沼液营养物的沸石吸附回收与利用
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摘要
大中型沼气工程在处理畜禽废弃物、生产沼气的同时,也会大量的产生集中型沼液。沼液是有机物经过厌氧发酵后的残留液体,其氮、磷、有机物等营养物含量较高,若直接排放则会造成环境严重污染,若环保达标处理则会费用高昂,若直接利用则需大量消纳面积。尽管目前沼液的处置方式有低成本的还田利用、自然生态净化、高成本的工厂化处理、高附加值的开发性处理等,但理想方式是将低耗处理与附加利用相结合,寻求低成本回收有用成分的同时,减轻沼液的后续处理工艺压力。
选用天然多孔介质吸附污染物是废水低成本处理常用的方法之一。沸石具有强大的离子交换性、吸附性、扩散性和催化性等特点,且取材广泛、价格低廉,常被用作废水吸附处理剂。为了提高天然沸石的吸附效率,人们常采用物理方法(如增加沸石比表面积)和化学方法(如改变阳离子交换容量)对天然沸石进行改性。鉴于目前国内外尚未见沸石吸附回收沼液中氮、磷、有机物等营养物的研究报道,本文选用天然沸石(TRF)、微波氯化钠联合改性沸石(WLF)、十六烷基溴化吡啶改性沸石(CPBF)、粉煤灰合成微米级沸石(WF)及亚微米级沸石(YWF),通过吸附-解吸试验和吸附柱试验,研究不同沸石对沼液中氮、磷、COD的吸附-解吸特征,优化吸附工作参数；然后采用沸石强化SBR系统处理沼液经吸附柱吸附后的残液；最后通过盆栽试验研究沼液饱和吸附沸石的农业肥效,达到低成本回收氮、磷、COD,实现沼液后续处理达标排放的目的。研究结果表明：
1、相比Freundlich方程,Langmuir方程对TRF、WLF、CPBF、WF、YWF等5种沸石材料的氨氮、磷、COD的等温吸附特征拟合性更好。由此计算出氨氮的吸附容量大小顺序是YWF (29.155mg/g)>WF (17.637mg/g)>WLF (10.020mg/g)>TRF (8.326mg/g)>CPBF (7.599mg/g);磷为YWF(3.169mg/g)>WF(2.653mg/g)>CPBF (1.138mg/g)>WLF (0.693mg/g)>TRF (0.611mg/g); COD为CPBF(37.736mg/g)>YWF (23.256mg/g)>WF (20.121mg/g)>WLF (13.423mg/g)>TRF (12.987mg/g).解吸试验表明,YWF、WF的氨氮和磷解吸率要显著小于其它3种材料；而对于COD,5种沸石解吸率大小顺序则是TRF>WLF> WF>YWF> CPBF。
通过吸附动力学研究可知,5种沸石对沼液氨氮、磷和COD的吸附匀呈现出“快速吸附,缓慢平衡”的特点,其中,YWF吸附速率明显高于其他4种沸石。动力学模型拟合表明,对于氨氮的吸附,5种沸石的吸附过程皆以准二级动力学方程的拟合效果为最优；对于磷的吸附,WLF、 TRF以及WF的吸附过程以一级动力学模型拟合效果为最优,而CPBF和YWF的吸附过程则以Elovich模型拟合效果最优；对于COD的吸附,TRF、 WLF、 WF和YWF的咐附过程以一级动力学方程模型拟合效果为最优,从动力学曲线和一级动力学方程表观速率常数B值的变化来看,可以认为这4种沸石材料对沼液COD的吸附反应主要由快反应膜扩散所控制。由于CPBF对沼液COD的吸附同时存在原矿区表面吸附和有机相分配作用,因而也同时存在快、慢速两种吸附反应,所以更适用于双室一级动力学模型。
结合等温吸附-解吸试验和动力学吸附试验,发现在5种沸石中,YWF具有较好的沼液氨氮、磷、COD综合吸附性能,是较理想的沼液吸附剂。
对沼液吸附影响因素进行研究发现,随着初始pH值增加,YWF和WF对氨氮的吸附量先升高后下降,而CPBF、 TRF和WLF对氨氮的吸附量则随初始pH值的增加缓慢减少。5种吸附材料中,YWF、 WF对磷的吸附量受沼液初始pH值影响较大,而CPBF、 TRF和WLF对磷的吸附量受沼液初始pH值影响较小。COD吸附研究表明,YWF、 WF对COD的吸附量随pH值的增加而逐步减小,而CPBF、 TRF和WLF则随pH值的增加出现“两低一高”趋势。沼液离子强度对吸附的影响研究表明,5种沸石对沼液氨氮的吸附量随着离子强度的增加迅速降低,其中以WLF的下降幅度最大；离子强度对沸石吸附磷和COD的影响要显著小于对氨氮吸附的影响。
2、利用CPBF与WLF作为吸附剂按体积比1：1构建改性沸石滤柱,吸附柱试验表明,在合适范围内,改性沸石填料对NH4+、TP、COD的单位吸附量与沼液进水流速成负相关,与沼液进水初始浓度成正相关；进水流速和进水初始浓度的增加,都会使目标物在改性沸石滤柱中的穿透时间减少；而随着沸石柱层高度的增加,目标物的穿透时间以及改性沸石填料对NH4+、TP、COD的单位吸附量也随之增加。因此,适当的增加柱层高度和沼液浓度、适量的减小进水流量都可有效的提高吸附柱中改性沸石填料的吸附容量和利用率,提高处理工艺的效率和经济性。
在饱和吸附柱的再生试验中,饱和吸附改性沸石填料在45℃热水中进行物理振荡后,以NaCl+Na2SO4(摩尔比为5：1,质量浓度6g/L溶液)混合液和NaCl+NaOH(摩尔比为7：13,质量浓度6g/L溶液)混合液作为再生液进行连续化学洗脱,再生后沸石对NH4+、TP、COD吸附容量恢复到新鲜改性沸石的88.15%、93.30%、84.57%。表明混合沸石具有较好的再生性,且再生成本可接受,具有一定的推广应用价值。但出于经济性考虑,再生次数应控制在3次以内。
沸石对COD的吸附效果和沼液的接触时间密切相关,对沼液中极性小、分子量大、溶解度小的有机物吸附效果较差。因此,利用改性沸石滤柱进行沼液COD吸附去除很难达到理想效果,有必要在吸附柱处理后辅以生化处理工艺,以去除沼液中难吸附有机类物质。
3、将粒径范围在40-60μm之间的粉煤灰合成沸石投入SBR系统组成ZFA-SBR系统(粉煤灰合成沸石投加型SBR),随着驯化时间的延长,生物膜逐渐在粉煤灰合成沸石上形成,为SND(同步硝化反硝化作用)创造了物质条件。ZFA-SBR和SBR相比,系统内活性污泥性能得到改善,稳定运行期SVI、 MLSS指标优于SBR。在运行周期内,ZFA-SBR与SBR的pH值变化趋势相似,但整体要比SBR高0.5-0.7个单位。ZFA-SBR反应器中的脱氮和反硝化效率较高,曝气期COD降解速率也更高。
沼液经改性沸石滤柱过滤后,按照调整沼液滤液BOD5/TN值到4左右的目的,与养殖场原水按配比进行混合,所得的混合液的可生化性相比沼液有较大改善,将其投入ZFA-SBR系统,构建“改性沸石滤柱过滤→BOD5/TN调整→ZFA-SBR"沼液处理强化工艺流程。在强化工艺稳定运行的30d内,ZFA-SBR的NH3-N、COD.TP出水达到《畜禽养殖行业污染物排放标准》规定要求,实现沼液的低耗达标处理,与SBR相比,表现出更高的去除率和抗水质负荷冲击能力。
4、通过盆栽试验,考察5种沸石吸附沼液后的产物对土壤-冬小麦系统的影响,发现A处理组(5种沸石材料+化肥)和B处理组(5种沼液饱和吸附沸石材料+部分化肥)对土壤-植物系统产生了较明显的良性影响。
在土壤方面,A处理组中的AYWF (YWF+化肥)、AWF (WF+化肥)与B处理组中的BYWF(沼液饱和吸附YWF+部分化肥)、BWF(沼液饱和吸附WF+部分化肥),均能显著提高土壤pH值,其中又以AYWF效果最为明显。土壤总氮、有机质和碱解氮含量均在BCPBF(沼液饱和吸附CPBF+部分化肥)为最高,分别为1.09、13.97mg/g和97.18mg/kg;而土壤总磷最高值由BYWF处理获得,为0.43mg/g; AYWF (YWF+化肥)处理增加土壤速效磷效果最明显,达到5.82mg/kg,可能是由于AYWF提高土壤pH值效果最明显,从而减少了土壤中磷的固定性,也促进闭蓄态磷酸盐转为非闭蓄态磷酸盐,增加了土壤磷的有效性。土壤总磷和速效磷最低值则均出现在CYWF(仅施YWF),为0.33mg/g和3.92mg/kg。
在冬小麦方面,最高生物量出现在AYWF处理,达到33.48g/pot;最高产量和千粒重分别由BYWF处理与BCPBF处理取得,相比CKl(仅施化肥)分别提高了15.29%和10.29%。
冬小麦吸氮量、吸磷量及相应的氮磷养分利用率在BywF处理中均为最高值,分别达到668.28、122.3lmg/pot和34.06%、12.93%。在A、B两个处理组内,AyWF处理和AWF处理之间以及ByWF与BWF之间吸氮量、吸磷量差异不显著(p<0.05)。
利用吸附沼液营养物至饱和的沸石(B处理组)替代部分氮磷肥,既可减少化肥成本投入,又可在一定程度上改善冬小麦生物学指标和酸性紫色土理化性质。
最后指出,虽然本文系统研究了不同沸石对沼液NH3-N、TP、COD吸附-解吸特征及其影响因素,但后续研究中应改进方法,研究吸附后的原位表征技术,以期观察到吸附前后变化情况。
In the process of treating the wastes of livestock and poultry and producing biogas, large and medium sized biogas project produces large quantity of byproduct-centralized biogas slurry. Biogas slurry is the residual liquid of organic compound by anaerobic fermentation and has high concentration of nutrients, like nitrogen, phosphorus and organic compound. If the biogas slurry is directly discharged, there will be serious environmental pollution; if the treatment of biogas slurry reach the required standards of environmental protection, the cost will be high; if the biogas slurry is directly utilized, there needs to be large area of land for digestion and accommodation。 At present, the biogas slurry disposal methods mostly consists of low-cost cropland application, natural ecological purification, high-cost factory treatment, high additional value oriented treatment and so on. The ideal treatment of biogas slurry is to couple low-consumption disposal with value added utilization, so that the valuable components of biogas slurry could be recycled at a low cost and the pressure of the subsequent treatment process could be relieved.
Using the natural porous media to absorb the pollutants is one of the most common methods of low-costly treating wastewater. In view of the powerful ion-exchange adsorbability, adsorbability, diffusivity, and catalytic property of zeolite, with extensive material and in low cost, it is commonly be used as adsorption medium in wastewater treatment. In order to raise the adsorption efficiency of natural zeolite, the physical method(for example, increasing specific surface area) and chemical method (for example, improving cation exchange capacity) are often utilized to modify the natural zeolites. In view of the fact that the adsorption of the nutrients like nitrogen, phosphorus and organic compound in biogas slurry by zeolite has not been reported at home and abroad, the thesis took TRF(Natural zeolite), WLF(Microwave-sodium chloride modified zeolite), CPBF (Cetylpyridinium Bromize modified zeolite), WF(Micro-sized zeolite synthesized from coal fly ash) and YWF(Submicro-sized zeolite synthesized from coal fly ash) as the research objects, studied the isothermal adsorption-desorption characteristics of nitrogen, phosphorus, COD in biogas slurry by five zeolite substrates through isothermal adsorption-desorption experiment and optimized working parameters through filter column experiment; treated the effluent of filter column by Zeolite-strengthened SBR; studied on the agricultural fertilizer efficiency of biogas slurry saturated adsorption zeolite through pot experiment. And then achieve the goal of low-cost recovering nutrients, like nitrogen, phosphorus and COD and promoting the subsequent treatment process of biogas slurry, reaching the required standards of environmental protection, the results showed that:
1. The isothermal adsorption characteristics of nitrogen, phc=sphorus and COD by five zeolite substrates were more suitable for Langmuir equation than Freundlich equation. According to Langmuir equation, the order of absorption capacity of anmmonium was YWF (29.155mg/g)>WF (17.637mg/g)>WLF (10.020mg/g)>TRF (8.326mg/g)>CPBF(7.599mg/g); the order of absorption capacity of phosphorus was YWF (3.169mg/g)>WF (2.653mg/g)>CPBF (1.138mg/g)>WLF (0.693mg/g)>TRF (0.611mg/g); the order of absorption capacity of COD was CPBF (37.736mg/g)>YWF (23.256mg/g)>WF (20.121mg/g)> WLF (13.423mg/g)>TRF (12.987mg/g); on the desorption rate of anmmonium and phosphorus, YWF and WF were much smaller than that of the other three materials. The order of desorption rate of COD was TRF>WLF> WF>YWF> CPBF.
On the research of absorption kinetics, the absorption of anmmonium, phosphorus and COD by the five zeolites enjoyed the characteristic of "fast absorption, slow balance ". The absorption rate of YWF was obviously higher than that of the other four zeolites.
The kinetic model fitting showed that the fitting effect of second-order kinetic model was the best for all the5zeolite materials of the ammonium absorption; the fitting effect of first-order kinetic model was the best for WLF、TRF and WF of phosphorus absorption; the fitting effect of Elovich equation was best for CPBF and YWF. In the COD absorption dynamics model, the fitting effect of first-order kinetic model was the best for TRF, WLF, WF, YWF. From the change of kinetic curve and the apparent rate constant B of first-order kinetic model, it could be concluded that the absorption of COD of biogas slurry was mainly controlled by membrane diffusion which was fast reaction.Both the effect of surface adsorption in original mining area and effect of organic distribu-tion existed in the adsorption of COD of biogas slurry by CPBF, and rapid ad-sorption and slow adsorption also existed at the same time, so CPBF was more suitable for the two-compartment first-order dynamic model.
Combined with the results of isothermal adsorption-desorption and adsorption kinetics experiments, it was found out that of the five different zeolites, YWF had better comprehensive adsorption capability of anmmonium, phosphorus and COD in biogas slurry, and was ideal adsorption medium for biogas slurry.
(?) of the influential factors on the adsorption capacity, it was found out that of the five zeolite materials, the ammonium absorption quantity of YWF and WF slowly rose along with pH value increased and then it slowly decreased with the further increase of pH value, while the ammonium absorption' quantity of CPBF、TRF and WLF slowly decreased with the increase of pH value. The phosphorus absorption quantity of YWF and WF was mostly influenced by the change of pH value, while the change of pH value had little effect on the phosphorus absorption quantity of CPBF, TRF and WLF. The COD absorption quantity of YWF and WF decreased with the increased of pH value, that of CPBF, TRF, WLF appeared the tendency of "two low and one high" with the increased of pH value. The ammonium absorption quantity of the five different zeolite materials decreased with the rose of ionic strength, of which the decrease range of the ammonium absorption quantity of WLF was the highest of the five zeolite materials. The influence exerted by ionic strength on the absorption capacity of anmmonium in biogas slurry exceeded that on phosphorus and COD.
2. WLF and CPBF were used as adsorption medium to construct mixed modified-zeolite filter column in volume ratio1:1, the research found out that in proper range, there was a negative correlation between the adsorption capacity of NH4+, TP, COD by the modified zeolites filler and inlet velocity of biogas slurry, positive correlation between that and initial concentration of biogas slurry, the strengthening of the biogas slurry influent velocity and influent initial concentration would make the penetrating time of target object decrease. With the increase of the height of filter column, the penetrating time also increase, the unit absorption of NH4+, TP, COD by modified-zeolite would increase too. Therefore, properly increasing the height of filter column and concentration of biogas slurry and reducing the biogas slurry influent velocity could effectively improve the absorption capacity and utilization ratio of the modified-zeolite contents in the filter column, and would make the process more efficiency and economic.
In the experiment of the regeneration of saturated filter column, after oscillated in hot water at45°C, then using the mixture of NaCl+Na2SO4(the molar ratio of the solution was5:1, the mass concentration was6g/L) and the mixture NaCl+NaOH(the molar ratio of the solution was7:13, the mass concentration was6g/L) as the regeneration fluid to make continuous chemical removal of the modified-zeolite saturated adsorption of biogas slurry, the absorption capacity of NH4+, TP, COD by the regenerated modified-zeolite reached88.15%,93.30%,84.57%of that of the fresh modified-zeolite. It indicated that modified-zeolite had better reproducibility and the cost of reproducing was acceptable, therefore, the mixed modified-zeolite had great value of application.But for the sake of economic consideration, the regeneration times should be controlled within3.
The absorption of COD by zeolite was closely related to the contact time with biogas slurry, and organic matters which were low polarity,small molecular weight and low solubility were difficult to be adsorbed. Therefore, the using of modified-zeolite column to absorb COD biogas slurry was not easy to reach desirable effects. In order to get the desirable effects, it was necessary to supplement the biochemical treatment after the filter column treatment, so that the organic compounds which was difficult to be absorbed in the biogas slurry could be removed.
3. Put the zeolite synthesized from coal fly ash whose range of particle size between40μm and60μm into SBR system to form ZFA-SBR system. With the prolongation of acclimation time, the biofilm was formed around the zeolite synthesized from coal fly ash, which created material prerequisite for simultaneous nitrification and denirifica-tion(SND). Compared with SBR, the properties of the activated sludge in ZFA-SBR(SBR added zeolite synthesized from coal fly ash)was improved. During the stable stage, the index of SVI, MLSS in ZFA-SBR was better than that of SBR. During the operation period, compared ZFA-SBR with SBR, the change of pH value was similar while the total value of the former was higher than SBR for0.5to0.7. The nitrogen removal and denitrification efficiency in the ZFA-SBR reactor was relatively high; the degradation rate of COD in the aeration period was also faster.
After filtrating by modified-zeolite filter column, the biogas slurry mixed with raw livestock wastewater in order to adjust the BOD5/TN value of filtrate to4, the biodegradability of mixture was improved obviously compared with biogas slurry. Put the mixture into ZFA-SBR system, and then constructed strengthening process of biogas slurry which named "filtration by modified-zeolite filter column-adjusting BOD5/TN value-ZFA-SBR".
During the30days period of stable operation of Zeolite-strengthened SBR, the effluent concentration of NH3-N, COD, TP of ZFA-SBR reached at discharge standard of pollatants (?) Lvestook and poultry breeding and realized low consumption standard treatment of biogas slurry. Compared with SBR, it showed better removal rate and resistance to impact load.
4. Through pot experiment, the influence on soil-plant system by5kinds of zeolite (?) of biogas slurry nutrients were investigated. It was found out that both A treatment group(5kinds of zeolite materials+chemical fertilizers) and B treatment group(5kinds of zeolites which saturated adsorption of biogas slurry+part of chemical fertilizers) exerted benign effect on soil-plant system.
Both AYWF treatment(YWF+chemical fertilizers), AWF treatment(WF+chemical fertilizers) of A treatment group and BYWF treatment(YWF which saturated adsorption of biogas slurry+part of chemical fertilizers), BWF treatment (WF which saturated adsorption of biogas slurry+part of chemical fertilizers) of B treatment group could dramatically raise the pH value of soil. The effect of AYWF in raising pH was the most obvious.
Of the influence on Total nitrogen, organic matter and available nitrogen, the maximum were reached by BCPBF treatment (CPBF which saturated adsorption of biogas slurry+part of chemical fertilizers), that were1.09mg/g,13.97mg/g and121.18mg/kg respectively. The maximum total phosphate and available phosphorus of soil were reached by BYWF treatment and AYWF treatment at0.43mg/g and8.02mg/kg respectively. While the minimum were reached by CYWF treatment(only YWF), that were0.33mg/g and4.12mg/kg. Probably because AWF treatment could most effectively improve soil pH value, in turn reduced the fixation of phosphorus in soil and promote occluded phosphate to convert into non occluded phosphate.
Of the various processing of the influence on winter wheat, the highest biomass of winter wheat was in AYWF treatment, that was33.48g/pot. The highest yield and1000-grain weight were reached by BYWF treatment and BCPBF treatment, compared with CK1(only using NPK), increased for15.29%and10.29%respectively.
The nitrogen, phosphorus uptake and utilization ratios of winter wheat, all reached the highest value in BYWF treatment at668.28,122.31mg/pot and34.06%,12.93% respectively.
Within the range of A treatment group, the difference of nitrogen uptake and phosphorous uptake between AYWF treatment and AWF treatment was not obvious(p<0.05), and the difference between BYWF treatment and BWF treatment in B treatment group was also not obvious(p<0.05).
The zeolite saturated adsorption of biogas slurry nutrients could partially substitute nitrogen and phosphorus fertilizers, and this would reduce the cost of fertilizers, improve the physicochemical properties of acid purple soil and the biological indexes and nutrient utilization of winter wheat to some extents, and mitigate water environment and atmospheric environment damage caused by the low utilization ratio of fertilizer.
In the end, the thesis pointed out that the test systematically studied the adsorption-desorption characteristics and the influential factors of NH3-N, TP, COD in biogas slurry by different zeolites, but in the subsequent research the in situ characterization techniques should be used in order to observe the changes before and after adsorption factually.
选用天然多孔介质吸附污染物是废水低成本处理常用的方法之一。沸石具有强大的离子交换性、吸附性、扩散性和催化性等特点,且取材广泛、价格低廉,常被用作废水吸附处理剂。为了提高天然沸石的吸附效率,人们常采用物理方法(如增加沸石比表面积)和化学方法(如改变阳离子交换容量)对天然沸石进行改性。鉴于目前国内外尚未见沸石吸附回收沼液中氮、磷、有机物等营养物的研究报道,本文选用天然沸石(TRF)、微波氯化钠联合改性沸石(WLF)、十六烷基溴化吡啶改性沸石(CPBF)、粉煤灰合成微米级沸石(WF)及亚微米级沸石(YWF),通过吸附-解吸试验和吸附柱试验,研究不同沸石对沼液中氮、磷、COD的吸附-解吸特征,优化吸附工作参数；然后采用沸石强化SBR系统处理沼液经吸附柱吸附后的残液；最后通过盆栽试验研究沼液饱和吸附沸石的农业肥效,达到低成本回收氮、磷、COD,实现沼液后续处理达标排放的目的。研究结果表明：
1、相比Freundlich方程,Langmuir方程对TRF、WLF、CPBF、WF、YWF等5种沸石材料的氨氮、磷、COD的等温吸附特征拟合性更好。由此计算出氨氮的吸附容量大小顺序是YWF (29.155mg/g)>WF (17.637mg/g)>WLF (10.020mg/g)>TRF (8.326mg/g)>CPBF (7.599mg/g);磷为YWF(3.169mg/g)>WF(2.653mg/g)>CPBF (1.138mg/g)>WLF (0.693mg/g)>TRF (0.611mg/g); COD为CPBF(37.736mg/g)>YWF (23.256mg/g)>WF (20.121mg/g)>WLF (13.423mg/g)>TRF (12.987mg/g).解吸试验表明,YWF、WF的氨氮和磷解吸率要显著小于其它3种材料；而对于COD,5种沸石解吸率大小顺序则是TRF>WLF> WF>YWF> CPBF。
通过吸附动力学研究可知,5种沸石对沼液氨氮、磷和COD的吸附匀呈现出“快速吸附,缓慢平衡”的特点,其中,YWF吸附速率明显高于其他4种沸石。动力学模型拟合表明,对于氨氮的吸附,5种沸石的吸附过程皆以准二级动力学方程的拟合效果为最优；对于磷的吸附,WLF、 TRF以及WF的吸附过程以一级动力学模型拟合效果为最优,而CPBF和YWF的吸附过程则以Elovich模型拟合效果最优；对于COD的吸附,TRF、 WLF、 WF和YWF的咐附过程以一级动力学方程模型拟合效果为最优,从动力学曲线和一级动力学方程表观速率常数B值的变化来看,可以认为这4种沸石材料对沼液COD的吸附反应主要由快反应膜扩散所控制。由于CPBF对沼液COD的吸附同时存在原矿区表面吸附和有机相分配作用,因而也同时存在快、慢速两种吸附反应,所以更适用于双室一级动力学模型。
结合等温吸附-解吸试验和动力学吸附试验,发现在5种沸石中,YWF具有较好的沼液氨氮、磷、COD综合吸附性能,是较理想的沼液吸附剂。
对沼液吸附影响因素进行研究发现,随着初始pH值增加,YWF和WF对氨氮的吸附量先升高后下降,而CPBF、 TRF和WLF对氨氮的吸附量则随初始pH值的增加缓慢减少。5种吸附材料中,YWF、 WF对磷的吸附量受沼液初始pH值影响较大,而CPBF、 TRF和WLF对磷的吸附量受沼液初始pH值影响较小。COD吸附研究表明,YWF、 WF对COD的吸附量随pH值的增加而逐步减小,而CPBF、 TRF和WLF则随pH值的增加出现“两低一高”趋势。沼液离子强度对吸附的影响研究表明,5种沸石对沼液氨氮的吸附量随着离子强度的增加迅速降低,其中以WLF的下降幅度最大；离子强度对沸石吸附磷和COD的影响要显著小于对氨氮吸附的影响。
2、利用CPBF与WLF作为吸附剂按体积比1：1构建改性沸石滤柱,吸附柱试验表明,在合适范围内,改性沸石填料对NH4+、TP、COD的单位吸附量与沼液进水流速成负相关,与沼液进水初始浓度成正相关；进水流速和进水初始浓度的增加,都会使目标物在改性沸石滤柱中的穿透时间减少；而随着沸石柱层高度的增加,目标物的穿透时间以及改性沸石填料对NH4+、TP、COD的单位吸附量也随之增加。因此,适当的增加柱层高度和沼液浓度、适量的减小进水流量都可有效的提高吸附柱中改性沸石填料的吸附容量和利用率,提高处理工艺的效率和经济性。
在饱和吸附柱的再生试验中,饱和吸附改性沸石填料在45℃热水中进行物理振荡后,以NaCl+Na2SO4(摩尔比为5：1,质量浓度6g/L溶液)混合液和NaCl+NaOH(摩尔比为7：13,质量浓度6g/L溶液)混合液作为再生液进行连续化学洗脱,再生后沸石对NH4+、TP、COD吸附容量恢复到新鲜改性沸石的88.15%、93.30%、84.57%。表明混合沸石具有较好的再生性,且再生成本可接受,具有一定的推广应用价值。但出于经济性考虑,再生次数应控制在3次以内。
沸石对COD的吸附效果和沼液的接触时间密切相关,对沼液中极性小、分子量大、溶解度小的有机物吸附效果较差。因此,利用改性沸石滤柱进行沼液COD吸附去除很难达到理想效果,有必要在吸附柱处理后辅以生化处理工艺,以去除沼液中难吸附有机类物质。
3、将粒径范围在40-60μm之间的粉煤灰合成沸石投入SBR系统组成ZFA-SBR系统(粉煤灰合成沸石投加型SBR),随着驯化时间的延长,生物膜逐渐在粉煤灰合成沸石上形成,为SND(同步硝化反硝化作用)创造了物质条件。ZFA-SBR和SBR相比,系统内活性污泥性能得到改善,稳定运行期SVI、 MLSS指标优于SBR。在运行周期内,ZFA-SBR与SBR的pH值变化趋势相似,但整体要比SBR高0.5-0.7个单位。ZFA-SBR反应器中的脱氮和反硝化效率较高,曝气期COD降解速率也更高。
沼液经改性沸石滤柱过滤后,按照调整沼液滤液BOD5/TN值到4左右的目的,与养殖场原水按配比进行混合,所得的混合液的可生化性相比沼液有较大改善,将其投入ZFA-SBR系统,构建“改性沸石滤柱过滤→BOD5/TN调整→ZFA-SBR"沼液处理强化工艺流程。在强化工艺稳定运行的30d内,ZFA-SBR的NH3-N、COD.TP出水达到《畜禽养殖行业污染物排放标准》规定要求,实现沼液的低耗达标处理,与SBR相比,表现出更高的去除率和抗水质负荷冲击能力。
4、通过盆栽试验,考察5种沸石吸附沼液后的产物对土壤-冬小麦系统的影响,发现A处理组(5种沸石材料+化肥)和B处理组(5种沼液饱和吸附沸石材料+部分化肥)对土壤-植物系统产生了较明显的良性影响。
在土壤方面,A处理组中的AYWF (YWF+化肥)、AWF (WF+化肥)与B处理组中的BYWF(沼液饱和吸附YWF+部分化肥)、BWF(沼液饱和吸附WF+部分化肥),均能显著提高土壤pH值,其中又以AYWF效果最为明显。土壤总氮、有机质和碱解氮含量均在BCPBF(沼液饱和吸附CPBF+部分化肥)为最高,分别为1.09、13.97mg/g和97.18mg/kg;而土壤总磷最高值由BYWF处理获得,为0.43mg/g; AYWF (YWF+化肥)处理增加土壤速效磷效果最明显,达到5.82mg/kg,可能是由于AYWF提高土壤pH值效果最明显,从而减少了土壤中磷的固定性,也促进闭蓄态磷酸盐转为非闭蓄态磷酸盐,增加了土壤磷的有效性。土壤总磷和速效磷最低值则均出现在CYWF(仅施YWF),为0.33mg/g和3.92mg/kg。
在冬小麦方面,最高生物量出现在AYWF处理,达到33.48g/pot;最高产量和千粒重分别由BYWF处理与BCPBF处理取得,相比CKl(仅施化肥)分别提高了15.29%和10.29%。
冬小麦吸氮量、吸磷量及相应的氮磷养分利用率在BywF处理中均为最高值,分别达到668.28、122.3lmg/pot和34.06%、12.93%。在A、B两个处理组内,AyWF处理和AWF处理之间以及ByWF与BWF之间吸氮量、吸磷量差异不显著(p<0.05)。
利用吸附沼液营养物至饱和的沸石(B处理组)替代部分氮磷肥,既可减少化肥成本投入,又可在一定程度上改善冬小麦生物学指标和酸性紫色土理化性质。
最后指出,虽然本文系统研究了不同沸石对沼液NH3-N、TP、COD吸附-解吸特征及其影响因素,但后续研究中应改进方法,研究吸附后的原位表征技术,以期观察到吸附前后变化情况。
In the process of treating the wastes of livestock and poultry and producing biogas, large and medium sized biogas project produces large quantity of byproduct-centralized biogas slurry. Biogas slurry is the residual liquid of organic compound by anaerobic fermentation and has high concentration of nutrients, like nitrogen, phosphorus and organic compound. If the biogas slurry is directly discharged, there will be serious environmental pollution; if the treatment of biogas slurry reach the required standards of environmental protection, the cost will be high; if the biogas slurry is directly utilized, there needs to be large area of land for digestion and accommodation。 At present, the biogas slurry disposal methods mostly consists of low-cost cropland application, natural ecological purification, high-cost factory treatment, high additional value oriented treatment and so on. The ideal treatment of biogas slurry is to couple low-consumption disposal with value added utilization, so that the valuable components of biogas slurry could be recycled at a low cost and the pressure of the subsequent treatment process could be relieved.
Using the natural porous media to absorb the pollutants is one of the most common methods of low-costly treating wastewater. In view of the powerful ion-exchange adsorbability, adsorbability, diffusivity, and catalytic property of zeolite, with extensive material and in low cost, it is commonly be used as adsorption medium in wastewater treatment. In order to raise the adsorption efficiency of natural zeolite, the physical method(for example, increasing specific surface area) and chemical method (for example, improving cation exchange capacity) are often utilized to modify the natural zeolites. In view of the fact that the adsorption of the nutrients like nitrogen, phosphorus and organic compound in biogas slurry by zeolite has not been reported at home and abroad, the thesis took TRF(Natural zeolite), WLF(Microwave-sodium chloride modified zeolite), CPBF (Cetylpyridinium Bromize modified zeolite), WF(Micro-sized zeolite synthesized from coal fly ash) and YWF(Submicro-sized zeolite synthesized from coal fly ash) as the research objects, studied the isothermal adsorption-desorption characteristics of nitrogen, phosphorus, COD in biogas slurry by five zeolite substrates through isothermal adsorption-desorption experiment and optimized working parameters through filter column experiment; treated the effluent of filter column by Zeolite-strengthened SBR; studied on the agricultural fertilizer efficiency of biogas slurry saturated adsorption zeolite through pot experiment. And then achieve the goal of low-cost recovering nutrients, like nitrogen, phosphorus and COD and promoting the subsequent treatment process of biogas slurry, reaching the required standards of environmental protection, the results showed that:
1. The isothermal adsorption characteristics of nitrogen, phc=sphorus and COD by five zeolite substrates were more suitable for Langmuir equation than Freundlich equation. According to Langmuir equation, the order of absorption capacity of anmmonium was YWF (29.155mg/g)>WF (17.637mg/g)>WLF (10.020mg/g)>TRF (8.326mg/g)>CPBF(7.599mg/g); the order of absorption capacity of phosphorus was YWF (3.169mg/g)>WF (2.653mg/g)>CPBF (1.138mg/g)>WLF (0.693mg/g)>TRF (0.611mg/g); the order of absorption capacity of COD was CPBF (37.736mg/g)>YWF (23.256mg/g)>WF (20.121mg/g)> WLF (13.423mg/g)>TRF (12.987mg/g); on the desorption rate of anmmonium and phosphorus, YWF and WF were much smaller than that of the other three materials. The order of desorption rate of COD was TRF>WLF> WF>YWF> CPBF.
On the research of absorption kinetics, the absorption of anmmonium, phosphorus and COD by the five zeolites enjoyed the characteristic of "fast absorption, slow balance ". The absorption rate of YWF was obviously higher than that of the other four zeolites.
The kinetic model fitting showed that the fitting effect of second-order kinetic model was the best for all the5zeolite materials of the ammonium absorption; the fitting effect of first-order kinetic model was the best for WLF、TRF and WF of phosphorus absorption; the fitting effect of Elovich equation was best for CPBF and YWF. In the COD absorption dynamics model, the fitting effect of first-order kinetic model was the best for TRF, WLF, WF, YWF. From the change of kinetic curve and the apparent rate constant B of first-order kinetic model, it could be concluded that the absorption of COD of biogas slurry was mainly controlled by membrane diffusion which was fast reaction.Both the effect of surface adsorption in original mining area and effect of organic distribu-tion existed in the adsorption of COD of biogas slurry by CPBF, and rapid ad-sorption and slow adsorption also existed at the same time, so CPBF was more suitable for the two-compartment first-order dynamic model.
Combined with the results of isothermal adsorption-desorption and adsorption kinetics experiments, it was found out that of the five different zeolites, YWF had better comprehensive adsorption capability of anmmonium, phosphorus and COD in biogas slurry, and was ideal adsorption medium for biogas slurry.
(?) of the influential factors on the adsorption capacity, it was found out that of the five zeolite materials, the ammonium absorption quantity of YWF and WF slowly rose along with pH value increased and then it slowly decreased with the further increase of pH value, while the ammonium absorption' quantity of CPBF、TRF and WLF slowly decreased with the increase of pH value. The phosphorus absorption quantity of YWF and WF was mostly influenced by the change of pH value, while the change of pH value had little effect on the phosphorus absorption quantity of CPBF, TRF and WLF. The COD absorption quantity of YWF and WF decreased with the increased of pH value, that of CPBF, TRF, WLF appeared the tendency of "two low and one high" with the increased of pH value. The ammonium absorption quantity of the five different zeolite materials decreased with the rose of ionic strength, of which the decrease range of the ammonium absorption quantity of WLF was the highest of the five zeolite materials. The influence exerted by ionic strength on the absorption capacity of anmmonium in biogas slurry exceeded that on phosphorus and COD.
2. WLF and CPBF were used as adsorption medium to construct mixed modified-zeolite filter column in volume ratio1:1, the research found out that in proper range, there was a negative correlation between the adsorption capacity of NH4+, TP, COD by the modified zeolites filler and inlet velocity of biogas slurry, positive correlation between that and initial concentration of biogas slurry, the strengthening of the biogas slurry influent velocity and influent initial concentration would make the penetrating time of target object decrease. With the increase of the height of filter column, the penetrating time also increase, the unit absorption of NH4+, TP, COD by modified-zeolite would increase too. Therefore, properly increasing the height of filter column and concentration of biogas slurry and reducing the biogas slurry influent velocity could effectively improve the absorption capacity and utilization ratio of the modified-zeolite contents in the filter column, and would make the process more efficiency and economic.
In the experiment of the regeneration of saturated filter column, after oscillated in hot water at45°C, then using the mixture of NaCl+Na2SO4(the molar ratio of the solution was5:1, the mass concentration was6g/L) and the mixture NaCl+NaOH(the molar ratio of the solution was7:13, the mass concentration was6g/L) as the regeneration fluid to make continuous chemical removal of the modified-zeolite saturated adsorption of biogas slurry, the absorption capacity of NH4+, TP, COD by the regenerated modified-zeolite reached88.15%,93.30%,84.57%of that of the fresh modified-zeolite. It indicated that modified-zeolite had better reproducibility and the cost of reproducing was acceptable, therefore, the mixed modified-zeolite had great value of application.But for the sake of economic consideration, the regeneration times should be controlled within3.
The absorption of COD by zeolite was closely related to the contact time with biogas slurry, and organic matters which were low polarity,small molecular weight and low solubility were difficult to be adsorbed. Therefore, the using of modified-zeolite column to absorb COD biogas slurry was not easy to reach desirable effects. In order to get the desirable effects, it was necessary to supplement the biochemical treatment after the filter column treatment, so that the organic compounds which was difficult to be absorbed in the biogas slurry could be removed.
3. Put the zeolite synthesized from coal fly ash whose range of particle size between40μm and60μm into SBR system to form ZFA-SBR system. With the prolongation of acclimation time, the biofilm was formed around the zeolite synthesized from coal fly ash, which created material prerequisite for simultaneous nitrification and denirifica-tion(SND). Compared with SBR, the properties of the activated sludge in ZFA-SBR(SBR added zeolite synthesized from coal fly ash)was improved. During the stable stage, the index of SVI, MLSS in ZFA-SBR was better than that of SBR. During the operation period, compared ZFA-SBR with SBR, the change of pH value was similar while the total value of the former was higher than SBR for0.5to0.7. The nitrogen removal and denitrification efficiency in the ZFA-SBR reactor was relatively high; the degradation rate of COD in the aeration period was also faster.
After filtrating by modified-zeolite filter column, the biogas slurry mixed with raw livestock wastewater in order to adjust the BOD5/TN value of filtrate to4, the biodegradability of mixture was improved obviously compared with biogas slurry. Put the mixture into ZFA-SBR system, and then constructed strengthening process of biogas slurry which named "filtration by modified-zeolite filter column-adjusting BOD5/TN value-ZFA-SBR".
During the30days period of stable operation of Zeolite-strengthened SBR, the effluent concentration of NH3-N, COD, TP of ZFA-SBR reached at discharge standard of pollatants (?) Lvestook and poultry breeding and realized low consumption standard treatment of biogas slurry. Compared with SBR, it showed better removal rate and resistance to impact load.
4. Through pot experiment, the influence on soil-plant system by5kinds of zeolite (?) of biogas slurry nutrients were investigated. It was found out that both A treatment group(5kinds of zeolite materials+chemical fertilizers) and B treatment group(5kinds of zeolites which saturated adsorption of biogas slurry+part of chemical fertilizers) exerted benign effect on soil-plant system.
Both AYWF treatment(YWF+chemical fertilizers), AWF treatment(WF+chemical fertilizers) of A treatment group and BYWF treatment(YWF which saturated adsorption of biogas slurry+part of chemical fertilizers), BWF treatment (WF which saturated adsorption of biogas slurry+part of chemical fertilizers) of B treatment group could dramatically raise the pH value of soil. The effect of AYWF in raising pH was the most obvious.
Of the influence on Total nitrogen, organic matter and available nitrogen, the maximum were reached by BCPBF treatment (CPBF which saturated adsorption of biogas slurry+part of chemical fertilizers), that were1.09mg/g,13.97mg/g and121.18mg/kg respectively. The maximum total phosphate and available phosphorus of soil were reached by BYWF treatment and AYWF treatment at0.43mg/g and8.02mg/kg respectively. While the minimum were reached by CYWF treatment(only YWF), that were0.33mg/g and4.12mg/kg. Probably because AWF treatment could most effectively improve soil pH value, in turn reduced the fixation of phosphorus in soil and promote occluded phosphate to convert into non occluded phosphate.
Of the various processing of the influence on winter wheat, the highest biomass of winter wheat was in AYWF treatment, that was33.48g/pot. The highest yield and1000-grain weight were reached by BYWF treatment and BCPBF treatment, compared with CK1(only using NPK), increased for15.29%and10.29%respectively.
The nitrogen, phosphorus uptake and utilization ratios of winter wheat, all reached the highest value in BYWF treatment at668.28,122.31mg/pot and34.06%,12.93% respectively.
Within the range of A treatment group, the difference of nitrogen uptake and phosphorous uptake between AYWF treatment and AWF treatment was not obvious(p<0.05), and the difference between BYWF treatment and BWF treatment in B treatment group was also not obvious(p<0.05).
The zeolite saturated adsorption of biogas slurry nutrients could partially substitute nitrogen and phosphorus fertilizers, and this would reduce the cost of fertilizers, improve the physicochemical properties of acid purple soil and the biological indexes and nutrient utilization of winter wheat to some extents, and mitigate water environment and atmospheric environment damage caused by the low utilization ratio of fertilizer.
In the end, the thesis pointed out that the test systematically studied the adsorption-desorption characteristics and the influential factors of NH3-N, TP, COD in biogas slurry by different zeolites, but in the subsequent research the in situ characterization techniques should be used in order to observe the changes before and after adsorption factually.
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