2月10日，一項石(shi)(shi)油煉化(hua)(hua)(hua)領域的重要成果(guo)在(zai)北(bei)京(jing)首次公開(kai)——由(you)石(shi)(shi)油化(hua)(hua)(hua)工(gong)科學研究院牽頭完成的“硫化(hua)(hua)(hua)反應環境精準控(kong)制的加氫催(cui)化(hua)(hua)(hua)劑真硫化(hua)(hua)(hua)技術開(kai)發及應用”項目順(shun)利通過中國石(shi)(shi)油和化(hua)(hua)(hua)學工(gong)業聯合會組織(zhi)的科技成果(guo)鑒定。

        由中國工(gong)程(cheng)院院士曹湘洪，中國科(ke)學(xue)院院士段雪(xue)、張濤、徐春明，以及(ji)來(lai)自中國石(shi)油、中國石(shi)化(hua)(hua)企(qi)業界的煉油專家(jia)(jia)和(he)各(ge)大高(gao)校的學(xue)者(zhe)組成的鑒(jian)定(ding)委員會(hui)，中國石(shi)油和(he)化(hua)(hua)學(xue)工(gong)業聯合會(hui)科(ke)技項目(mu)處處長(chang)趙明、項目(mu)主管邢(xing)雪(xue)健(jian)，石(shi)科(ke)院院長(chang)李(li)明豐、研究(jiu)室主任劉鋒以及(ji)來(lai)自參研單位的業內專家(jia)(jia)代表參加(jia)了(le)鑒(jian)定(ding)會(hui)。鑒(jian)定(ding)委員會(hui)一(yi)致認定(ding)：加(jia)氫(qing)催化(hua)(hua)劑器外真(zhen)硫化(hua)(hua)反應器屬國際首創，成果整體達到國際領先水平，將為我國石(shi)化(hua)(hua)行(xing)業的高(gao)質量發展提供強有力的技術支撐。

又一(yi)(yi)項技術(shu)瓶頸被國內科研團隊(dui)突破，曾(ceng)經困擾行業的“老大難”問題如今正(zheng)逐一(yi)(yi)被破解(jie)。

行業矚目的硫化處理難題

        加氫(qing)(qing)技術是提升油(you)品質量(liang)的關(guan)鍵手段，而加氫(qing)(qing)催化(hua)劑的性(xing)能直接(jie)影響加氫(qing)(qing)效(xiao)果。長期(qi)以來，含Co、Mo、Ni、W金屬的硫化(hua)物是煉油(you)加氫(qing)(qing)催化(hua)劑的主要(yao)活性(xing)物質，加氫(qing)(qing)催化(hua)劑在制備過(guo)程(cheng)中(zhong)影響其性(xing)能發(fa)揮的關(guan)鍵之一(yi)在于金屬氧(yang)化(hua)物向金屬硫化(hua)物轉變生成(cheng)活性(xing)相的過(guo)程(cheng)。因此，硫化(hua)反應過(guo)程(cheng)的研究(jiu)及控制是目前國(guo)內外關(guan)注的熱(re)點。

       現(xian)階段，加氫(qing)催化(hua)劑的(de)硫化(hua)主(zhu)要在加氫(qing)反應器內(nei)完成(cheng)，不(bu)僅占用(yong)了(le)加氫(qing)裝置的(de)開工時間，給現(xian)場硫化(hua)帶來安(an)全環保問題(ti)，器內(nei)硫化(hua)還會受到現(xian)場條件限制無法實現(xian)活性相的(de)可(ke)控合成(cheng)，進而影響催化(hua)劑的(de)加氫(qing)活性。

     石油化(hua)(hua)(hua)工科(ke)學(xue)研究(jiu)院加(jia)(jia)氫催(cui)(cui)(cui)化(hua)(hua)(hua)劑研究(jiu)室副(fu)主任劉鋒表示，要實(shi)現對(dui)加(jia)(jia)氫催(cui)(cui)(cui)化(hua)(hua)(hua)劑硫化(hua)(hua)(hua)反應過(guo)程(cheng)的(de)精(jing)準控(kong)制，目(mu)前主要有三大技(ji)術難(nan)題：一是(shi)(shi)對(dui)硫化(hua)(hua)(hua)過(guo)程(cheng)及活(huo)性(xing)(xing)金(jin)屬硫化(hua)(hua)(hua)行為的(de)系統性(xing)(xing)認識不(bu)(bu)(bu)足，導(dao)致硫化(hua)(hua)(hua)過(guo)程(cheng)活(huo)性(xing)(xing)相(xiang)結(jie)構的(de)不(bu)(bu)(bu)可(ke)(ke)控(kong)生長；二是(shi)(shi)不(bu)(bu)(bu)同的(de)加(jia)(jia)氫反應場景(jing)需要具有特(te)定活(huo)性(xing)(xing)相(xiang)結(jie)構的(de)催(cui)(cui)(cui)化(hua)(hua)(hua)劑，而(er)現有的(de)硫化(hua)(hua)(hua)技(ji)術不(bu)(bu)(bu)具備(bei)實(shi)現可(ke)(ke)控(kong)合成目(mu)標活(huo)性(xing)(xing)相(xiang)結(jie)構的(de)全部條件，并(bing)且(qie)采用(yong)的(de)硫化(hua)(hua)(hua)設備(bei)無法實(shi)現溫度(du)和(he)(he)氣氛濃度(du)等(deng)工藝參數的(de)精(jing)準控(kong)制，導(dao)致硫化(hua)(hua)(hua)效率和(he)(he)產(chan)品質(zhi)量低等(deng)問題；三是(shi)(shi)硫化(hua)(hua)(hua)態(tai)催(cui)(cui)(cui)化(hua)(hua)(hua)劑在空氣中易自熱(re)，給包裝(zhuang)、運輸、存儲和(he)(he)裝(zhuang)填帶來安全隱(yin)患。

      在(zai)此背景下，器外真硫(liu)化(hua)(hua)技術應運而生。這(zhe)是一種在(zai)催化(hua)(hua)劑(ji)生產時(shi)，將(jiang)氧化(hua)(hua)態(tai)(tai)催化(hua)(hua)劑(ji)加工為真硫(liu)化(hua)(hua)態(tai)(tai)催化(hua)(hua)劑(ji)的技術。煉化(hua)(hua)企業(ye)采購真硫(liu)化(hua)(hua)態(tai)(tai)催化(hua)(hua)劑(ji)后便可直接使用開(kai)工，無需再硫(liu)化(hua)(hua)處理，經濟效(xiao)益(yi)和社會效(xiao)益(yi)相較于傳統技術都(dou)具有顯著優勢。

讓反應精準控制成為可能

        然(ran)而瓶頸突破的(de)背后，是一場需要研(yan)究團隊跋涉于多個(ge)省市之(zhi)間、攻關十余(yu)年的(de)持久(jiu)戰。

地處北京(jing)的石(shi)(shi)科院聯合淄(zi)博市臨淄(zi)恒興化(hua)(hua)(hua)工(gong)(gong)(gong)廠有(you)(you)限(xian)(xian)公(gong)(gong)(gong)(gong)司(si)(si)(si)、中(zhong)國(guo)石(shi)(shi)油化(hua)(hua)(hua)工(gong)(gong)(gong)股份(fen)有(you)(you)限(xian)(xian)公(gong)(gong)(gong)(gong)司(si)(si)(si)安慶分公(gong)(gong)(gong)(gong)司(si)(si)(si)、中(zhong)國(guo)石(shi)(shi)油化(hua)(hua)(hua)工(gong)(gong)(gong)股份(fen)有(you)(you)限(xian)(xian)公(gong)(gong)(gong)(gong)司(si)(si)(si)齊魯分公(gong)(gong)(gong)(gong)司(si)(si)(si)、中(zhong)國(guo)石(shi)(shi)化(hua)(hua)(hua)青(qing)島煉(lian)油化(hua)(hua)(hua)工(gong)(gong)(gong)有(you)(you)限(xian)(xian)責任公(gong)(gong)(gong)(gong)司(si)(si)(si)、中(zhong)國(guo)石(shi)(shi)油化(hua)(hua)(hua)工(gong)(gong)(gong)股份(fen)有(you)(you)限(xian)(xian)公(gong)(gong)(gong)(gong)司(si)(si)(si)滄(cang)州(zhou)分公(gong)(gong)(gong)(gong)司(si)(si)(si)、中(zhong)國(guo)石(shi)(shi)油天(tian)然氣股份(fen)有(you)(you)限(xian)(xian)公(gong)(gong)(gong)(gong)司(si)(si)(si)哈爾(er)濱石(shi)(shi)化(hua)(hua)(hua)分公(gong)(gong)(gong)(gong)司(si)(si)(si)、中(zhong)國(guo)科學院過(guo)程工(gong)(gong)(gong)程研究(jiu)所、中(zhong)國(guo)石(shi)(shi)化(hua)(hua)(hua)催化(hua)(hua)(hua)劑有(you)(you)限(xian)(xian)公(gong)(gong)(gong)(gong)司(si)(si)(si)等(deng)9家單(dan)位聯手合作，發明(ming)出了新型(xing)硫化(hua)(hua)(hua)反應器系統，并把它從(cong)實驗室帶到生產一線。

        劉鋒介(jie)紹說，項目聚(ju)焦加氫(qing)(qing)(qing)催(cui)化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)劑(ji)硫(liu)(liu)(liu)化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)反應過程精準(zhun)控制(zhi)(zhi)(zhi)難(nan)點，逐一(yi)突破。在(zai)基礎研(yan)(yan)究方(fang)面(mian)，團(tuan)隊揭(jie)示了(le)(le)(le)(le)加氫(qing)(qing)(qing)催(cui)化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)劑(ji)活性(xing)金(jin)屬(shu)(shu)硫(liu)(liu)(liu)化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)行(xing)為的演(yan)變(bian)規律，闡明了(le)(le)(le)(le)不(bu)同(tong)金(jin)屬(shu)(shu)間(jian)的協(xie)(xie)同(tong)硫(liu)(liu)(liu)化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)機制(zhi)(zhi)(zhi)，發(fa)現了(le)(le)(le)(le)硫(liu)(liu)(liu)化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)助劑(ji)對(dui)硫(liu)(liu)(liu)化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)行(xing)為的調節作用，提出了(le)(le)(le)(le)可控調節活性(xing)金(jin)屬(shu)(shu)協(xie)(xie)同(tong)硫(liu)(liu)(liu)化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)的創(chuang)新策略，取得了(le)(le)(le)(le)加氫(qing)(qing)(qing)催(cui)化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)劑(ji)真硫(liu)(liu)(liu)化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)基礎研(yan)(yan)究的新認識。在(zai)反應控制(zhi)(zhi)(zhi)方(fang)面(mian)，團(tuan)隊研(yan)(yan)制(zhi)(zhi)(zhi)了(le)(le)(le)(le)新型硫(liu)(liu)(liu)化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)反應器系(xi)統，實現了(le)(le)(le)(le)硫(liu)(liu)(liu)化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)條(tiao)(tiao)件的靈活精準(zhun)控制(zhi)(zhi)(zhi)以及硫(liu)(liu)(liu)化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)溫度、硫(liu)(liu)(liu)化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)氣氛的均勻和物料分布的均勻；針對(dui)硫(liu)(liu)(liu)化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)氫(qing)(qing)(qing)介(jie)質(zhi)反應器開發(fa)的密封結構(gou)，確(que)保了(le)(le)(le)(le)在(zai)高濃度硫(liu)(liu)(liu)化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)氫(qing)(qing)(qing)介(jie)質(zhi)條(tiao)(tiao)件下的安全(quan)生產(chan)；針對(dui)多(duo)金(jin)屬(shu)(shu)硫(liu)(liu)(liu)化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)行(xing)為及各類(lei)氧化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)態(tai)催(cui)化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)劑(ji)物化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)性(xing)質(zhi)的差(cha)異，開發(fa)了(le)(le)(le)(le)基于硫(liu)(liu)(liu)化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)反應環(huan)境精準(zhun)匹配的多(duo)金(jin)屬(shu)(shu)協(xie)(xie)同(tong)硫(liu)(liu)(liu)化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)的器外真硫(liu)(liu)(liu)化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)技術，實現了(le)(le)(le)(le)各類(lei)型催(cui)化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)劑(ji)活性(xing)相結構(gou)的可控合(he)成，提升(sheng)了(le)(le)(le)(le)催(cui)化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)劑(ji)性(xing)能(neng)。值(zhi)得一(yi)提的是，研(yan)(yan)發(fa)團(tuan)隊首創(chuang)了(le)(le)(le)(le)硫(liu)(liu)(liu)化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)態(tai)催(cui)化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)劑(ji)表面(mian)鈍化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)技術，使硫(liu)(liu)(liu)化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)態(tai)催(cui)化(hua)(hua)(hua)(hua)(hua)(hua)(hua)(hua)劑(ji)在(zai)空氣環(huan)境中能(neng)夠安全(quan)包裝、運輸、存(cun)儲和裝填。

      通過對設備(bei)、工藝(yi)及安(an)全(quan)技(ji)術等方面的創新，團隊成功構(gou)建起了(le)硫化(hua)反應環境精準控制的加(jia)氫催(cui)化(hua)劑器(qi)外(wai)真硫化(hua)技(ji)術平臺，技(ji)術水平國際領先。

經濟社會效益顯著提升

        據了解，在攻關階段，淄(zi)博市臨淄(zi)恒(heng)興化工(gong)廠(chang)有限公司(si)就(jiu)率先采用(yong)石科院牽頭開發的加氫(qing)催化劑(ji)器(qi)外真硫化技術，投資建成的首套基于新型反(fan)應器(qi)的加氫(qing)催化劑(ji)器(qi)外真硫化工(gong)業生(sheng)產線，生(sheng)產效率較傳統固定床器(qi)外硫化技術提升(sheng)一倍以上。

      “器外真(zhen)硫(liu)化(hua)技術(shu)相較于傳統技術(shu)效益(yi)突出顯(xian)著，可以使(shi)加氫(qing)裝置(zhi)開工(gong)(gong)過程(cheng)(cheng)的(de)主要操作步驟減(jian)少40%以上，縮短開工(gong)(gong)時間，節(jie)省開工(gong)(gong)費用，讓煉化(hua)企(qi)業(ye)可實(shi)現(xian)(xian)早投產、早產出、早盈利。”石油化(hua)工(gong)(gong)科(ke)學研究院(yuan)加氫(qing)催化(hua)劑(ji)(ji)研究室副主任劉鋒表示，“而且這項技術(shu)更安全、更綠色。通過技術(shu)升級(ji)取消加氫(qing)催化(hua)劑(ji)(ji)硫(liu)化(hua)過程(cheng)(cheng)，開工(gong)(gong)過程(cheng)(cheng)不(bu)產生硫(liu)化(hua)氫(qing)，無(wu)需在開工(gong)(gong)階段采集和(he)分析高濃度硫(liu)化(hua)氫(qing)氣體，也無(wu)需采購(gou)、存(cun)儲和(he)使(shi)用硫(liu)化(hua)劑(ji)(ji)；也不(bu)產生酸性(xing)氣、酸性(xing)水和(he)硫(liu)化(hua)廢油，無(wu)需考慮后續排(pai)放問題，裝置(zhi)現(xian)(xian)場無(wu)臭味，從根本上去除了現(xian)(xian)有的(de)安全隱(yin)患。”

        目前(qian)，該技術生產的(de)真硫化(hua)態催(cui)化(hua)劑已在國內(nei)(nei)76套(tao)次加氫裝置中成(cheng)功應用(yong)，顯著簡(jian)化(hua)了(le)加氫裝置開工流程(cheng)，縮短開工時間2-5天，并消(xiao)除了(le)器內(nei)(nei)硫化(hua)過程(cheng)的(de)“三廢”排放問題，催(cui)化(hua)劑性(xing)能更優，且經濟效(xiao)益和社(she)會(hui)效(xiao)益顯著。該成(cheng)果已獲國家發明專利授權(quan)28件，發表論文24篇，形成(cheng)了(le)完整的(de)自(zi)主知識產權(quan)體(ti)系。