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clearfix"><p>摘要：甲醇合成催化劑失活是導(dǎo)致甲醇合成裝置停車的重要因素之一，嚴(yán)重影響生產(chǎn)企業(yè)的經(jīng)濟效益。對來自兩種甲醇工廠的催化劑樣品進(jìn)行了表征分析，包括X射線熒光光譜、X射線衍射、紅外光譜、物理吸附和電感耦合等離子體發(fā)射光譜等，以探究其失活原因。結(jié)果表明，經(jīng)過約兩年工業(yè)使用，催化劑出現(xiàn)了徑向強度減小、粉化、銅晶粒尺寸增大、比表面積下降和有害雜質(zhì)元素（硫和鐵）富集的現(xiàn)象。失活催化劑中銅晶粒尺寸最高可達(dá)32.72 nm，相應(yīng)的比表面積由102.3 m<sup>2</sup> /g下降到最低的16.0 m<sup>2</sup> /g，硫和鐵元素含量（質(zhì)量分?jǐn)?shù)）由小于0.05%和362 × 10<sup>-6</sup>分別增加至最高0.36%和2629 × 10<sup>-6</sup>。兩個工廠采集的催化劑表現(xiàn)出不同的失活特征，需要采取有針對性的措施延長催化劑使用壽命。</p><p>關(guān)鍵詞：甲醇；催化劑；失活；銅晶粒；中毒</p><p> 煤炭是一種重要的化石資源，為我國經(jīng)濟發(fā)展作出了巨大貢獻(xiàn)。社會對生態(tài)環(huán)境日益重視，隨著碳達(dá)峰、碳中和目標(biāo)的提出，對煤化工產(chǎn)業(yè)的發(fā)展形成了挑戰(zhàn)。甲醇合成是煤炭清潔高效利用的重要組成部分，也是促進(jìn)煤化工產(chǎn)業(yè)高端化、多元化和低碳化發(fā)展的路徑之一。工業(yè)上合成甲醇，一般以合成氣為原料，采用固定床反應(yīng)裝置，以Cu/ZnO/Al<sub>2</sub>O<sub>3</sub>作催化劑，在220~300 ℃和5~10 MPa 的條件下進(jìn)行，其中催化劑是甲醇合成的核心技術(shù)之一。銅基甲醇合成催化劑活性好、選擇性高，隨著反應(yīng)裝置的長期運行，其催化性能會逐步降低。為保證生產(chǎn)，甲醇合成單元一般2~3年停車更換一次催化劑。在計劃生產(chǎn)期間，如果催化劑能長時間保持較高的耐熱活性和選擇性，會給生產(chǎn)單位帶來持續(xù)的甲醇產(chǎn)量和經(jīng)濟效益；反之，則會使生產(chǎn)單位受到較大的經(jīng)濟損失。</p><p> 銅基甲醇合成催化劑在使用過程中存在燒結(jié)、中毒、積炭，以及物理破壞催化劑結(jié)構(gòu)等問題，從而失去活性。研究發(fā)現(xiàn)，相比其他金屬催化劑，銅基催化劑銅晶粒更容易燒結(jié)長大。催化劑床層溫度波動過大，操作溫度過高，會導(dǎo)致銅晶粒受熱燒結(jié)；反應(yīng)環(huán)境中CO<sub>2</sub>含量過高，導(dǎo)致水分壓升高，會使銅晶粒出現(xiàn)水熱燒結(jié)的現(xiàn)象。燒結(jié)導(dǎo)致催化劑銅的比表面積降低，以及一些特定活性位的消失，催化劑逐漸失活。喻健等認(rèn)為單質(zhì)銅燒結(jié)主要通過CuCO發(fā)生，推測通過Ostwald熟化完成。抑制燒結(jié)失活，一方面可以通過改善催化劑制備方法提高催化劑的穩(wěn)定性，另一方面可以通過優(yōu)化合成工藝條件（如氣體組成、溫度等）提供適宜的反應(yīng)環(huán)境。</p><p> 引起催化劑中毒的元素有硫、氯、鐵和鎳等。硫元素在原料氣中一般以H<sub>2</sub>S和COS的形式存在，這些形式的硫易與單質(zhì)銅反應(yīng)生成Cu<sub>2</sub>S，覆蓋活性中心，導(dǎo)致催化劑快速失活。氯元素一般由催化劑生產(chǎn)原料和工廠工藝蒸汽帶入，反應(yīng)過程中易與催化劑中的鋅元素結(jié)合生成低熔點的氯化鋅，削弱氧化鋅的“隔離體”作用，加速銅晶粒的燒結(jié)。氯元素毒性較強，但與硫中毒相比，氯中毒比較少見。鐵和鎳元素由原料氣中的CO腐蝕管道，形成Fe(CO)<sub>5</sub>和Ni(CO)<sub>4</sub>帶入催化劑床層，受熱分解后形成高分散的單質(zhì)鐵和鎳，吸附在催化劑表面堵塞孔道，同時催化甲烷、石蠟和高碳醇等副產(chǎn)物的生成，降低了催化劑的目標(biāo)產(chǎn)物選擇性。原料氣中的有害雜質(zhì)可以通過使用保護(hù)劑脫除，控制其含量在規(guī)定的范圍內(nèi)。</p><p> 在氫碳比較低的條件下，甲醇合成反應(yīng)易發(fā)生還原析碳和歧化析碳兩種副反應(yīng)，產(chǎn)生的積炭覆蓋催化劑表面活性位，造成催化劑性能下降以及催化劑床層阻力上升，在空速較大的合成條件下，積炭影響一般不明顯。物理破壞催化劑結(jié)構(gòu)一般出現(xiàn)在搬運和裝卸過程中，催化劑墜落或受擠壓而破碎，產(chǎn)生的粉末被反應(yīng)氣帶出催化劑床層。在裝填進(jìn)合成塔之前，對催化劑進(jìn)行過篩，裝填過程中合理操作，避免踩踏，可以減輕和避免催化劑結(jié)構(gòu)物理破壞。</p><p> 導(dǎo)致甲醇合成催化劑失活的因素較多，不同工業(yè)生產(chǎn)裝置使用催化劑的失活原因是否相同，是否因采用的催化劑和合成工藝不同而有差異，尚未見到詳細(xì)報道。本研究采集兩種工業(yè)甲醇合成裝置中卸出的催化劑，采用多種表征手段分析其質(zhì)構(gòu)變化和失活原因，以期為延長工業(yè)甲醇合成催化劑使用壽命提供參考。</p><p><strong>1 實驗部分</strong></p><p><strong>1.1</strong> 催化劑樣品</p><p> 本研究對取自不同甲醇廠的兩種工業(yè)甲醇合成催化劑進(jìn)行測試分析，將A甲醇廠取得的催化劑樣品標(biāo)記為催化劑A，將B甲醇廠取得的催化劑樣品標(biāo)記</p><p> 為催化劑B。新鮮的催化劑A樣品外觀為兩端凸起的黑色圓柱體，外形尺寸（直徑 × 高）約為0.6 cm × 0.4cm，比表面積為123 m<sup>3</sup> /g，主要由銅、鋅和鋁等的金屬氧化物和少量石墨組成，催化劑徑向抗壓碎力為304 N/cm。新鮮的催化劑B樣品外觀也為兩端凸起的黑色圓柱體，外形尺寸約為0.50 cm × 0.45 cm，比表面積為102.3 m<sup>3</sup> /g，也主要由銅、鋅和鋁等的金屬氧化物組成，含有少量的石墨，催化劑徑向抗壓碎力為340 N/cm。采用與本研究相同方法得到的新鮮甲醇合成催化劑，銅晶粒尺寸為5~8 nm，硫和鐵元素含量（質(zhì)量分?jǐn)?shù)，下同）要求控制在0.05%以下。</p><p> 失活的催化劑A樣品A-01和A-02分別取自甲醇合成單元水冷塔的上下床層，A-03 和 A-04分別取自同一甲醇合成單元氣冷塔的上下床層，催化劑運行約17271 h。失活的催化劑B樣品B-01和B-02分別取自甲醇合成單元水冷塔的上下床層，催化劑運行約16560 h。上述測試樣品，具體取樣位置見圖1。為了安全地卸出失活催化劑，提前使用微量O<sub>2</sub>對還原態(tài)的催化劑進(jìn)行了鈍化處理。取得的失活催化劑樣品見圖2，可見樣品存在較多粉化現(xiàn)象。催化劑A的樣品表面較多地呈現(xiàn)出黑棕色，在破裂的截面處可以觀察到紅棕色。催化劑B的樣品主要表現(xiàn)為紅棕色，結(jié)合本研究X射線衍射分析的分析結(jié)果，推測是單質(zhì)銅的顏色。</p><p><img class="fr-dib" src="http://v1.cdn-static.cn/2024/6/20/_lxmiafwu_2.png?imageView2/2/w/1800" style="width: 381px;"></p><p><img class="fr-dib" src="http://v1.cdn-static.cn/2024/6/20/_lxmiblmp_2.png?imageView2/2/w/1800" style="width: 343px;"><br></p><p><strong>1.2</strong> 催化劑表征</p><p> 催化劑徑向強度測試采用顆?？箟簭姸葴y定儀（DLⅢ型，大連鵬輝科技公司），按照國標(biāo)HG/T 2782—2011 的方法，每種樣品均采用四分法隨機選取25顆進(jìn)行測試，對測試結(jié)果取平均值獲得該條件下樣品的徑向強度。</p><p> 催化劑含粉率測定方法為：采用10目的金屬篩，將100 g樣品分3次手動預(yù)篩1~5 min，對篩下物進(jìn)行收集稱重，計算3次篩下物的總重量占樣品總重量的百分?jǐn)?shù)，即為含粉率。</p><p> X-射線熒光光譜（XRF）分析采用 X-射線熒光光譜儀（S8 TIGER型，德國Bruker公司），采用半定量全掃描方法分析樣品，樣品于90 ℃烘干8 h，磨好</p><p>的樣品摻入硼酸壓片，將制好的樣片放入樣品杯，在真空條件下測試。</p><p> X 射線衍射（XRD）分析采用X射線衍射系統(tǒng)（D8型，德國Bruker公司），在40 kV、40 mA的條件下，采用Cu K<em>α</em>射線（<em>λ</em> =15.406 nm）對樣品粉末進(jìn)行</p><p>測試。</p><p> 比表面積測定采用表面分析儀（BEL sorp-max型，日本MicrotracBEL公司），測定前樣品在 120 ℃下預(yù)處理 12 h。比表面積采用 Brunauer-Emmett Teller（BET）公式進(jìn)行計算，采用Barrett-JoynerHalenda（BJH）模型計算孔徑分布。</p><p> 煤中全硫測定采用高頻紅外碳硫分析儀（JS-HW2000B 型，南京金石分析儀器廠），方法采用紅外光譜法（GB/T 25214—2010）。</p><p> 催化劑微量鐵元素分析采用電感耦合等離子體發(fā)射光譜儀（ iCAP 7200 ICP-OES 型，美國Thermo Fisher Scientific公司），稱取0.100 g 的催化劑樣品于消解管中，依次加入8 mL硝酸置于消解器中加熱至近干，加入硝酸溶液定容至50 mL，依次編號并取其過濾液進(jìn)行測試。</p><p><strong>2 結(jié)果與討論</strong></p><p><strong>2.1</strong> 強度及含粉率分析</p><p> 催化劑的強度和含粉率與合成塔內(nèi)的壓降密切相關(guān)，催化劑粉化程度較高，會導(dǎo)致合成塔的壓降升高，進(jìn)而增加循環(huán)壓縮機負(fù)荷，降低甲醇收率，嚴(yán)重時還會導(dǎo)致合成裝置停車。失活催化劑樣品的徑向強度和含粉率測試結(jié)果見表1。與新鮮催化劑相比，失活催化劑的徑向強度均出現(xiàn)了大幅下降，這是因為新鮮催化劑在還原之后氧化銅變?yōu)閱钨|(zhì)銅，同時殘留的碳酸鹽以CO<sub>2</sub>的形式逸出，使催化劑結(jié)構(gòu)變得疏松，強度減弱。進(jìn)一步看出，催化劑A失活后的樣品徑向強度呈現(xiàn)上層低下層高的趨勢，催化劑B失活后的樣品徑向強度隨反應(yīng)管位置變化基本不變。催化劑A失活后的樣品粉化程度高于催化劑B的，也呈現(xiàn)出了反應(yīng)塔上層含粉率高，下層含粉率低的趨勢。除運輸、裝填過程中催化劑結(jié)構(gòu)遭受物理性破壞，在甲醇合成反應(yīng)過分劇烈的情況下，也會引起催化劑的破碎和粉化。在軸向床反應(yīng)塔中，合成反應(yīng)一般主要發(fā)生在上層，下層催化劑的利用率相對較低，這可以解釋催化劑呈現(xiàn)上層含粉率高、下層含粉率低的現(xiàn)象。不同的成型方法、裝填方式和合成工藝可能導(dǎo)致兩種催化劑呈現(xiàn)不同的含粉率。</p><p> <img class="fr-dib" src="http://v1.cdn-static.cn/2024/6/20/_lxmicaly_2.png?imageView2/2/w/1800" style="width: 411px;"></p><p><strong>2.2 XRF</strong>結(jié)果分析</p><p> 采用 X 射線熒光光譜分析了兩種甲醇合成催化劑的元素組成，結(jié)果見表2。由表2可知，兩種催化劑主要含銅、鋅和鋁元素，還含有鈉、硫和鐵等元素，含量較低。與新鮮催化劑相比，失活催化劑均出現(xiàn)了<em>n</em>(Cu):<em>n</em>(Zn)降低。催化劑中的銅、鋅元素以鈉米顆粒的形式均勻分布，出現(xiàn)單一銅或鋅元素流失的可能性較小。結(jié)合水冷塔內(nèi)樣品A-01、A-02中ZnO比例高于氣冷塔內(nèi)樣品A-03、A-04的，推測原料氣經(jīng)過前端脫硫罐后，夾帶少量ZnO粉塵進(jìn)入了催化劑床層，導(dǎo)致失活催化劑ZnO比例偏高。</p><p> <img class="fr-dib" src="http://v1.cdn-static.cn/2024/6/20/_lxmicxuh_2.png?imageView2/2/w/1800" style="width: 862px;"></p><p> 依據(jù)元素比例，可以發(fā)現(xiàn)兩種催化劑不同的設(shè)計理念。與催化劑A相比，催化劑B的銅元素比例較高，鋅和鋁元素相對較低。一般認(rèn)為，在甲醇合成催化劑中，Cu/ZnO是活性組分，甲醇合成反應(yīng)發(fā)生在 Cu和ZnO 的接觸界面處，ZnO 不僅是活性助劑，促進(jìn)了反應(yīng)的發(fā)生，同時還分布在單質(zhì)銅晶粒周圍，抑制銅晶粒長大。因此，催化劑組成中，Cu和Zn元素比例的選擇對催化劑活性和穩(wěn)定性的影響較為顯著（圖3）。<img class="fr-dib" src="http://v1.cdn-static.cn/2024/6/20/_lxmidr8w_2.png?imageView2/2/w/1800" style="width: 339px;"></p><p> BEHRENS等研究了甲醇合成催化劑中的銅鋅比例，認(rèn)為合適的<em>n</em>(Cu):<em>n</em>(Zn)在70:30左右，銅鋅比例過高，活性組分Cu/ZnO的前驅(qū)體鋅孔雀石不能實現(xiàn)足夠多的同晶取代，銅鋅比例過低，在催化劑沉淀制備過程中會形成副產(chǎn)物綠銅鋅礦前驅(qū)體，導(dǎo)致催化劑性能下降。近年來，一些學(xué)者致力于開發(fā)新的催化劑合成技術(shù)，如低溫共沉淀和定向同晶取代等，以提高活性前驅(qū)體鋅孔雀石中鋅元素的含量，使之達(dá)到或突破銅鋅比例。由表2可知，催化劑A的<em>n</em>(Cu):<em>n</em>(Zn)約為70:30，催化劑B的<em>n</em>(Cu):<em>n</em>(Zn)約為76:24，后者可能會缺乏足夠多的ZnO 與銅晶粒產(chǎn)生協(xié)同效應(yīng)，減少了催化劑活性位，反應(yīng)過程中單質(zhì)銅晶粒易于長大。</p><p> <strong>2.3 XRD</strong>結(jié)果分析</p><p> 采用X射線衍射對失活催化劑樣品進(jìn)行了檢測分析，對比了物相變化，結(jié)果見圖4。由圖4可以觀察到明顯的Cu 和ZnO 的特征衍射峰，表明失活催化劑中主要存在Cu和ZnO的物相，Al<sub>2</sub>O<sub>3</sub>可能由于含量相對較少，同時多處于無定形態(tài)，未被檢出。盡管進(jìn)行了鈍化處理，樣品內(nèi)的銅元素仍主要以單質(zhì)銅的形式存在，這可能是因為高溫鈍化過程中，催化劑外表面的單質(zhì)銅先與氧氣接觸，反應(yīng)形成一層氧化銅薄膜，抑制了氧氣進(jìn)入催化劑結(jié)構(gòu)內(nèi)部。以單質(zhì)銅（2<em>θ</em> = 43.341°）處的特征衍射峰為基準(zhǔn)，采用Scherrer方程，對銅晶粒的大小進(jìn)行了計算，結(jié)果見表3。對比樣品A-01、A-02和A-03、A-04，A-03、A-04的銅晶粒尺寸略高，這可能是因為氣冷塔的操作溫度略高于水冷塔的，加快了氣冷塔內(nèi)催化劑中銅晶粒的生長。對比樣品B-01和B-02可以發(fā)現(xiàn)，合成塔上層樣品的銅晶粒尺寸略低于合成塔下層樣品的，這可能是因為合成塔內(nèi)的溫度分布不太均勻。由于甲醇合成是放熱反應(yīng)，沿著催化劑床層從上到下溫度逐步升高，使得合成塔出口處的氣體溫度高于合成塔入口處的氣體溫度。對比催化劑A和催化劑B的失活樣品，可以發(fā)現(xiàn)，催化劑B的失活樣品中銅晶粒尺寸（≈ 30 nm）要高于催化劑A的失活樣品（≈ 15 nm）。一方面，這與甲醇合成工藝有關(guān)，操作溫度過高，反應(yīng)環(huán)境中CO2含量過高，均會促使銅晶粒燒結(jié)長大。另一方面，銅晶粒尺寸的變化也可能與催化劑的設(shè)計有關(guān)。見XRF結(jié)果分析，催化劑 B 的 <em>n</em>(Cu):<em>n</em>(Zn)略高，銅元素沒有足夠的ZnO作為間隔屏障，可能導(dǎo)致其銅晶粒的穩(wěn)定性略弱于催化劑A。</p><p> <img class="fr-dib" src="http://v1.cdn-static.cn/2024/6/20/_lxmien7s_2.png?imageView2/2/w/1800" style="width: 309px;"></p><p><strong>2.4</strong> 織構(gòu)參數(shù)分析</p><p> 對于非均相反應(yīng)，催化劑的比表面積與催化活性有著密切關(guān)系，本研究測得兩種催化劑樣品的織構(gòu)參數(shù)見表3。由表3可知，失活催化劑樣品的比表面積和孔體積出現(xiàn)了不同程度的下降。催化劑A的比表面積從使用前的 123.3 m<sup>2</sup> /g 下降至最低的34.3 m<sup>2</sup> /g，相應(yīng)的孔體積也出現(xiàn)明顯下降。同時，可以發(fā)現(xiàn)從氣冷塔取出的失活催化劑A-03、A-04比表面積要低于從水冷塔取出的失活催化劑A-01、A-02，這可能是因為氣冷塔的操作溫度高于水冷塔的，對催化劑的孔結(jié)構(gòu)影響更大。失活催化劑 B 的比表面積下降幅度更大，從102.3 m<sup>2</sup> /g下降至最低的16.0 m<sup>2</sup> /g。綜合對比催化劑A和催化劑B，下降幅度從大到小為B-01/B-02、A-03/A-04、A-01/A-02。比表面積的下降一方面與引入雜質(zhì)堵塞孔道有關(guān)，另一方面也與催化劑自身的物相變化有關(guān)。</p><p> 催化劑比表面積與銅晶粒尺寸的關(guān)系見圖5。由圖5可知，比表面積與銅晶粒尺寸存在較強的相關(guān)性，當(dāng)銅晶粒尺寸較大時，失活催化劑的比表面積相對較小。這一關(guān)系與其他學(xué)者的研究結(jié)果相似，可以推測銅晶粒長大對催化劑的微觀孔結(jié)構(gòu)有著較強的破壞作用。這可以解釋不同失活催化劑比表面積出現(xiàn)不同幅度下降的現(xiàn)象。樣品A-01的比表面積低于A-02，原因可能是因為其處于水冷塔上層，受雜質(zhì)堵塞孔道的影響較大。如XRF結(jié)果分析，ZnO 粉塵的帶入也可能導(dǎo)致催化劑孔道堵塞。</p><p><img class="fr-dib" src="http://v1.cdn-static.cn/2024/6/20/_lxmifkhd_2.png?imageView2/2/w/1800" style="width: 404px;"><img class="fr-dib" src="http://v1.cdn-static.cn/2024/6/20/_lxmify52_2.png?imageView2/2/w/1800" style="width: 372px;"><br></p><p><strong>2.5</strong> 硫及微量金屬元素含量分析</p><p> 除催化劑本身的物相結(jié)構(gòu)變化外，外來雜質(zhì)的引入也會造成銅基甲醇合成催化劑的失活，其中以硫和鐵等元素的影響最為引人關(guān)注。硫元素以H<sub>2</sub>S、COS、CS<sub>2</sub>和硫醚等形式存在于原料氣中，與催化劑中的單質(zhì)銅接觸后容易發(fā)生反應(yīng)生成硫化亞銅，使其失去催化活性。造氣過程或原料氣中的CO侵蝕設(shè)備和管道產(chǎn)生Fe(CO)<sub>5</sub>，使鐵元素被帶入到甲醇合成反應(yīng)器中。此外，裝劑前反應(yīng)器清掃不</p><p> 徹底或裝劑過程操作不規(guī)范也會引入鐵元素。鐵元素的引入一方面堵塞孔道，覆蓋活性位，造成催化劑活性下降，還會導(dǎo)致費托蠟和高碳醇等副產(chǎn)物的生成，降低合成反應(yīng)效率，堵塞設(shè)備管道，甚至導(dǎo)致裝置停車。</p><p> 催化劑樣品硫元素和微量金屬元素含量見表4。由表4可知，樣品A-01、A-02的硫含量顯著高于B-01、B-02，這可能是因為兩個甲醇廠的原料氣硫元素的凈化程度不同所致。A甲醇廠采用水冷塔和氣冷塔串聯(lián)的工藝，原料氣中的硫元素大部分被水冷塔內(nèi)的甲醇合成催化劑吸收，這可能是樣品A-03、A-04的硫含量低于 A-01、A-02 的原因。與硫元素的結(jié)果相似，樣品A-01、A-02的鐵元素含量要顯著高于B-01、B-02，樣品A-03、A-04的鐵含量要略低于A-01、 A-02。其他測得的金屬元素（如錳、鎂和鉛）含量低且沒有明顯的變化規(guī)律，可能是催化劑生產(chǎn)過程中引入的極微量雜質(zhì)?？傮w來看，B甲醇廠對硫和鐵元素的控制要略優(yōu)于A甲醇廠。有文獻(xiàn)報道，當(dāng)催化劑上硫元素質(zhì)量分?jǐn)?shù)為0.21%~0.29%時，合成甲醇的總碳轉(zhuǎn)化率下降約 19%，甲醇選擇性下降約13.5%；當(dāng)鐵元素質(zhì)量分?jǐn)?shù)為0.207%時，催化劑合成甲醇的總碳轉(zhuǎn)化率下降約17.5%，甲醇選擇性下降約29.2%。硫和鐵元素的富集可能是催化劑A失活的重要原因之一。</p><p> <img class="fr-dib" src="http://v1.cdn-static.cn/2024/6/20/_lxmigoh4_2.png?imageView2/2/w/1800" style="width: 384px;"></p><p><strong>3 結(jié)論</strong></p><p> 對兩種來自不同甲醇廠的失活甲醇合成催化劑進(jìn)行了表征分析，包括強度、含粉率、元素組成、物相構(gòu)成、孔結(jié)構(gòu)和雜質(zhì)元素，探究了導(dǎo)致催化劑失活的原因，得到如下主要結(jié)論。</p><p> （1）軸向床合成塔中的失活催化劑上床層含粉率高、下床層含粉率低；銅晶粒尺寸與催化劑所在床層的操作溫度密切相關(guān)，溫度越高，銅晶粒尺寸相對越大；失活催化劑的比表面積與銅晶粒尺寸具有較強的相關(guān)性，銅晶粒尺寸大，則比表面積低。</p><p> （2）催化劑 A 表現(xiàn)出相對較高的穩(wěn)定性，長周期運轉(zhuǎn)之后，銅晶粒尺寸仍控制在15 nm左右；但在使用過程中富集了較高含量的硫和鐵元素，硫元素質(zhì)量分?jǐn)?shù)由小于 0.05% 上升至最高的 0.36%，鐵元素由362 × 10<sup>-6</sup>上升至最高的2629 × 10<sup>-6</sup>，對甲醇生產(chǎn)帶來不利影響。</p><p> （3）催化劑B配套的合成工藝對雜質(zhì)元素實現(xiàn)了有效控制，但在生產(chǎn)過程中，銅晶粒尺寸增長明顯并引發(fā)了比表面積的大幅度下降，銅晶粒尺寸增至最高的32.72 nm，比表面積下降至最低的16.0 m<sup>2</sup> /g，催化劑失活。</p><p> 兩套甲醇合成裝置采集的失活催化劑表現(xiàn)出不同的失活特征。對于A甲醇廠，需要加強原料氣凈化，將原料氣中的雜質(zhì)含量控制在較低水平；對于B甲醇廠，一方面需要選擇高穩(wěn)定性的甲醇合成催化劑，另一方面需要優(yōu)化合成工藝操作條件，如選擇合適的氣體組成和操作溫度。對甲醇合成催化劑進(jìn)行失活原因分析，有助于甲醇生產(chǎn)單位采取針對性的措施延長催化劑的使用壽命，實現(xiàn)甲醇合成裝置的長期穩(wěn)定運行。</p></div><div id="yu4k4o2qm" 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