有机硅废触体合成四氯化硅项目圆满完成科研攻关任务

日前 ,由中油吉林石化公司研究院与吉林化学工业股份有限公司电石厂共同研发的有机硅废触体合成四氯化硅技术开发项目经全体科研人员的共同努力 ,中试装置实现连续稳定开车 5 5 0h ,各项数据指标均达到预期要求 ,这标志着该项课题攻关任务圆满完成。有机硅废触体合成四氯化硅技术开发项目是中油吉林石化公司 2 0 0 3年“六大投产项目”之一——— 5万t/a有机硅生产装置的配套技术 ,属中油股份有限公司级科研项目。废触体是有机硅单体合成过程中产生的以硅、铜、碳为主的废渣 ,不易储存 ,对环境污染严重 ,同时也成为生产安全隐患。随着有机硅…     

吉林石化废触体合成四氯化硅技术获国家专利

吉林石化公司研究院开发成功的利用废触体合、成四氯化硅技术成果，日前获国家发明专利。     

吉林石化废触体合成四氯化硅技术获国家专利

吉林石化公司研究院开发成功的利用废触体合成四氯化硅技术成果，日前获国家发明专利。     

我国第一套年产5000吨利用废触体合成四氯化硅装置在吉化开工建设

我国第一套年产5000吨利用废触体合成四氯化硅装置在吉化开工建设     

有机硅废触体处理的研究进展

综述了有机硅废触体处理的研究进展,介绍了包括氧化还原回收铜、废触体深度转化和其他用途在内的3种处理方法及其处理效果的影响因素,并展望了有机硅废触体处理的发展方向。     

吉林石化废触体合成四氯化硅技术获国家专利

吉林石化公司研究院开发成功的利用废触体合成四氯化硅技术成果，日前获国家发明专利。     

5 kt/a利用废触体合成四氯化硅装置开工建设

我国第一套5kt／a利用废触体合成四氯化硅生产装置于2004年9月20日在吉化集团公司中部生产基地开工建设,预计在2004年12月底建成投产。     

我国第一套5000t／a利用废触体合成四氯化硅装置在吉化集团建设

我国第一套5000t／a利用废触体合成四氯化硅生产装置在吉化集团中部生产基地开工建设。这套装置是采用吉林石化公司研究院目行开发的、属国内首创的技术。针对有机硅单体合成过程中产生的废触体不易储存，严重污染环境和存在安全隐患等问题进行综合利用，化害为利．变废为宝，为我国四氯化硅生产开辟了一条新途径。     

有机硅废触体的综合利用

介绍了合成甲基氯硅烷的废触体的主要利用方法——氧化法、深度转化法、？台炼法、去活性法等，并对国内废触体的综合利用提出了建议。     

ICP-MS测定床内触体中铅的含量

文章采用电感耦合等离子体质谱仪(ICP-MS)测定了甲基氯硅烷生产使用的有机硅床内触体中的铅(Pb)含量,研究了触体中存在的主要元素铜(Cu)对Pb的基体干扰。探讨了采取不同试样预处理方法对测定结果的影响。经测试对比,先加王水热熔,后用硫酸洗脱的方式结果较为准确,测得有机硅合成床内触体中Pb含量1.516 ppm,且RSD值仅为1.03%。     

ICP-AES法测定有机硅触体中铅的含量

采用电感耦合等离子体发射光谱测定了甲基氯硅烷生产使用的触体中铅(Pb)的含量,研究了触体中存在的主要元素铜对Pb测定的光谱干扰。选择灵敏度较高的220.353 nm为分析谱线,采用与试样Cu含量基本匹配的测试方法。被测元素样品加标回收率为103%,RSD(n=10)小于3%。     

二羟基硅酞菁合成方法的研究

对二氯硅酞菁的合成进行了研究,并采用甲醇析出法分离出生成的二氯硅酞菁。利用二氯硅酞菁硫酸溶液冰水析出法将二氯硅酞菁转化为二羟基硅酞菁,收率达到77%,比文献的醇解法收率有较大提高,并通过红外分析对两种化合物的结构进行了确认。     

Combustion Synthesis of Silicon Nitride-Silicon Carbide Composites

The feasibility of synthesizing silicon nitride-silicon carbide composites by self-propagating high-temperature reactions is demonstrated. Various mixtures of silicon, silicon nitride, and carbon powders were ignited under a nitrogen pressure of 30 atm (∼ 3 MPa), to produce a wide composition range of Si₃N₄-SiC powder products. Products containing up to 17 vol% of SiC, after being attrition milled, could be hot-pressed to full density under 1700°C, 3000 psi (∼ 21 MPa) with 4 wt% of Y₂O₃. The microhardness and fracture toughness of these composites were superior to those of the pure β-Si₃N₄ matrix material and compared very well with the properties of "traditionally" prepared composites.     

Shock Synthesis of Cubic Silicon Nitride

The phase transitions of α-Si₃N₄ and β-Si₃N₄ have been investigated by shock compression through the recovery technique and Hugoniot measurements. α- and β-Si₃N₄ are transformed into a cubic spinel structure ( c -Si₃N₄). The yield of c -Si₃N₄ increases with increasing shock pressure and reaches 100% at 63 GPa. The shock-synthesized c -Si₃N₄ powders are nanocrystals and display a high-temperature metastability up to about 1620 K. c -Si₃N₄ is one of the hard materials based on the measured equation of state. c -Si₃N₄ powders have been characterized by electron microscopy and ²⁹Si magic angle spinning NMR spectroscopy. The purification and separation method has been developed to obtain pure c -Si₃N₄ powders.     

四氯化硅的合成与精制

重点介绍了四氯化硅的制备及精制工艺。四氯化硅的工业制备方法主要有硅铁氯化法、废触体氯化法、硅氢氯化法、二氧化硅氯化法等,并分别介绍了各方法的特点。其精制方法主要有吸附法、反应法、精馏法以及这些方法的组合。通过采用2级精馏方法可得到光纤级高纯四氯化硅,同时介绍了高纯四氯化硅的充装和质量标准。此外,还简要介绍了四氯化硅的应用、经济概况及展望。     

Thermogravimetry, Differential Thermal Analysis, and Mass Spectrometry Study of the Silicon Nitride–Boron Carbide–Carbon Reaction System for the Synthesis of Silicon Carbide–Boron Nitride Composites

Thermogravimetry, differential thermal analysis, mass spectrometry, and X-ray diffractometry were used to study the reaction process of the in situ reaction between Si₃N₄, B₄C, and carbon for the synthesis of silicon carbide–boron nitride composites. Atmospheres with a low partial pressure of nitrogen (for example argon + 5%–10% nitrogen) seemed to inhibit denitrification and also maintain a high reaction rate. However, the reaction rate decreased significantly in a pure nitrogen atmosphere. The experimental mass spectrometry results also revealed that B₄C in the Si₃N₄–B₄C–C system inhibited the reaction between Si₃N₄ and carbon and, even, the decomposition of Si₃N₄. The present results indicate that boron could be a composition stabilizer for ceramic materials in the Si-N-C system used at high temperature.     

直接由SiO2低温合成四配位硅衍生物及其结构表征

研究了直接从无定型二氧化硅出发,与乙二醇、氢氧化钾反应,低温合成高反应活性的五配位硅钾化合物,然后再与氯化苄（C6H5CH2CI）反应制备四配位硅化合物,并对合成的物质作了红外光谱、核磁共振（^1H、^13C)、元素分析的结构表征。     

Synthesis and Characterization of Silicon Carbide Powders Converted from Metakaolin‐Based Geopolymer

Silicon carbide (SiC) ceramic powders were synthesized by carbothermal reduction in specific geopolymers containing carbon nanopowders. Geopolymers containing carbon and having a composition M₂O·Al₂O₃·4.5SiO₂·12H₂O+18C, where M is an alkali metal cation (Na⁺, K⁺, and Cs⁺) were carbothermally reacted at 1400°C, 1500°C, and 1600°C, respectively, for 2 h under flowing argon. X‐ray diffraction and microstructural investigations by SEM/EDS and TEM were made. The geopolymers were gradually crystallized into SiC on heating above 1400°C and underwent significant weight loss. SiC was seen as the major phase resulting from Na‐based geopolymer heated to ≥1400°C, even though a minor amount of Al₂O₃ was also formed. However, phase pure SiC resulted with increasing temperature. While a slight increment of the Al₂O₃ amount was seen in potassium geopolymer, Al₂O₃ essentially replaced cesium geopolymer on heating to 1600°C. SEM revealed that SiC formation and a compositionally variable Al₂O₃ content depended on the alkaline composition. Sodium geopolymer produced high SiC conversion into fibrous and globular shapes ranging from ~5 μm to nanosize, as seen by X‐ray diffraction as well as SEM and TEM, respectively.     

In Situ Synthesis of Silicon Carbide Whiskers from Silicon Nitride Powders

Silicon carbide whiskers were synthesized in situ by direct carbothermal reduction of silicon nitride with graphite in an argon atmosphere. Phase evolution study reveals that the formation of β-SiC was initiated at 1400° to 1450°C; above 1650°C silicon was formed when carbon was deficient. Nevertheless, Si₃N₄ could be completely converted to SiC with molar ratio Si₃N₄:C = 1:3 at 1650°C. The morphology of the SiC whiskers is needlelike, with lengths and diameters changing with temperature. SiC fibers were produced on the surface of the sample fired at 1550°C with an average diameter of 0.3 μm. No catalyst was used in the syntheses, which minimizes the amount of impurities in the final products. A reaction mechanism involving the decomposition of silicon nitride has been proposed.