The Progress in the Research on Carbon Emissions from Livestock and Poultry Breeding in China
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摘要: 为了实现全球气温上升不超过2 ℃的目标，探索碳减排的措施迫在眉睫。鉴于畜禽养殖业是碳排放的一个重要来源，文章综述了国内畜禽养殖业碳排放相关的研究进展，介绍了畜禽养殖业碳排放的测算方法、时空特征、影响因素与减排措施。Abstract: It is urgent to explore measures for reducing carbon emissions in order to achieve the goal that the global temperature will not rise above 2 ℃. Livestock and poultry breeding is an important source of carbon emissions. The progress in the research on carbon emissions from domestic livestock and poultry breeding is summarized and the calculation method, spatio-temporal characteristics, factors and emission reduction measures regarding carbon emissions from livestock and poultry breeding are introduced.
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葡萄糖可以大量地从自然界中获取，是一种可再生的资源. 5-羟甲基糠醛(HMF)，是一种重要的生物基平台化合物，可以通过加氢、氧化脱氢、酯化、卤化、聚合、水解等化学反应制备多种衍生物，减少人类对化石能源的依赖[1-3]. 葡萄糖转化为HMF的化学反应并不容易发生，需要较高的活化能[4-5]. 为了提高HMF的收率和选择性，反应通常在高温条件下进行. 同时，葡萄糖在转化为HMF的过程中，容易发生副反应，而且以水作为反应溶剂时，生成的HMF容易水解，产生大量的副反应产物，使得HMF的收率降低[6-7].
过去多数研究以有机溶剂作为反应溶剂抑制HMF的水解，减少副反应的发生，例如二甲基亚砜(DMSO)[8]. ROMÁN-LESHKOV[9]提出了一种双相体系，通过在反应过程中不断将水相中的HMF萃取到有机相中，同样可以减少副反应的发生. ZHAO等[10]提出以[EMIM][Cl]离子液体作为反应溶剂，能够显著减少副反应的发生，以葡萄糖作为反应底物时，HMF的收率达到70%(100 ℃，3 h).
通过对反应溶剂的选择，可以获得较高的HMF收率，特别是离子液体的应用有效抑制了副反应的发生，降低了反应温度. 与有机溶剂相比，离子液体更环保，目前尚未有数据证明离子液体对环境有污染. 但现实的问题是，离子液体的价格昂贵，难以与产物分离，不适合在工业上生产HMF[11-13].
研究人员尝试在水中将葡萄糖转化为HMF，但这十分困难. 以水作为反应溶剂时，反应通常在高温、高压下进行，且通过以果糖作为反应底物获得较高的HMF收率. 例如，HANSEN等[6]报道了以HCl作为催化剂、果糖作为反应底物，200 ℃下微波水热反应60 s后，果糖的转化率为95%，HMF的选择性为55%；TUERCKE等[14]采用连续微反应器工艺，在185 ℃条件下，以HCl作为催化剂、果糖作为反应底物，果糖的转化率为71%，HMF的选择性为75%. 通常情况下，以果糖作为反应底物能够获得更高的HMF收率. 目前主流的假设：葡萄糖在转化为HMF的过程中，先异构成果糖，再以果糖为起始物进行反应. 葡萄糖转化为HMF的速率主要受葡萄糖异构成果糖速率的影响，而葡萄糖异构成果糖所需的活化能较高，导致HMF的收率和选择性较低.
NOMA等[13]通过同位素标记法，跟踪了3-deoxyglucosone(脱氧葡萄糖酮醛)中间体的形成，证明了以TiO2和磷酸/TiO2作为催化剂时，葡萄糖先异构成活泼的烯醇中间体，然后脱水形成脱氧葡萄糖酮醛中间体，最后脱水形成HMF(Pathway D). 在这种路径下，由于不需要先异构成果糖，葡萄糖转化为HMF的收率得到了较大的提高. LANZIANO等[7]制备了hybrid-TiO2催化剂，在130 ℃下水热反应5 h催化葡萄糖转化为HMF的收率为45%，葡萄糖转化率为75%. 因此，以TiO2作为催化剂时，可以在较低的反应温度下，以廉价、易得、无污染的水作为反应溶剂，获得较高的HMF收率.
为了进一步降低HMF的制备成本，推动HMF的工业化生产进程. 本研究以聚乙二醇200为溶剂[15]，采用溶胶凝胶法[16]制备纳米TiO2溶胶催化剂，产物为交联丝状[17]；以水作为反应溶剂、葡萄糖作为反应底物，利用一锅法制备HMF，采用高效液相色谱法进行检测[18]，并对其工艺进行评估，寻找适合工业化生产的条件.
1. 实验部分
1.1 试剂与仪器
主要试剂：聚乙二醇200(PEG 200)、甲酸、氘代氯仿为分析纯，乙腈为色谱纯，购于中国阿拉丁试剂(上海)有限公司；钛酸丁酯(TiO2质量分数为33%~35%)、无水乙醇、二甲基亚砜(DMSO)为分析纯，购于中国天津大茂化学试剂有限公司；钛酸乙酯(TiO2质量分数为33%~35%)为分析纯，购于中国上海麦克林生化科技有限公司；D-葡萄糖、5-羟甲基糠醛(HMF)为色谱纯，购于中国源叶生物科技(上海)有限公司.
主要仪器：陶瓷纤维马弗炉(HG-12-4B，上海禾工科学仪器有限公司)、X射线粉末衍射仪(D8 ADVANCE，布鲁克(北京))、透射电子显微镜(JEOL JSM 2100，200 kV，日本电子)、场发射扫描电子显微镜(ZEISS Gemini 500，德国卡尔·蔡司)、纳米粒径电位分析仪(SZ-100, 英国马尔文).
1.2 催化剂的制备
纳米TiO2溶胶的制备：将20 mL去离子水与250 mL乙醇混合，用5%的HNO3溶液调节溶液pH至1.8，记为A溶液；将10 mL钛酸丁酯与250 mL无水乙醇混合得到B溶液；在搅拌状态下，将B溶液迅速加入到A溶液中，30 min后加入200 mL水，搅拌均匀，记为纳米TiO2溶胶.
纳米TiO2粉体的制备：将100 mL水与500 mL乙醇混合，用5%的HNO3溶液调节pH至1.8，记为A溶液；将10 mL钛酸丁酯与90 mL乙醇混合得到B溶液；将B溶液慢慢滴入A溶液中，搅拌并静置足够长的时间，形成溶胶. 将溶胶置于鼓风干燥箱中100 ℃下干燥12 h，将得到的固体研磨30 min，记为纳米TiO2粉体.
PEG-TiO2溶胶的制备：在烘箱中加热PEG 200和钛酸乙酯至50 ℃，然后在搅拌条件下将50 mL钛酸乙酯倒入200 mL PEG 200溶剂中，快速倒入120 mL去离子水，钛酸乙酯快速水解生成氢氧化钛水合物，搅拌4 h，得到分散性良好的370 mL PEG-TiO2溶胶. 在此过程中，前期钛酸乙酯快速水解可能会导致溶胶成蜡状，但通过增加机械搅拌的力度使溶胶恢复为流体，制得PEG-TiO2溶胶性质稳定，静置不发生沉淀.
PEG-TiO2的制备：将制得的PEG-TiO2溶胶用水蒸气蒸馏法除去溶剂，然后在烘箱中90 ℃下干燥，在马弗炉中600 ℃下反应2 h，所得产物记为PEG-TiO2.
1.3 催化剂的表征结果
采用透射电子显微镜(TEM)和场发射扫描电子显微镜(SEM)对催化剂进行表征. 采用X-射线衍射仪进行表征，扫描角度从20°到90°，扫描速率为5°/min. 采用纳米粒径电位分析仪进行表征，采用粒径样品池测量平均粒径.
2. 结果与讨论
2.1 不同催化剂的TEM和SEM表征
纳米TiO2溶胶为无定形的结构(图 1A), 纳米TiO2为球形微粒，其粒径约10~15 nm(图 1B). 采用钛酸乙酯和PEG 200为原料制备得到PEG-TiO2溶胶，其形貌为交联丝状的无定形结构(图 1C). 根据文献[15]的研究，钛酸乙酯在PEG 200溶剂中水解时，会形成Ti—O—PEG键，使得形成的PEG-TiO2溶胶呈交联丝状结构，疏松且不易团聚. 将PEG-TiO2溶胶干燥后在600 ℃下烧结，得到的PEG-TiO2为质密的片状结构(图 1D).
2.2 不同催化剂的XRD表征结果
将PEG-TiO2溶胶干燥后得到的PEG-TiO2，无明显的X射线衍射现象，说明其没有形成晶体，为无定形(图 2曲线a). 将PEG-TiO2在600 ℃下烧结得到锐钛矿型TiO2 (图 2曲线b)；在700、800 ℃下烧结得到金红石型TiO2 (图 2曲线c、d). 因此，通过对干燥后的PEG-TiO2溶胶进行烧结，可以得到锐钛矿型和金红石型的TiO2，但PEG-TiO2溶胶为无定形.
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图 2 不同催化剂的XRD图谱注：a为干燥的PEG-TiO2溶胶，b为600 ℃下烧结得到的PEG-TiO2溶胶，c为700 ℃下烧结得到的PEG-TiO2溶胶，d为800 ℃下烧结得到的PEG-TiO2溶胶.Figure 2. The XRD pattern of different catalysts2.3 不同催化剂的平均粒径
新制纳米TiO2溶胶的平均粒径为52 nm(表 1)，放置2 d后，最终纳米TiO2溶胶的平均粒径为352 nm，粒径较均匀(PdI < 0.5). PEG-TiO2溶胶的平均粒径为1 510 nm，说明其交联网状结构的聚集体使平均粒径更大，且粒径不均匀(PdI=1.000).
表 1 催化剂的平均粒径Table 1. The average particle size of catalysts样品 平均粒径/nm PdI 纳米TiO2溶胶a 52 0.184 纳米TiO2溶胶b 352 0.303 PEG-TiO2溶胶c 1 510 1.000 PEG-TiO2溶胶d 1 580 1.000 注：a为新制的纳米TiO2溶胶; b为放置2 d后的纳米TiO2溶胶；c为新制的PEG-TiO2溶胶; d为放置2 d后的PEG-TiO2溶胶. 2.4 纳米TiO2溶胶的催化性能
以纳米TiO2溶胶作为催化剂时，将葡萄糖直接加入到纳米TiO2溶胶中，然后在冷凝回流条件下对体系进行加热，测得体系的温度为79 ℃. 这是由于纳米TiO2溶胶中存在大量的乙醇，使得体系的沸点较低. 取100 mL纳米TiO2溶胶，加入0.5 g葡萄糖，反应6 h后，葡萄糖转化率为93.74%，HMF收率为21.72%，HMF的选择性为23.17%. 反应12 h后，葡萄糖转化率为93.84%，HMF收率为28.58%，HMF的选择性为30.45%(图 3A). 以纳米TiO2粉体作为催化剂时，以水作为反应溶剂，同样在冷凝回流条件下对体系进行加热，测得体系的温度为100 ℃. 取3 g纳米TiO2，加入0.5 g葡萄糖，反应6 h后，葡萄糖的转化率接近100%，HMF收率为1.41%(图 3B). 因此，采用纳米TiO2溶胶作为催化剂能够有效提高HMF的收率，可以避免纳米TiO2粉体在干燥、烧结过程中的团聚，充分发挥纳米TiO2粉体的催化效果.
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图 3 纳米TiO2溶胶和粉体的催化效果注：A采用100 mL纳米TiO2溶胶和0.5 g葡萄糖，在79 ℃下反应; B采用100 mL水和2 g葡萄糖，在100 ℃下反应.Figure 3. The catalytic effects of nano TiO2 gel and powders2.5 PEG-TiO2溶胶的催化性能
纳米TiO2溶胶具有更好的催化效果，但其纳米TiO2固含量较低，这增加了储存和运输的成本. 因此我们以PEG 200作为反应溶剂制备了PEG-TiO2溶胶，具有更高的纳米TiO2固含量. 当以PEG-TiO2溶胶为催化剂时，分别取20、30和40 mL溶胶，加入水至总体积为100 mL，加入0.5 g葡萄糖，在100 ℃温度下反应6 h. 如图 4所示，在PEG-TiO2溶胶最佳投加量(30 mL)条件下，HMF收率为17.70%，葡萄糖转化率为55.55%，对HMF的选择性为31.86%. 因此，以PEG-TiO2溶胶为催化剂对HMF具有更高的选择性，也更具有经济优势.
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图 4 催化剂体积对收率和转化率的影响注：以PEG-TiO2溶胶为催化剂，加水至反应液总体积为100 mL，葡萄糖为0.5 g，温度为100 ℃，反应时间为6 h.Figure 4. The effect of catalyst volume on the yield and the conversion rate2.6 PEG-TiO2溶胶的催化性能
为了进一步提高HMF的收率，研究以PEG-TiO2溶胶和甲酸作为协同催化剂，研究了甲酸的体积和反应时间对HMF收率和葡萄糖转化率的影响(图 5). 最佳的甲酸体积为40 mL，此时HMF的选择性最大(43.17%，图 5A). 当甲酸体积为40 mL时，连续反应12 h研究最佳的反应时间. 反应6 h后，HMF收率为46.4%，葡萄糖转化率为79.30%，HMF的选择性为58.51%；反应12 h后，HMF收率为56.20%，葡萄糖转化率为92.00%，HMF的选择性为61.09%. 因此，在最佳条件下，反应12 h，HMF收率可达56.20%，HMF的选择性可达61.09%. 因此，以PEG-TiO2和甲酸为催化剂可以获得较高的HMF收率，同时HMF的选择性较高.
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图 5 甲酸体积和反应时间对收率和转化率的影响注：反应液总体积为100 mL，葡萄糖为2 g，温度为100 ℃.Figure 5. The effects of the volume of formic acid and reaction time on the the yield and the conversion rate![]()
图 6 催化剂的循环使用次数对收率和转化率的影响注：采用30 mL水、30 mL PEG-TiO2溶胶、40 mL甲酸、2 g葡萄糖，在100 ℃下反应6 h.Figure 6. The influence of catalyst cycle times on the yield and the conversion rate催化剂的循环使用可以有效降低工业生产的成本，同时减少催化剂对环境的污染. 但这需要催化剂有较强的稳定性，在多次使用后仍有较强的催化活性. PEG-TiO2溶胶的循环使用实验，以水作为反应溶剂，与甲酸协同催化，在100 ℃下反应6 h，将葡萄糖转化为HMF. PEG-TiO2溶胶采用过滤法回收，然后经3次水洗后分散在水中，即活化完成. 结果表明：PEG-TiO2溶胶在循环1次后，HMF收率由44.43%降低到18.07%，催化效果降低了50%(图 5). 这是因为腐殖质沉积在催化剂表面，使其催化效果降低，而且由于腐殖质的沉积，反应之后PEG-TiO2的颜色由白色变为黑色. 值得注意的是，PEG-TiO2溶胶在第1次使用时，对HMF的选择性为57.46%，在循环1、2、3、4次后，对HMF的选择性分别为56.66%、58.43%、63.37%、45.51%. 催化剂的循环使用过程中保持着对葡萄糖转化为HMF的较高的选择性.
3. 结论
以更低成本、更高效的方法制备并研究HMF，希望实现HMF的大规模工业化生产，缓解能源危机. 纳米TiO2被广泛用作非均相催化剂，但纳米TiO2溶胶作为均相催化剂的研究尚少. 纳米TiO2溶胶作为均相催化剂可以避免纳米粒子团聚，可以提供更多的Lewis酸位点，表面效应更显著. 本研究制备了纳米TiO2溶胶、纳米TiO2粉体、PEG-TiO2溶胶等催化剂，催化葡萄糖转化为HMF；相比纳米TiO2粉体，纳米TiO2溶胶的催化效果大大提高. 同样是以水作为反应溶剂，纳米TiO2粉体催化葡萄糖转化为HMF的收率为1.41%，而纳米TiO2溶胶和PEG-TiO2溶胶催化葡萄糖转化为HMF的收率分别为28.58%和17.70%. 在最佳条件下，以PEG-TiO2溶胶作为催化剂，HMF的收率可以达到56.20%，葡萄糖转化率达92.00%，反应在水溶液中进行，添加适量的甲酸协同催化剂，在100 ℃下反应12 h. 因此，以纳米TiO2溶胶作为催化剂，可以在不添加有机溶剂以及在较低的反应温度下，获得较高的HMF收率，大大降低了HMF的制备成本. 研究结果为HMF的大规模工业化生产提供了可行方法和技术指导.
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图 1 我国畜牧养殖业碳排放的时序变化
Figure 1. The temporal change of carbon emission from animal husbandry in China
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