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    丁苯橡膠優級品率提升措施
    【摘 要】 丁苯橡膠產品分析項目較多,包括揮發份、門尼、混煉膠300%定伸應力等10項物性和產品外觀指標,影響這些指標的因素較多,為了保證產品質量合格,需要生產中工藝平穩控制,助劑配制加料準確,配方合理,并適時調整。本文就影響產品質量的因素進行分析、論述。
      【關鍵詞】 丁苯橡膠 質量 定伸應力
      撫順石化20萬噸/年丁苯橡膠裝置采用吉林石化公司低溫乳液聚合丁苯橡膠專有技術,于2012年建成投產。裝置開車后出現了諸多問題,突出表現在產品質量不穩定、用戶投訴多、優級品率低。丁苯橡膠車間與石油化工研究院蘭州化工研究中心就撫順石化丁苯橡膠裝置分析檢測人員對橡膠檢測認識深度有欠缺、分析測試標準執行不到位、裝置優級品率低、產品在市場推廣中存在的問題等開展全流程技術合作,全面提升了產品優級品率和市場認知度。
      1 產品質量存在的問題
      (1)裝置設計存在先天不足,開車遇到了很大挑戰,試車前期(2012年),產品力學指標不穩定,優級品率僅為30%。(2)丁苯橡膠產品2012年11月份投入市場后,主要銷售區域為華東、華北、華南下游企業,由于開車前期對質量控制認識不夠,出現了外包裝標識與實物不符、膠表面含水、含油、濕斑膠、花斑膠等一些問題。(3)產品力學性能不穩定,突出表現為批次間門尼波動大,市場反饋定伸高,扯斷伸長率低,混煉膠硬度高等問題。
      2 原因分析
      (1)設計先天不足;前部兩套氫氧化鈉潷淅器分配不均,真空泵和壓縮機系統油水分離不好,苯乙烯潷淅器分離不好,后處理凝聚槽和水洗槽存在攪拌器設計問題,影響凝聚效果,干燥箱布料器布料不均勻,影響成品膠揮發份等問題。www.zhidachem.com(2)原料丁二烯中阻聚劑tbc含量高;堿洗后tbc含量在10~30mg/kg,超過丁二烯優級品規格指標(tbc<10mg/kg)要求。(3)助劑配制存在問題;試生產初期,原設計乳化劑配制廠不能與裝置同步開車投用,前期生產由車間自己配制,釜小、批多、質量不穩,往往混合不均,對門尼粘度影響較大。(4)分析及檢測方面;計量器具檢定及對檢定結果的應用存在漏洞、部分操作規程不規范、標準執行不嚴格,造成分析誤差,誤導了實際操作。(5)反應調整不科學;轉化率及門尼粘度的調整主要通過調整聚合反應停留時間、調節活化相的用量以及運用置換塔進行調節。每條生產線有3臺置換塔,每個置換塔的停留時間10~12min,置換塔中膠乳溫度可達到10~13℃。膠乳在置換塔中停留時間雖然短,但溫度較高,產生支化和凝膠,影響產品的質量。(6)凝聚、干燥狀態不好;膠乳在凝聚槽內停留時間短,凝聚槽攪拌剪切力大,膠粒細碎,膠料在干燥箱內干燥效果不好,容易產生濕斑膠。
      3 控制措施及實施效果
      3.1 產品干燥特性分析
      裝置膠乳凝聚后細膠粒子多,容易堵塞設備,干燥效果不好,濕斑膠嚴重。針對此情況,產品干燥特性與蘭化橡樣進行對比,研究結果見圖1和圖2。
      從圖1數據可以看出,在70~100℃(高于100℃時,膠樣容易發生塑化現象),隨著溫度升高,干燥時間縮短,70℃、80℃、90℃和100℃下干燥時間分別為90分鐘、70分鐘、40分鐘和30分鐘,可見提高干燥溫度可以大幅度縮短干燥時間。
      圖2為膠樣水分比與時間的關系圖,水分比為測試點膠樣所含水分占膠樣總水分質量百分數。由數據可以看出,70~80℃時,60~70%的水分在干燥的前10分鐘失去,此區間為水分失去的主要區間; 90~100℃時,60%的水分在干燥的前15分鐘失去,此區間為水分失去的主要區間。
      上述研究結果表明干燥箱干燥特性正常,因此,細膠粒子多、干燥效果不好主要是凝聚設備和干燥箱布料不均勻等原因造成,需要對凝聚攪拌及干燥布料器進行改造。
      3.2 調節劑加入方式對sbr1500e產品性能的影響研究
      按照sbr1500e配方進行試驗,分別考察調節劑一點加入和調節劑兩點加入(首次加入70%,轉化率30%左右加入其余30%)方式對聚合反應過程和產品性能的影響。
      (1)對聚合反應過程的影響;調節劑加入方式對聚合反應動力學影響見圖3。
      從圖3中可以看出,調節劑加入方式對聚合反應動力學影響不大,達到相同轉化率的時間均在8~9小時。
      (2)對聚合物凝膠及門尼黏度的影響;調節劑加入方式對產品凝膠含量影響見表1。
      從表1中可以看出調節劑兩點加入方式所得產品的凝膠含

    稍低于一次加入方式,且所得門尼黏度較為穩定,調節劑一點加入所得門尼黏度波動大。這是因為調節劑一次加入,在反應前期就會逐漸被消耗,對于反應后期的門尼黏度得不到較好的調節作用,分兩次加入方式調節劑逐漸被消耗,得到的聚合物分子量均勻。
      (3)對sbr1500e性能的影響;調節劑加入方式對sbr1500e產品性能的影響見表2。
      從表2可見,調節劑兩點加入所得產品的性能較為穩定。
      3.3 300%定伸應力影響因素分析
      硫化促進劑am2(三烷基氯化銨)對300%定伸應力的影響;增加am2的用量,一定程度上對硫化橡膠的定伸應力有提高作用,從而保證橡膠的產品質量。在大生產中改變三烷基氯化銨加入量,定伸影響情況如表3。
      表3反應了不同am2加料量情況下產品定伸應力的變化情況,隨著am2加料量的增加300%定伸應力25min、35min、50min均有所增加,特別是25min定伸應力改變較大,改變0.01phr可提高1~2個mpa。
      從實際生產看,隨著am2加入量的提高,凝聚顆粒粒徑變小,加劇了系統堵掛狀況,干燥效果變差,am2加入量多,膠發粘。在生產中,找出am2加入的最佳值,確保硫化橡膠的25分定伸應力未受影響的前提下使凝聚效果得到改善,膠粒粒徑增大。
      4 結語
      (1)針對干燥箱干燥特性的研究,控制干燥溫度在85-95℃,可保證產品揮發份合格。(2)針對膠粒細碎的問題,對凝聚槽、轉化槽折流檔板進行改造,第二凝聚槽保留1/3高度,轉化槽增加導流板,凝聚槽進料管線由上進料改為側進料,可有效果解決膠料細碎的問題,產品灰分、揮發分合格,減少了濕斑膠的產生量。(3)針對干燥箱布料不均,容易產生濕斑膠的問題,對干燥箱進料端進行改造,增加振動布料器,原螺旋均料器保留。(4)調節劑由一點加入改為兩點加入,其中第二點在3釜入口加料,加料比例控制在30%,從生產看,門尼控制更加穩定,門尼調節速度更快、更便捷。(5)am2和終止劑的加料量主要影響產品的300%定伸,將am加料量控制在0.055phr,sdd終止劑加料比例控制在260-270%之間,可保證產品定伸處于中限值。 (6)am2與膠乳混合進料可提高am2的利用率,提高產品300%定伸。
      參考文獻:
      [1]朱敏.橡膠化學與物理[m].北京:化學工業出版社,1984.
      [2]曹湘洪主編.乳液聚合丁苯橡膠.北京:中國石化出版社,2011.
      [3]合成橡膠生產.中國石油撫順石化公司培訓教程.
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