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    科學技術論文

    淺談氯乙烯生產提高氯乙烯轉化率的方法

    時間:2019年06月28日 所屬分類:科學技術論文 點擊次數:

    摘要:電石法生產氯乙烯過程中,有很多影響氯乙烯轉化率的因素,結合實際生產經驗,闡述各種影響因素,提出解決方法。 關鍵詞:氯乙烯;轉化率;工藝原理;影響因素 甘肅銀光聚銀公司PVC廠采用電石法懸浮聚合工藝生產SG-5型PVC樹脂,年生產能力為12萬噸。經過多

      摘要:電石法生產氯乙烯過程中,有很多影響氯乙烯轉化率的因素,結合實際生產經驗,闡述各種影響因素,提出解決方法。

      關鍵詞:氯乙烯;轉化率;工藝原理;影響因素

    工業技術創新

      甘肅銀光聚銀公司PVC廠采用電石法懸浮聚合工藝生產SG-5型PVC樹脂,年生產能力為12萬噸。經過多年的實踐探索,分廠生產工藝運行質量得到很大提升。為了不斷降低生產成本,增加企業效益,分廠引進先進的工藝技術方法,并利用現有的工藝技術和設備條件,開展技術創新活動,取得了很好的效果。其中在提高氯乙烯轉化率方面的研究,用于指導生產,使氯乙烯轉化率得到提升。

      1氯乙烯生產工藝簡述

      氯乙烯的生產方法有乙烯氧氯化、乙烷氧氯化、電石乙炔法合成等生產工藝。我分廠使用電石乙炔法合成工藝,該工藝是將電石水解精制后的乙炔氣和氯化氫合成氯乙烯。乙炔與氯化氫混合、脫水、預熱后進入列管式反應器。反應器列管內裝有以活性炭為載體的氯化汞催化劑,反應在常壓下進行,管外用加壓循環熱水除去反應熱。粗制的氯乙烯經過泡沫脫酸塔、水洗塔、堿洗塔除去未參加反應的氯化氫等氣體后進入氣柜。粗制的氯乙烯氣體經過壓縮機壓縮后,經過全凝器冷卻后,進入水分離器出水后,經過低塔進料泵進入低沸塔除去乙炔氣體和氮氣等氣體,利用壓差進入高沸塔分離出二氯乙烷,精餾后的氯乙烯儲存在單體儲槽中。

      2影響氯乙烯轉化率的因素

      乙炔的轉化率和氯乙烯的合成收率是衡量氯乙烯轉化率的重要標準。正常情況下乙炔和氯乙烯乙炔的轉化率為99%,氯乙烯的合成收率為95%以上。但是實際生產中,由于工藝運行條件的限制,這兩項指標會下降。我分廠經過不斷地技術創新,乙炔轉化率達到99.0%以上,氯乙烯合成收率達到98.5%以上。

      2.1原料氣質量的影響

      氯乙烯合成對乙炔的純度和雜質含量有嚴格的要求:乙炔純度要求≥98.5%,磷硫含量采用浸硝酸銀試紙在氣體樣中不變色。氯化氫氣體純度要求≥93%,含氧要求<0.5%[1]。乙炔純度低會使原料氣中的二氧化碳、氫氣等惰性氣體增多。乙炔氣中的硫化氫和磷化氫等能與汞觸媒發生不可逆的化學吸附,使催化劑中毒。乙炔中含有的水分易與氯化氫反應生成鹽酸,使轉化器和管線嚴重腐蝕;水分還使催化劑結塊,降低催化劑的活性,導致轉化器阻力上升,乙炔流量降低,影響生產。

      我分廠使用的氯化氫是生產甲苯二異氰酸酯副產品純度可達到96.5%以上,分廠用兩臺串聯的使用-35℃冷凍鹽水為冷卻介質的石墨冷卻器冷卻,兩臺換熱器出口溫度分別控制在為-10—-1℃,-18—-13℃之間,冷卻后的氣體經過酸霧捕集器被含氟硅油的玻璃棉進一步除去水分,酸霧捕集器出口采樣含水率≤600ppm。

      2.2設備對氯乙烯轉化率的影響

      轉化器是氯乙烯合成反應的重要設備。轉化器在制造過程中對列管和管板脹接技術有很高的要求,避免出現滲漏的現象。如果有滲漏管間的熱水會泄漏到設備內,與氣相中的氯化氫生成鹽酸,不僅腐蝕設備,而且造成觸媒結塊,降低氯乙烯的轉化率[1]。反應熱由殼層循環熱水移出。循環熱水可以采取分段進入、排出的方式。

      在轉化器的上段和下段分別安裝熱水的進出口。在催化劑裝填使用初期,通過增加上段循環熱水進出口流量,提高轉化率。為了及時移出反應熱,增加轉化器的換熱面積。在加工時,將列管由φ57mm×3.5mm縮小到φ50mm×3.0mm,增加換熱面積,達到了良好的效果。目前我分廠使用的轉化器規格為ID3000×3150×5650,換熱面積為1040m3,經過設備升級改造,滿足工藝生產的要求。

      2.3乙炔與氯化氫分子配比對合成轉化率的影響[2]

      提高原料氣乙炔或氯乙烯的的濃度或使一種原料氣配比過量,有利于反應速度和轉化率增加。但氯化氫過多,則增加的原料的消耗,還會生成1,1-二氯乙烷副產物。試驗和實踐的經驗,控制乙炔和氯化氫摩爾比在1:(1.05-1.10)為宜。實踐操作中通過控制乙炔和氯化氫的流量來控制摩爾比,以后臺轉化器出口乙炔、氯化氫含量和除汞器出口乙炔含量進行配比調整。

      2.4反應溫度的影響

      提高溫度有加快合成反應的速度,獲得較高的轉化率。但是過高的溫度使氯化汞觸媒升華,降低氯化汞觸媒的活性,如果溫度超過180℃,有“燒壞”氯化汞觸媒及轉化器的危險,一般合成溫度控制在100-180℃,合成反應的最佳反應溫度是130-150℃。分廠控制反應溫度是通過控制乙炔氣的流量和轉化器的循環熱水量。如果反應溫度過高,通過降低乙炔氣的通入量和控制循環熱水循環量,或者通過排放循環熱水中的飽和蒸汽,達到降低反應溫度。

      2.5氯化汞觸媒活性的影響

      氯化汞觸媒的使用時間直接影響到合成反應的正常進行,其使用周期分為早期、中期和衰老期三個階段。在早期新裝填的氯化汞觸媒反應活性高,反應集中在轉化器列管的上端,熱點在氯化汞催化劑的上層,此時為限制熱點下移速度,提高轉化率,可以進行給轉化器循環熱水排氣,降低轉化器殼層上部的飽和蒸汽量,達到降低轉化器上層溫度的目的,提高氯化汞的使用壽命[3]。此階段一定要嚴控好乙炔氣的通入量和轉化器循環熱水的循環量,防止合成溫度超過180℃。

      當汞觸媒使用時間在500-1000h以后,這是氯化汞觸媒反應最佳時期,可以將乙炔流量調整至最大值,轉化器的轉化率最高。使用3000-4000小時后氯化汞觸媒進入衰老期,這時的氯乙烯轉化率下降,可以降低乙炔氣的通入量。我分廠設立專用臺賬,記錄每一臺轉化中氯汞觸媒翻換時間結合實際反應情況來判斷氯化汞觸媒的活性,當氯化汞觸媒活性到后期,降低乙炔通量,翻換觸媒,以保證氯乙烯轉化率達到最大值。

      參考文獻:

      [1]鄭石子,顏才南,胡志宏,曾建華.聚氯乙烯生產與操作(第二版)[D].2007(10).

      [2]嚴福英.聚氯乙烯工藝學(第一版)[M].1990(06).

      [3]邴涓林,黃志明.聚氯乙烯工藝技術(第一版)[M].2008(04).

      相關刊物推薦:《工業技術創新》是工業和信息化部主管、中國電子信息產業發展研究院主辦的國家級科技學術類期刊。本刊主要面向工業技術創新領域的有關工業主管部門、工業企業、科研創新的學術交流平臺、技術創新成果的宣傳轉化園地和戰略政策研究的理論探討陣地。

      

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