WO2019095306A1 - 一种热塑性树脂固定生物质炭的生物载体制备方法 - Google Patents

一种热塑性树脂固定生物质炭的生物载体制备方法 Download PDF

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Publication number
WO2019095306A1
WO2019095306A1 PCT/CN2017/111713 CN2017111713W WO2019095306A1 WO 2019095306 A1 WO2019095306 A1 WO 2019095306A1 CN 2017111713 W CN2017111713 W CN 2017111713W WO 2019095306 A1 WO2019095306 A1 WO 2019095306A1
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Prior art keywords
thermoplastic resin
functional material
charcoal
preparing
temperature
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PCT/CN2017/111713
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English (en)
French (fr)
Inventor
全燮
毛彦俊
陈硕
于洪涛
张耀斌
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Dalian University of Technology
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Dalian University of Technology
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Priority to US16/761,315 priority Critical patent/US11511472B2/en
Priority to EP17932137.7A priority patent/EP3695955B1/en
Priority to PCT/CN2017/111713 priority patent/WO2019095306A1/zh
Publication of WO2019095306A1 publication Critical patent/WO2019095306A1/zh
Anticipated expiration legal-status Critical
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/80—Component parts, details or accessories; Auxiliary operations
    • B29B7/88—Adding charges, i.e. additives
    • B29B7/90—Fillers or reinforcements, e.g. fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/07—Flat, e.g. panels
    • B29C48/08—Flat, e.g. panels flexible, e.g. films
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B13/00—Conditioning or physical treatment of the material to be shaped
    • B29B13/02—Conditioning or physical treatment of the material to be shaped by heating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B13/00—Conditioning or physical treatment of the material to be shaped
    • B29B13/04—Conditioning or physical treatment of the material to be shaped by cooling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/002—Methods
    • B29B7/007—Methods for continuous mixing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/74—Mixing; Kneading using other mixers or combinations of mixers, e.g. of dissimilar mixers ; Plant
    • B29B7/7466—Combinations of similar mixers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/80—Component parts, details or accessories; Auxiliary operations
    • B29B7/82—Heating or cooling
    • B29B7/826—Apparatus therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00—Making granules
    • B29B9/02—Making granules by dividing preformed material
    • B29B9/04—Making granules by dividing preformed material in the form of plates or sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00—Making granules
    • B29B9/12—Making granules characterised by structure or composition
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/001—Combinations of extrusion moulding with other shaping operations
    • B29C48/0022—Combinations of extrusion moulding with other shaping operations combined with cutting
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/022—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the choice of material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/92—Measuring, controlling or regulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C69/00—Combinations of shaping techniques not provided for in a single one of main groups B29C39/00 - B29C67/00, e.g. associations of moulding and joining techniques; Apparatus therefore
    • B29C69/001—Combinations of shaping techniques not provided for in a single one of main groups B29C39/00 - B29C67/00, e.g. associations of moulding and joining techniques; Apparatus therefore a shaping technique combined with cutting, e.g. in parts or slices combined with rearranging and joining the cut parts
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F3/00—Biological treatment of water, waste water, or sewage
    • C02F3/02—Aerobic processes
    • C02F3/10—Packings; Fillings; Grids
    • C02F3/105—Characterized by the chemical composition
    • C02F3/106—Carbonaceous materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
    • B29B7/34—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices
    • B29B7/38—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00—Making granules
    • B29B9/02—Making granules by dividing preformed material
    • B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92009—Measured parameter
    • B29C2948/92209—Temperature
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/92704—Temperature
    • 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
    • C02F2101/30—Organic compounds
    • C02F2101/34—Organic compounds containing oxygen
    • C02F2101/345—Phenols
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/005—Black water originating from toilets
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F3/00—Biological treatment of water, waste water, or sewage
    • C02F3/02—Aerobic processes
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F3/00—Biological treatment of water, waste water, or sewage
    • C02F3/28—Anaerobic digestion processes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/10—Biological treatment of water, waste water, or sewage

Definitions

  • the present invention relates to a method for preparing a biological carrier for immobilizing biomass carbon by a thermoplastic resin, which is applied to biological treatment of environmental pollutants, and is particularly suitable for biological treatment of sewage, and belongs to the field of biological treatment and functional materials of pollutants. .
  • refractory organic components such as phenols, southern compounds, monocyclic aromatic compounds, polycyclic aromatic hydrocarbons, polychlorinated biphenyls, insecticides, herbicides and dyes.
  • Their environmental hazards have been The universal attention of all countries in the world. Controlling refractory organic pollutants is an important issue in the field of water pollution prevention and control.
  • Recent studies have shown that the addition of artificial redox mediators can accelerate the extracellular electron transport rate of microorganisms, which in turn helps to enhance the biodegradability of refractory organic pollutants and shorten the degradation time. Therefore, redox mediators have potential application value and are receiving more and more attention at home and abroad.
  • the so-called redox mediator transfers electrons through its own redox ability, mainly involved in the extracellular electron transport process of microorganisms, in order to accelerate the electron transfer rate, and the degradation rate of pollutants is significantly improved.
  • these substances are all soluble, and in the biological water treatment process, regular dosing is required, which causes problems such as treatment cost and secondary pollution to the environment.
  • Carbonaceous materials such as graphite, carbon nanotubes, and biochar are widely used as redox mediators with high recyclability in recent years.
  • biochar Biochar
  • Black carbon under low or no oxygen conditions.
  • biochar a class of insoluble, stable, highly aromatic, carbon-rich solid residues produced by biomass at high temperatures (usually ⁇ 700 ° (:) pyrolysis (carbonization).
  • the cost of preparing biochar is low, Wide range of sources, mainly wood, nutshell, straw, sludge, animal waste, etc.
  • oxygen-containing functional groups such as carbonyl, hydroxyl, etc.
  • Carbon can receive electrons generated by biodegradation. After receiving electrons, the reduced biochar can transfer electrons to electron acceptors.
  • biochar acts as a redox mediator to improve the processing efficiency.
  • the object of the present invention is to fix a biochar material to a thermoplastic resin and develop it.
  • the present invention is directed to a biological water treatment technology, the problem of slow processing rate of refractory organic matter in a water body due to limitation of electron transport rate, and the present invention is to provide a bio-carrier preparation of a thermoplastic resin-fixed biomass carbon. method.
  • a method for preparing a biological carrier for immobilizing biomass carbon with a thermoplastic resin the steps are as follows:
  • step ( 2 ) mechanically blending the pretreated biochar functional material powder with the thermoplastic resin particles in step ( 1 ) and stirring uniformly, and standby; the mass ratio of the biomass carbon functional material powder to the thermoplastic resin particles is 20 %
  • step ( 3 ) using a screw extruder to melt blend and extrude the solid mixture in step ( 2 ), strip, and mechanically cut to obtain a granular blend;
  • the processing temperature of the screw extruder is 130 °0190° (:, to ensure that the thermoplastic resin is thoroughly mixed with the biomass carbon functional material powder in a molten state;
  • thermoplastic resin particles are mechanically stirred uniformly, added to a screw extruder for blending and extrusion, and according to the design of the die head, different carriers are obtained.
  • the ratio of the mass of the biomass carbon in the granular mixture of the pipe to the total mass of the thermoplastic resin particles is not more than 20%; ⁇ 0 2019/095306 ⁇ (:1' 2017/111713
  • the biomass carbon functional material is one or a combination of two or more of grass charcoal, rice straw charcoal, rice husk charcoal, nutshell charcoal, sludge biochar, and animal fecal biomass charcoal.
  • thermoplastic resin particles are extrusion grade polyethylene particles or extrusion grade polypropylene particles.
  • the screw extruder is heated in four stages, and the temperature range and effect of each section of heating are as follows: ( 1 ) Temperature 1 20-140° (:, can satisfy the semi-molten state of the thermoplastic resin, which is favorable for solid transportation Continuity; (2) Temperature 130-160° (:, to accelerate the conversion of the thermoplastic resin from a semi-molten state to a molten state, which facilitates uniform mixing of the blend in the heating section; ( 3 ) Temperature 140- 170° (:, the blend is in a solid-liquid mixed state to sufficiently mix the molten thermoplastic resin with the solid biomass carbon functional material, which is advantageous for the uniform distribution of the biomass carbon functional material and the thermoplastic resin in a molten state; ( 4 ) The temperature is 115-145 to allow the quantitative and constant pressure of the blend to flow out, to ensure the stability and continuity of the extrusion and the subsequent smooth setting.
  • the method for preparing a biological carrier for fixing a biomass carbon by a thermoplastic resin provided by the invention has the advantages of simple process, flexible and controllable method, strong adaptability and large-scale production, and the biological carrier has high-efficiency removal of refractory organic pollutants. effectiveness.
  • thermoplastic resin-fixed biomass carbon biocarrier ( 1 ) grinding the rice straw charcoal functional material into a powder, 60 ° (: drying to constant weight, standby; ( 2 ) step ( 1 ) The pretreated straw charcoal functional material powder is mechanically blended with the high density polyethylene pellets and stirred uniformly, and used; ( 3 ) melt-blending and extruding the solid mixture in the step ( 2 ) by using a screw extruder. Strip, and mechanically cut to obtain a granular blend.
  • the processing temperature of the screw extruder is 175 ° (: The mass percentage of straw charcoal functional material and high density polyethylene pellet is 30%; ( 4 ) Step ( 3) Granular blend prepared with thermoplastic resin ⁇ 0 2019/095306 ⁇ (:1' 2017/111713
  • the melt-mixed extruded material is slivered, cooled, drawn, pelletized, and different according to the design of the die head. Shape carrier.
  • the bio-carrier is applied to the aerobic biodegradation experiment of phenol wastewater (dissolved oxygen is controlled at 2.0-3.0)
  • thermoplastic resin-fixed biomass carbon biocarrier ( 1 ) grinding the rice-shell charcoal functional material into a powder, 60 ° (: drying to constant weight, standby; ( 2 ) step ( 1 ) The pretreated pretreated rice husk charcoal functional material powder is mechanically blended with the high density polyethylene granules and stirred uniformly, and used; ( 3 ) melt-blending and extruding the solid mixture in step ( 2 ) by using a screw extruder, The strips are mechanically cut to obtain a granular blend.
  • the processing temperature of the screw extruder is 185° (: The mass percentage of the rice husk carbon functional material and the high density polyethylene granules is 50%; ( 4 ) ( 3 ) The granular blend prepared in the middle and the high-density polyethylene pellets are mechanically stirred uniformly, and then added to a screw extruder for blending and extruding. The mass of the rice shell charcoal and the total mass of the high-density polyethylene in the granular blend The percentage is 8%; ( 5 ) The melt-mixed extruded material is slivered, cooled, drawn, pelletized, and the carrier of different shapes is obtained according to the design of the die head.
  • carbonyl graphene oxide as a modification of the biological function of the carrier material prepared as follows: Preparation of (1) the carbonylation graphene oxide modified functional material: graphene oxide dispersion thereof was adjusted to 10 with aqueous ammonia 11 , 9 0° (: water heat 6 hours; cooling; 60 ° (: drying, the obtained solid is recorded as 00; add 0 00 to 2 ⁇ 11 ⁇ water, ultrasonically make it fully dispersed, in the ice water bath, add 51111112304 , and 1.2 ⁇ potassium dichromate, fully stirred, reacted for 3 hours, 60 ° (: drying. The resulting carbonylation modified graphene oxide ( ⁇ 00 ).
  • the bio-supporting biochar, the bio-carrier of the carbonylation-modified graphene oxide as a functional material, and the unmodified carrier are respectively applied to the aerobic and anaerobic biodegradation experiments of the phenol wastewater, respectively.
  • the carrier dosage was 30% of the effective volume of the reactor.
  • Table 1 It can be seen from the table that under the conditions of aerobic, anaerobic and phenol concentration in different influent, the biodegradation performance of the reactor carrying the modified carrier is better than that of the unmodified carrier.
  • the biodegradation performance of the reactor of the biochar modified carrier is slightly better than that of the reactor carrying the carbonylated graphene oxide modified support.
  • the preparation method of the biocarrier of the carbonylation-modified graphene oxide as a functional material the preparation method of the bio-carrier of the thermoplastic resin-immobilized biochar is simpler, convenient to operate, time-saving, and more favorable for ensuring production. Process continuity. Compared with carbonylation-modified graphene oxide as a functional material, biochar functional materials are more widely used, and cheaper is more conducive to large-scale production and application.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Biodiversity & Conservation Biology (AREA)
  • Microbiology (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
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  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Biological Treatment Of Waste Water (AREA)

Abstract

一种热塑性树脂固定生物质炭的生物载体制备方法，以热塑性树脂挤出级聚乙烯颗粒或挤出级聚丙烯颗粒为基础原料，以草木炭、秸秆炭、稻壳炭、果壳炭、污泥生物质炭以及动物粪便生物质炭中的一种或组合为功能料，通过螺杆挤出工艺制备了热塑性树脂固定生物质炭载体。该制备方法工艺简单，方法灵活可控，适应性强，可规模化生产。

Description

\¥0 2019/095306 卩（：17€謂17/111713
1
说明书
发明名称:一种热塑性树脂固定生物质炭的生物载体制备方法 技术领域
[0001] 本发明涉及一种热塑性树脂固定生物质炭的生物载体制备方法， 应用于环境污 染物的生物处理， 尤其适用于污水的生物处理中， 属于污染物的生物处理及功 能性材料技术领域。
背景技术
[0002] 生活污水和工业废水是我国水体的主要污染源。 相比于生活污水， 工业废水的 排放量及废水中污染物的种类日益增多， 成分更加复杂， 其中含有多种难降解 有机污染物。 难降解有机污染物是指几乎不能被微生物降解， 或降解所需时间 非常长， 它们容易在水体、 土壤等自然介质中积累， 进而对环境造成危害的那 些有机化合物。 这些难降解有机废水涉及的行业很广， 主要有化工、轻工、 印 染、制药、 农药以及煤化工废水等。 这些废水中主要含有的难降解有机成分如 酚类、 南代化合物、 单环芳香化合物、 多环芳香烃、 多氯联苯、 杀虫剂、 除草 剂及染料等， 它们对环境的危害已受到世界各国的普遍重视。 控制难降解有机 污染物， 是水污染防治领域中面临的重要课题。 最近相关研究表明人工氧化还 原介体的加入可加速微生物的胞外电子传递速率， 进而有助于强化难降解有机 污染物的生物降解性能， 缩短降解时间。 因此， 氧化还原介体具有潜在的应用 价值而越来越受到国内外的广泛关注。
[0003] 所谓氧化还原介体是通过自身的氧化还原能力来传递电子， 主要参与到微生物 的胞外电子传递过程， 以加速电子传递速率， 污染物的降解速率得到显著提高 。 目前， 通常用到的氧化还原介体主要是一些醌、 吩嗪、酞菁等。 这类物质都 具有t- t共轭体系， 并且具有得失电子能力的活性位点， 如羰基 (c=o) 。 然而 这些物质都具有可溶性， 而且在生物水处理过程中， 需要定期的投加， 这样就 存在处理成本商， 对环境造成二次污染等问题。 炭质材料例如： 石墨稀、碳纳 米管、 生物炭等， 是近年来研究较多的一种重复利用率较高的氧化还原介体。 其中， 生物炭 (Biochar) 又叫做黑碳 (Black carbon) ， 是在低氧或无氧条件下 \¥0 2019/095306 卩（：1' 2017/111713
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， 生物质经高温 （通常＜700°（：） 热解 （炭化） 产生的一类难溶的、 稳定的、 高 度芳香化的、 富含碳素的固体残渣。 制备生物炭的原料成本低， 来源广泛， 主 要有木材、 果壳、 秸秆、 污泥、 动物粪便等。 相关研究结果表明， 生物炭表面 富含含氧官能团 （例如羰基、 羟基等） ， 在污染物的生物修复过程中， 生物炭 可以接收生物降解产生的电子， 接收电子后， 被还原的生物炭又可以将电子转 移给电子受体， 在整个降解过程中， 生物炭作为氧化还原介体提高了处理效率 。 然而直接将其作为氧化还原介体， 又会存在流失的问题， 因而同样会存在增 加投加成本和对环境造成二次污染等问题。 基于此， 本发明的目的是将生物炭 材料固定于热塑性树脂， 开发出一种新型热塑性树脂固定生物质炭的生物载体 技术问题
[0004] 本发明针对生物水处理技术中， 由于受到电子传递速率的限制， 对水体中难降 解有机物的处理速率慢的问题， 本发明旨在提供一种热塑性树脂固定生物质炭 的生物载体制备方法。
问题的解决方案
技术解决方案
[0005] 本发明的技术方案：
[0006] 一种热塑性树脂固定生物质炭的生物载体制备方法， 步骤如下：
[0007] （1） 将生物质炭功能料磨成粉末， 80°（:条件下烘干至恒重， 备用；
[0008] （2） 将步骤 （1） 中经过预处理的生物质炭功能料粉末与热塑性树脂颗粒机械 共混并搅拌均匀， 备用； 生物质炭功能料粉末与热塑性树脂颗粒的质量比为 20%
-50%；
[0009] （3） 利用螺杆挤出机对步骤 （2） 中的固体混合物进行熔融共混挤出、成条， 并经过机械切割得到颗粒状共混物； 螺杆挤出机的加工温度为 130°0190°（:， 保 证热塑性树脂在熔融状态下与生物质炭功能料粉末充分混合；
[0010] （4） 将步骤 （3） 中制备的颗粒状共混物与热塑性树脂颗粒机械搅拌均匀后， 添加到螺杆挤出机中共混挤出， 并根据模具头的设计得到不同形状的载体管材 颗粒状共混物中生物质炭的质量与热塑性树脂颗粒总质量比不超过 20% ; \¥0 2019/095306 卩（：1' 2017/111713
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[0011] （5） 将步骤 （4） 中制备的载体管材用机械切割的方式， 并根据所需要的尺寸 切割得到生物载体。
[0012] 所述的生物质炭功能料为草木炭、稻秆炭、稻壳炭、果壳炭、污泥生物质炭、 动物粪便生物质炭中的一种或两种以上的组合。
[0013] 所述的热塑性树脂颗粒为挤出级聚乙烯颗粒或挤出级聚丙烯颗粒。
[0014] 所述的螺杆挤出机分四段加热， 各段加热的温度范围与作用如下： （1） 温度 1 20-140°（:， 能够满足热塑性树脂达到半熔融状态， 有利于固体输送的连续性； （ 2） 温度 130-160°（:， 起到加速热塑性树脂从半熔融状态到熔融状态转化的作用， 有利于共混物在该加热段中均匀混合； （3） 温度 140-170°（:， 共混物呈固液混合 状态， 以使熔融状态的热塑性树脂与固态生物质炭功能料充分混合， 有利于生 物质炭功能料、在熔融状态下的热塑性树脂中均匀分布； （4） 温度为 115-145 以使共混物的定量、定压流出， 保证挤出的稳定性和连续性以及后续的顺利 定型。
发明的有益效果
有益效果
[0015] 本发明提供的热塑性树脂固定生物质炭的生物载体制备方法， 工艺简单， 方法 灵活可控， 适应性强， 可规模化生产， 该生物载体具有高效的对难降解有机污 染物的去除效率。
发明实施例
本发明的实施方式
[0016] 以下结合技术方案详细叙述本发明的具体实施方式。
[0017] 实施例 1
[0018] 热塑性树脂固定生物质炭生物载体的制备： （1） 将稻秆炭功能料磨成粉末， 6 0°（:条件下烘干至恒重， 备用； （2） 将步骤 （1） 中经过预处理的秸秆炭功能料 粉末与高密度聚乙烯颗粒机械共混并搅拌均匀， 备用； （3） 利用螺杆挤出机对 步骤 （2） 中的固体混合物进行熔融共混挤出、成条， 并经过机械切割得到颗粒 状共混物。 螺杆挤出机的加工温度为 175°（:。 秸秆炭功能材料与高密度聚乙烯颗 粒的质量百分比为 30%; （4） 将步骤 （3） 中制备的颗粒状共混物与热塑性树脂 \¥0 2019/095306 卩（：1' 2017/111713
4 机械搅拌均匀后， 添加到螺杆挤出机中共混挤出。 颗粒状共混物中秸秆炭的质 量与高密度聚乙烯总质量的百分比为 4% （5） 熔融混合挤出的物料经过成条、 冷却、 牵引、切粒， 并根据模具头的设计得到不同形状的载体。
[0019] 将该生物载体应用于苯酚废水的好氧生物降解实验中 （溶解氧控制在 2.0-3.0
¾/：〇 ， 已考察其对水体中微生物生物降解性能的影响。 实验中， 载体投加量 为反应器有效容积的 30%， 水力停留时间为 8小时。 实验结果表明： （1） 在无微 生物存在下， 进行了载体对水体中苯酚的吸附实验， 结果表明： 苯酚通过载体 的吸附作用的去除率不足 3%。 （2） 在由微生物存在的条件下， 相比于没有固定 生物炭的高密度聚乙烯载体， 应用高密度聚乙烯固定秸秆炭生物载体的反应器 ， 通过生物降解作用对苯酚的去除率提高了近 10%。
[0020] 实施例 2
[0021] 热塑性树脂固定生物质炭生物载体的制备： （1） 将稻壳炭功能料磨成粉末， 6 0°（:条件下烘干至恒重， 备用； （2） 将步骤 （1） 中经过预处理的稻壳炭功能料 粉末与高密度聚乙烯颗粒机械共混并搅拌均匀， 备用； （3） 利用螺杆挤出机对 步骤 （2） 中的固体混合物进行熔融共混挤出、成条， 并经过机械切割得到颗粒 状共混物。 螺杆挤出机的加工温度为 185°（:。 稻壳炭功能材料与高密度聚乙烯颗 粒的质量百分比为 50%; （4） 将步骤 （3） 中制备的颗粒状共混物与高密度聚乙 烯颗粒机械搅拌均匀后， 添加到螺杆挤出机中共混挤出。 颗粒状共混物中稻壳 炭的质量与高密度聚乙烯总质量的百分比为 8%; （5） 熔融混合挤出的物料经过 成条、 冷却、 牵引、切粒， 并根据模具头的设计得到不同形状的载体。
[0022] 羰基化改性石墨烯氧化物作为功能料的生物载体制备方法如下： （1） 羰基化 改性氧化石墨烯功能性材料的制备： 氧化石墨烯分散液， 用氨水调其 11为10, 9 0°（:水热 6小时； 冷却； 60°（:烘干， 所得固体记为 00; 将 0 00加入 2〇11^ 水中， 超声使其充分分散， 在冰水浴条件下， 加入 51111112304, 及 1.2§重铬酸钾 ， 充分搅拌， 反应 3小时， 60°（:烘干。 所得羰基化改性氧化石墨烯 （〇00） 。 （ 2） 生物载体的制备： 将羰基化改性氧化石墨烯功能料在水中超声使其充分分散 ， 聚乙烯颗粒基础原料加入到分散液中， 非溶性氧化还原介体功能材料与基础 原料的质量比为 1:100; 浸泡 211， 每半小时搅拌一次， 使水中的功能料能够充分 与高密度聚乙烯颗粒接触； 80°C烘干， 待用。 利用螺杆挤出机对物料进行熔融挤 出， 并经过冷却、 牵引、 切粒得到柱状载体。
[0023] 分别将热塑性树脂固定生物炭的生物载体、 羰基化改性石墨烯氧化物为功能料 的生物载体以及未改性载体应用于苯酚废水的好氧及厌氧生物降解实验中， 在 不同的进水负荷条件下， 对比探讨了添加不同载体的反应器对水体中微生物的 生物降解性能的影响。 实验中， 载体投加量为反应器有效容积的30%。 实验结果 如表1所示。 从表中可以看出在好氧、 无氧以及在不同进水苯酚浓度条件下， 载 有改性载体的反应器对苯酚的生物降解性能均好于未改性载体的反应器。 而在 改性载体的反应器之间， 生物炭改性载体的反应器的生物降解性能略好于载有 羰基化石墨烯氧化物改性载体的反应器。 此外， 相比于羰基化改性石墨烯氧化 物为功能料的生物载体的制备方法， 热塑型树脂固定化生物炭的生物载体制备 方法更加简单， 操作方便， 省时， 更加有利于保证生产过程的连续性。 相比于 羰基化改性石墨烯氧化物为功能料， 生物质炭功能料来源更加广泛， 廉价更有 利于实现规模化生产与应用。
[0024] 表1改性载体对苯酚生物降解能力的影响
[0025] Tab. 1 Effect of modified carriers on biodegradability of phenol
[]
\¥0 2019/095306 卩（：17€謂17/111713
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Figure imgf000007_0002
[0026] 注： ？£表示添加未改性生物载体的反应器；
Figure imgf000007_0001

Claims

\¥0 2019/095306 卩（：1' 2017/111713
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权利要求书
[权利要求 1] 一种热塑性树脂固定生物质炭的生物载体制备方法， 其特征在于， 步 骤如下：
(1) 将生物质炭功能料磨成粉末， 80° (:条件下烘干至恒重， 备用
(2) 将步骤 (1) 中经过预处理的生物质炭功能料粉末与热塑性树脂 颗粒机械共混并搅拌均匀， 备用； 生物质炭功能料粉末与热塑性树脂 颗粒的质量比为20%-50%;
(3) 利用螺杆挤出机对步骤 (2) 中的固体混合物进行熔融共混挤出 、 成条， 并经过机械切割得到颗粒状共混物； 螺杆挤出机的加工温度 为130°0190°:， 保证热塑性树脂在熔融状态下与生物质炭功能料粉 末充分混合；
(4) 将步骤 (3) 中制备的颗粒状共混物与热塑性树脂颗粒机械搅拌 均匀后， 添加到螺杆挤出机中共混挤出， 并根据模具头的设计得到不 同形状的载体管材； 颗粒状共混物中生物质炭的质量与热塑性树脂颗 粒总质量比不超过20%;
(5) 将步骤 (4) 中制备的载体管材用机械切割的方式， 并根据所需 要的尺寸切割得到生物载体。
[权利要求 2] 根据权利要求1所述的生物载体制备方法， 其特征在于， 所述的生物 质炭功能料为草木炭、 稻秆炭、 稻壳炭、 果壳炭、 污泥生物质炭、 动 物粪便生物质炭中的一种或两种以上组合。
[权利要求 3] 根据权利要求1或2所述的生物载体制备方法， 其特征在于， 所述的热 塑性树脂颗粒为挤出级聚乙烯颗粒或挤出级聚丙烯颗粒。
[权利要求 4] 根据权利要求1或2所述的生物载体制备方法， 其特征在于， 所述的螺 杆挤出机分四段加热， 各段加热的温度范围与作用如下：
(1) 温度120-140°(:， 满足热塑性树脂达到半熔融状态， 有利于固体 输送的连续性；
(2) 温度130-160°(:， 起到加速热塑性树脂从半熔融状态到熔融状态 \¥0 2019/095306 卩（：1' 2017/111713
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转化的作用， 有利于共混物在该加热段中均匀混合；
(3) 温度 140-170° (:， 共混物呈固液混合状态， 以使熔融状态的热塑 性树脂与固态生物质炭功能料充分混合， 有利于生物质炭功能料、在 熔融状态下的热塑性树脂中均匀分布；
(4) 温度为 115-145° (:， 以使共混物的定量、定压流出， 保证挤出的 稳定性和连续性以及后续的顺利定型。
[权利要求 5] 根据权利要求 3所述的生物载体制备方法， 其特征在于， 所述的螺杆 挤出机分四段加热， 各段加热的温度范围与作用如下：
(1) 温度 120-140° (:， 满足热塑性树脂达到半熔融状态， 有利于固体 输送的连续性；
(2) 温度 130-160° (:， 起到加速热塑性树脂从半熔融状态到熔融状态 转化的作用， 有利于共混物在该加热段中均匀混合；
(3) 温度 140-170° (:， 共混物呈固液混合状态， 以使熔融状态的热塑 性树脂与固态生物质炭功能料充分混合， 有利于生物质炭功能料、在 熔融状态下的热塑性树脂中均匀分布；
(4) 温度为 115-145° (:， 以使共混物的定量、定压流出， 保证挤出的 稳定性和连续性以及后续的顺利定型。
[权利要求 6] 根据权利要求 1、 2或 5所述的生物载体制备方法， 其特征在于， 所述 的生物质炭功能料表面富含含氧官能团， 具有氧化还原介体的作用。
[权利要求 7] 根据权利要求 3所述的生物载体制备方法， 其特征在于， 所述的生物 质炭功能料表面富含含氧官能团， 具有氧化还原介体的作用。
[权利要求 8] 根据权利要求 4所述的生物载体制备方法， 其特征在于， 所述的生物 质炭功能料表面富含含氧官能团， 具有氧化还原介体的作用。
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