MCT PROCESS BENCH SCALE UNIT RESULTS

In Sep. 2013, Beijing Huashi decided to design and build a bench scale experimental unit associating with the R&D institution, and on the basis of MCT theoretical research, in Sanju Fuda Fertilizer & Catalyst National Engineering Research Center (Hereinafter referred to as “Sanju Fuda”).

Fig.1 The bench scale experimental unit

After finishing designing the experimental scheme, dedicated catalysts were used regarding to certain types of inlet raw material, and the experiment was carried out in parallel several times with varying (one of the) reaction parameters. A large number of experimental data was obtained. Further in-depth research and analysation of these data provided deeper research results, which pointed out the direction of the design and development of the pilot plant.

Key Results Obtained

1. Research on the performance of different catalysts, mainly focused on the catalysts with size less than 5 μm. The appropriate inlet raw-catalyst ratio was found for different catalyst. Successfully located and figured the performance of the active functional group of hydrotreating, and established an infinitesimal reactor theory system.
2. Carried out the research on the coking substance adsorption performance of the catalyst in suspended bed. Observed the percentage conversion, coking status of the reactor etc. through modifying the catalyst’s pore volume, specific surface area. Several new suspended-bed-dedicated catalysts were developed which can effectively avoid the polymerization of coking precursor such as colloid and asphaltene base on these observations.
3. Research on the bed formed by catalysts with different size distribution. Through measuring and calculating parameters such as bed density, size of the bubble, gas holdups, solid concentration etc., a new reaction system was developed, which is called “three phase well-mixed bedless infinitesimal reaction system”. This system is capable of pushing the reaction rate towards its theoretical limit as far as possible, therefore maximized the catalysts’ reactivity, mixing rate, disperse performance, and reaction space usage efficiency.
4. Research on the change pattern of the percentage conversion regarding to the reaction temperature. The appropriate reaction temperature of different inlet materials was found ranged 430~450 ℃. Obtained the change pattern of the reaction rate of different inlet raw regarding to different heating rate (℃/min), and located the reaction-rate -sensitive temperature range.
5. Obtained the mass balance of different inlet raw under different reaction condition, and carried out in-depth research on the products to optimize the production route of the MCT process.
6. Research on the change pattern of the percentage conversion regarding to the reaction pressure. The appropriate reaction pressure of upgrading heavy-oil was found ranged 18~25 Mpa.
7. Construct the reaction model of the suspended bed hydrotreating process on the basis of the product yield under different reaction condition associating with the thermalcracking and hydrocracking model.
8. Through the analysation of the coking substance of different inlet raw, the coking features in hydrogen environment were obtained, along with a theoretical coking avoiding scheme involving usage of appropriate catalyst and operating condition.
9. Research on the percentage conversion regarding to the different contact time and optimized the process accordingly.
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MCT工藝小試階段成果

2013年9月，公司在研究MCT理論技術的基礎上，與科研單位合作，在福建三聚福大化肥催化劑國家工程研究中心設計并建立了小試裝置。

圖1  實驗小試裝置
在設計了科學的實驗方案基礎上，針對各種原料，采用不同的催化劑，在不同反應條件下做了多組平行實驗，得到了大量的實驗數據。針對這些數據我們又做了大量的分析研究工作，取得了重要的研究成果，為下一步中試裝置的設計及開發指明了方向。
主要實驗內容及取得的重要成果：
1、探究了不同催化劑的催化性能，重點實驗了小于5微米的納米型催化劑的催化反應性能，得到了不同催化劑適宜的加入比例，摸索出了加氫及裂化活性組元的關鍵性能，建立了一套無限微反應器的理論體系。
2、研究了懸浮床催化劑的吸附焦炭的性能，通過改變催化劑的孔容、比表面積等重要參數，來觀察反應轉化率、反應釜的結焦情況等一系列的現象，創造了多種能很好避免膠質、瀝青質等結焦前軀物縮合團聚的懸浮床催化劑。
3、研究了不同粒度范圍的催化劑所形成的床層，通過測量計算床層的密度、氣泡尺寸、氣含率、固含率等一系列參數，開發了獨具特色的三相均質無床層無限微反應體系，該體系具有無限接近反應動力極限的反應速率，更好的發揮催化劑的反應活性，快速有效的混合速率，高度均勻的分散性能，高效的反應空間利用率等優點
4、探究了轉化率隨反應溫度的變化規律，找出了不同原料適宜的反應溫度430~450℃。通過研究反應器的溫升速率，得出了不同原料反應速率的變化規律，找出了影響反應速率的敏感溫度區間。
5、通過實驗得到了大量的不同原料在不同反應條件下的物料平衡數據，并對產品性質進行了深入的分析研究，確定了MCT工藝可實現的產品路線。
6、探究了轉化率隨反應壓力及氫分壓的變化規律，得出了適宜重油加工的合適的反應壓力范圍（18~25MPa）。
7、通過分析不同條件下的產品收率數據，再結合熱裂化和加氫裂化的反應模型，建立了懸浮床加氫工藝的反應模型。
8、通過對不同原料的結焦物進行分析，得出了不同原料在氫環境下的結焦特性，并形成了一套控制結焦的理論，比如選擇合適的催化劑、工藝條件及反應器結構來避免結焦。
9、通過研究不同的反應時間對轉化率的影響，得出了不同原料所需的合適的反應時間。