碳复合材料中的应用。An application of seaweed biomass, the application of seaweed biomass in the preparation of micro-nano iron sulfide/porous carbon composite material.

海藻泛指海水中生长繁殖的各种藻类如浒苔、石莼、海带、鼠尾藻、江蓠、龙须菜及赤潮藻等。Seaweed generally refers to various algae that grow and reproduce in seawater, such as prolifera, Ulva, kelp, sage, gracilaria, asparagus and red tide algae.

本发明所具有的优点:The advantages of the present invention:

1)有效克服海藻生物质高值化利用所面临的多种技术难题,先期投资基建费用低廉、能够根据海藻的收获地点和集中收获打捞时间,快速应急架设反应器,制备微纳米硫化铁/多孔碳复合材料;1) Effectively overcome the various technical difficulties faced by the high-value utilization of seaweed biomass, the initial investment and infrastructure costs are low, and the reactor can be quickly set up according to the harvesting location of the seaweed and the time of centralized harvesting and salvage to prepare micro-nano iron sulfide/porous carbon composite;

2)所得微纳米硫化铁/海藻基多孔炭复合材料性质稳定,属于多用途的环境友好性材料。2) The obtained micro-nano iron sulfide/algae-based porous carbon composite material has stable properties and is a multi-purpose environment-friendly material.

3)本制备技术发挥了水热反应可以处理生物质鲜样的优点,可直接应用海藻鲜样或高含水率的生物质作为反应物料,去除了以往海藻生物质反应处理前需要预先烘干脱水的步骤,同时水热反应体系温度低于220℃,属于低温水热反应,从而减少了能耗,同时保证了应用水热反应制备微纳米硫化铁/海藻基多孔炭的可操作性和安全性。3) This preparation technology takes advantage of the hydrothermal reaction to process fresh biomass samples, and can directly use fresh seaweed samples or biomass with high moisture content as reaction materials, eliminating the need for pre-drying and dehydration before seaweed biomass reaction treatment. At the same time, the temperature of the hydrothermal reaction system is lower than 220 °C, which is a low-temperature hydrothermal reaction, thereby reducing energy consumption and ensuring the operability and safety of the preparation of micro-nano iron sulfide/algae-based porous carbon by hydrothermal reaction. .

附图说明Description of drawings

图1为本发明实施例获得材料的扫描电镜图(图中白色颗粒为硫化铁)。Fig. 1 is a scanning electron microscope image of a material obtained in an embodiment of the present invention (the white particles in the figure are iron sulfide).

具体实施方式Detailed ways

下面通过实施例对本发明进一步说明,然而本发明并不局限于以下实施例。The present invention is further illustrated by the following examples, but the present invention is not limited to the following examples.

实施例1Example 1

绿潮爆发期间,于青岛近海打捞绿潮藻浒苔或收集堆积上岸的浒苔,粉碎至生物质粒径<1mm制成海藻浆,将污泥(硫酸还原菌数量>1×107MPN/g)和硫酸亚铁各按照1%(质量比)的比例加入到上述海藻浆中,匀浆混合,35℃温度下启动匀浆中硫酸盐生物还原反应,反应72h后,将生成硫化铁/海藻生物质混合物直接放入水热反应釜,170℃快速水热反应24h,水热反应结束,收集残存于反应釜底部的黑色固体,真空干燥,通过扫描电镜分析,断定负载在多孔炭上的硫化铁颗粒为微纳米级颗粒,从而制得微纳米硫化铁/海藻基生物炭复合材料。所制备多孔炭复合材料的粒径主要分布在40-80μm之间。将所制备复合材料按照0.5%(质量比)的比例加入废水中,重金属的去除率超过99%。During the outbreak of the green tide, the green tide algae prolifera were salvaged from the offshore of Qingdao or the prolifera that accumulated on the shore were collected, crushed until the biomass particle size was less than 1 mm to make seaweed slurry, and the sludge (the number of sulfuric acid-reducing bacteria> 1×10 7 MPN/ g) and ferrous sulfate were added to the above seaweed slurry according to the proportion of 1% (mass ratio), the homogenate was mixed, and the sulfate biological reduction reaction in the homogenate was started at a temperature of 35 ° C. After the reaction for 72 hours, iron sulfide/ The seaweed biomass mixture was directly put into the hydrothermal reactor, and the rapid hydrothermal reaction was carried out at 170°C for 24 hours. The hydrothermal reaction was over. The black solid remaining at the bottom of the reactor was collected, dried in vacuum, and analyzed by scanning electron microscope. The iron sulfide particles are micro-nano-scale particles, thereby preparing the micro-nano iron sulfide/algae-based biochar composite material. The particle size of the prepared porous carbon composites is mainly distributed between 40-80 μm. The prepared composite material is added to the wastewater in a proportion of 0.5% (mass ratio), and the removal rate of heavy metals exceeds 99%.

实施例2Example 2

采集晾晒的江蓠与龙须菜,将海藻冲洗去除盐分,然后粉碎生物质至粒径<1mm匀浆,将牛粪(硫酸还原菌数量>1×107MPN/g)和硫酸亚铁各按照2%(质量比)的比例加入到海藻浆中,匀浆混合,25℃温度下启动硫酸盐生物还原反应,反应120h后生成微纳米硫化铁/海藻生物质混合物。生成硫化铁/海藻生物质混合物直接放入水热反应釜,190℃快速水热反应10h,收集残存于反应釜底部的黑色固体,冷冻干燥,通过扫描电镜观察到负载在多孔炭上的硫化铁颗粒为微纳米级颗粒,制得微纳米硫化铁/海藻基生物炭复合材料。所制备多孔炭复合材料的粒径在平均粒径在70μm。将所制备复合材料按照2%(质量比)的比例加入到土壤中,土壤中四溴双酚A的去除率超过90%。The dried Gracilaria and Astragalus were collected, the seaweed was washed to remove the salt, and then the biomass was pulverized to a particle size of < 1 mm and homogenized. According to the proportion of 2% (mass ratio), it was added into the seaweed slurry, homogenized and mixed, and the sulfate bioreduction reaction was started at 25°C. The iron sulfide/algal biomass mixture was directly put into the hydrothermal reaction kettle, and the rapid hydrothermal reaction was carried out at 190 °C for 10 h. The black solid remaining at the bottom of the reaction kettle was collected and freeze-dried. The iron sulfide supported on the porous carbon was observed by scanning electron microscope. The particles are micro-nano-scale particles, and the micro-nano iron sulfide/algae-based biochar composite material is prepared. The average particle size of the prepared porous carbon composites was 70 μm. The prepared composite material was added to the soil in a proportion of 2% (mass ratio), and the removal rate of tetrabromobisphenol A in the soil exceeded 90%.

实施例3Example 3

于某海带加工厂采集海带加工废弃物,冲洗海带加工废弃物,去除盐分,然后将海带加工废弃物粉碎至粒径<1mm匀浆,将沼渣(硫酸还原菌数量>1×107MPN/g)和硫酸亚铁各按照5%(质量比)的比例加入到海藻浆中,匀浆混合,15℃温度下启动硫酸盐生物还原反应,反应240h后生成硫化铁/海藻生物质混合物。将该混合物直接放入水热反应釜,220℃快速水热反应2h,水热反应结束,收集残存于反应釜底部的黑色固体,真空干燥,通过扫描电镜观察到负载在多孔炭上的硫化铁颗粒为微纳米级颗粒,即制得微纳米硫化铁/海藻基生物炭复合材料。所制备多孔炭复合材料的粒径在平均粒径在50μm。将所制备复合材料按照1%(质量比)的比例加入到地下水中,地下水中三氯乙烯的去除率超过90%。Collect kelp processing waste in a kelp processing factory, wash the kelp processing waste, remove the salt, and then pulverize the kelp processing waste to a particle size of <1mm to homogenize, and the biogas residue (the number of sulfuric acid reducing bacteria> 1×10 7 MPN/ g) and ferrous sulfate were added to the seaweed slurry according to the proportion of 5% (mass ratio), homogenized and mixed, and the sulfate biological reduction reaction was started at a temperature of 15 ° C, and the iron sulfide/seaweed biomass mixture was generated after the reaction for 240h. The mixture was directly put into the hydrothermal reaction kettle, and the rapid hydrothermal reaction was carried out at 220°C for 2 hours. The hydrothermal reaction was completed. The black solid remaining at the bottom of the reaction kettle was collected and dried in vacuum. The iron sulfide supported on the porous carbon was observed by scanning electron microscope. The particles are micro-nano-scale particles, that is, the micro-nano iron sulfide/algae-based biochar composite material is prepared. The average particle size of the prepared porous carbon composites was 50 μm. The prepared composite material was added to groundwater in a proportion of 1% (mass ratio), and the removal rate of trichloroethylene in groundwater exceeded 90%.

Claims (7)

1. a kind of micro-nano iron sulfide/porous carbon composite, it is characterised in that:
1) seaweed is crushed and obtains seaweed slurry, for use;
2) by the material containing sulfatereducting bacteria and ferrous sulfate respectively according to 1-5%(mass ratio) ratio be added to above-mentioned seaweed It is homogenized mixing in slurry, biological sulphate reduction in homogenate is reacted into 72-240 h at 15-35 DEG C, makes seaweed biomass particle Surface is covered with iron sulfide, generates iron sulfide/seaweed biomass mixture;
3) iron sulfide/seaweed biomass mixture will be obtained in step 2 put into hydrothermal reaction kettle, 170-220 DEG C of hydro-thermal reaction 2-24 h collects the black solid for remaining in reactor bottom, as micro-nano iron sulfide/porous carbon composite, through scanning Iron-sulphide particles of the Electronic Speculum proof load in porous charcoal are micro/nano level particle.
2. micro-nano iron sulfide/porous carbon composite according to claim 1, it is characterised in that: the seaweed biomass Seaweed, the seaweed for collecting disembarkation accumulation sunning or seaweed processing waste are directly salvaged for immediate offshore area.
3. a kind of preparation method of micro-nano iron sulfide/porous carbon composite described in claim 1, it is characterised in that: 1) Seaweed is crushed and obtains seaweed slurry, for use;
2) by the material containing sulfatereducting bacteria and ferrous sulfate respectively according to 1-5%(mass ratio) ratio be added to above-mentioned seaweed It is homogenized mixing in slurry, biological sulphate reduction in homogenate is reacted into 72-240 h at 15-35 DEG C, makes seaweed biomass particle Surface is covered with iron sulfide, generates iron sulfide/seaweed biomass mixture;
3) iron sulfide/seaweed biomass mixture will be obtained in step 2 put into hydrothermal reaction kettle, 170-220 DEG C of hydro-thermal reaction 2-24 h collects the black solid for remaining in reactor bottom, as micro-nano iron sulfide/porous carbon composite, through scanning Iron-sulphide particles of the Electronic Speculum proof load in porous charcoal are micro/nano level particle.
4. the preparation method of micro-nano iron sulfide/porous carbon composite as claimed in claim 3, it is characterised in that: the sea Algae is directly to salvage, directly salvage and collect disembarkation accumulation or directly salvage the washed rear crushing of seaweed for collecting sunning, for use.
5. the preparation method of micro-nano iron sulfide/porous carbon composite as claimed in claim 3, it is characterised in that: the object Material is matrix of the fermentation containing sulfatereducting bacteria;Matrix is sludge, cow dung, biogas residue or other bases rich in sulfate reducing bacteria Matter.
6. the preparation method of micro-nano iron sulfide/porous carbon composite as claimed in claim 3, it is characterised in that: the water The black solid for remaining in reactor bottom is collected after thermal response, carries out subsequent dry disposition, as micro-nano iron sulfide/porous Carbon composite.
7. a kind of application of micro-nano iron sulfide/porous carbon composite described in claim 1, it is characterised in that: described micro- Nanometer iron sulfide/porous carbon composite is applied in water pollution control, soil improvement or pollution law.
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