WO2013013518A1 - 一种密封圈及其制备方法 - Google Patents

一种密封圈及其制备方法 Download PDF

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Publication number
WO2013013518A1
WO2013013518A1 PCT/CN2012/073617 CN2012073617W WO2013013518A1 WO 2013013518 A1 WO2013013518 A1 WO 2013013518A1 CN 2012073617 W CN2012073617 W CN 2012073617W WO 2013013518 A1 WO2013013518 A1 WO 2013013518A1
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Prior art keywords
titanium
melting
sealing
aluminum
mixture
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PCT/CN2012/073617
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English (en)
French (fr)
Inventor
陈学敏
叶清东
袁纪敏
胡力平
殷鸣
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深圳市新星轻合金材料股份有限公司
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Priority to GB201317327A priority Critical patent/GB2503388B/en
Publication of WO2013013518A1 publication Critical patent/WO2013013518A1/zh

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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00Obtaining refractory metals
    • C22B34/10Obtaining titanium, zirconium or hafnium
    • C22B34/12Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16JPISTONS; CYLINDERS; SEALINGS
    • F16J15/00Sealings
    • F16J15/02Sealings between relatively-stationary surfaces
    • F16J15/06Sealings between relatively-stationary surfaces with solid packing compressed between sealing surfaces
    • F16J15/08Sealings between relatively-stationary surfaces with solid packing compressed between sealing surfaces with exclusively metal packing
    • F16J15/0806Sealings between relatively-stationary surfaces with solid packing compressed between sealing surfaces with exclusively metal packing characterised by material or surface treatment
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Definitions

  • the present invention relates to a sealing crucible and a method of preparing the same, and more particularly to a sealing crucible for use in preparing a titanium sponge device and a method of preparing the same.
  • the production process of sponge titanium at home and abroad is mainly: metal thermal reduction method, especially the preparation of metal M by the reaction of metal reducing agent (R) with metal oxide or chloride (M X).
  • the titanium metallurgical methods that have been industrially produced are the magnesium thermal reduction method (Kro l method) and the sodium thermal reduction method (Hunter method). Because the Hunter method is more expensive to produce than the Kro l method, the only widely used method in the industry is the Kro l method.
  • the main process in the Kroll method is as follows: after removing the oxide film and impurities, the magnesium ingot is placed in a reactor for heating and melting, and then titanium tetrachloride (T iC , titanium particles formed by the reaction) is introduced.
  • the formed liquid magnesium chloride is discharged through the slag mouth in a timely manner.
  • the reaction temperature is usually maintained at 800 ⁇ 900 ° C, and the reaction time is between several hours and several days.
  • the residual magnesium metal and magnesium chloride in the final product can be removed by hydrochloric acid, or It is distilled off at 900 °C and maintains the high purity of titanium.
  • the disadvantages of the Kroll method are higher cost, longer production cycle and environmental pollution, which limits further application and promotion. Currently, the process does not The fundamental change is still intermittent production, which has failed to achieve continuous production.
  • the seal between the reactor cover and the reactor needs to be sealed, and the performance of the seal ⁇ is very high. It is necessary to ensure that there is no air leakage in the high temperature and high pressure production environment. In the production process, the selection and preparation of the sealing crucible are less studied. The current sealing crucible is not subjected to high pressure and temperature, so that the safety can not be ensured during the operation, and the utilization rate of the equipment is also affected. Productivity.
  • the present invention provides a sealing ⁇ , which is a vital part of the reaction device, which is characterized by easy deformation and is certain Under high pressure conditions, the sealing jaw does not break.
  • the commonly used sealing material is rubber, which has the disadvantages of high airtightness but low pressure and low temperature.
  • the present invention has been made. Provides a sealing ⁇ , in percent by weight, Aluminum: 8 0% - 85%;
  • Titanium 10% - 15%
  • aluminum has a melting point of 660 ° C
  • titanium has a melting point of 1668 ° C
  • iron has a melting point of 15 35 ° C.
  • the present invention adopts the above technical features, and has the advantages that aluminum has excellent corrosion resistance and processing properties, and is suitable for Manufacture of double-clamp gaskets; Titanium has excellent corrosion resistance and high softening point under high temperature conditions. Iron can be used to adjust the hardness of the mat.
  • potassium fluoroaluminate is used as a flux component to improve the bonding strength between the sealing material and iron.
  • the reason why aluminum, titanium and iron are used as the main components of the sealing crucible is because one of the materials of the aluminum and titanium reaction process, and the iron and the main component of the reactor are identical, and the reaction is solved due to the melting of the mat.
  • the system causes pollution problems.
  • the invention also provides a method for preparing a sealing enamel material, comprising the following steps: Step A: The aluminum is melted in a medium frequency induction electric furnace, and after melting, potassium fluoroaluminate is added, melted, and stirred uniformly;
  • the melting time in the step C is 4 to 6 hours.
  • the mold in the step D is made of high alumina cement or copper material.
  • sealing enamels having different melting points and softening temperatures can be produced.
  • the sealing crucible prepared in Example 3 is applied to a reaction apparatus for titanium sponge production, the apparatus comprising: a reactor and a reactor cover with a stirring device, the reactor cover and the reactor a sealing raft is disposed between the sides of the reactor cover; a lifting device for controlling the lifting and lowering of the reactor cover is disposed, and an electric resistance furnace is further disposed above the reactor cover, and the electric resistance furnace is disposed under the electric resistance furnace A valve is disposed, and an evacuation tube and an inflation tube are disposed above the reactor cover.
  • Step A 36 g of aluminum and 36 g of magnesium are placed in an electric resistance furnace, evacuated, argon gas is passed, and heated to form a mixed liquid;
  • Step B Open the reactor lid, add a calculated amount of potassium fluorotitanate to the reactor, cover the reactor lid, check for leaks, slowly warm to 150 °C, evacuate and heat to 250 °C.
  • Step C argon gas was introduced into the reactor, and the temperature was further raised to 750 ° C;
  • Step E Open the cover of the reactor is removed with stirring, remove the upper KA1 F 4, KF and MgF 2, to give 45.12 g of titanium sponge; product content of titanium was 96.5%, the reduction rate is 90.7%.
  • Example 5 36 g of aluminum, 18 g of magnesium and 240 g of potassium fluorotitanate were reacted at 800 ° C under vacuum under argon atmosphere;

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • General Engineering & Computer Science (AREA)
  • Geology (AREA)
  • Manufacturing & Machinery (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Gasket Seals (AREA)

Abstract

一种密封圈,所述密封圈按重量百分比计,包括:铝:80%—85%;钛:1Q%—15%;铁屑:0.1%—1%;氟铝酸钾:4%—4.9%。还公开了一种制备方法,包括以下几个步骤:步骤A:将铝置于中频感应电炉内熔化,熔化后加入氟铝酸钾,熔融,搅拌均匀;步骤B:于上述混合物中先后加入钛屑或者海绵钛,以及,铁屑,于80(TC至120(TC下使所述混合物完全熔融混合,搅拌均匀后静置;步骤C:除去表面浮渣;步骤D:浇铸至模具中成型,得到最终的密封圈。该密封圈具有可调控的软化点和熔点,可以用作不同反应器或蒸馏器的密封垫圈,保证了高压状态下生产过程的顺利进行,解决了高温条件下反应器及蒸馏器的耐压密封问题。

Description

一种密封圏及其制备方法
技术领域
本发明涉及一种密封圏及其制备方法,尤其涉及一种用于制备海绵钛设 备中的密封圏及其制备方法。 背景技术
国内外的海绵钛生产工艺主要是: 金属热还原法, 尤其是指利用金属 还原剂(R)与金属氧化物或氯化物(M X)的反应制备金属 M。 已经实现工业 化生产的钛冶金方法为镁热还原法(Kro l l法)和钠热还原法(Hunter法)。 因为 Hunt er法比 Kro l l法生产成本高,所以目前在工业中广泛应用的方法 只有 Kro l l法。在克罗尔(Kro l l)法中的主要工艺过程为:镁锭经除氧化膜 与杂质之后, 置于反应器中加热熔化, 再通入四氯化钛(T iC , 反应生成 的钛颗粒沉积, 生成的液态氯化镁通过渣口及时排出。 反应温度通常保持 在 800 ~ 900 °C , 反应时间在几小时至几天之间。 最终产物中残留的金属镁 与氯化镁可用盐酸清洗除去, 也可在 900 °C下空蒸馏除去, 并保持钛的高 纯度。 克罗尔法的缺点是成本较高, 生产周期较长, 并且污染环境, 限制 了进一步的应用和推广。 目前, 该工艺并没有根本的改变, 仍然是间歇式 生产, 未能实现生产的连续化。
在生产海绵钛的设备中, 反应器盖与反应器之间需要用到密封圏进行 密封, 并且对密封圏的性能要求很高, 需保证在高温高压的生产环境下绝 对不漏气, 但现生产工艺中对密封圏的选择和制备研究得比较少, 目前的 密封圏所承受的压力和温度都不高, 使得设置在运转过程中安全性不能得 到保证, 并且也影响了设备的使用率和生产效率。
发明内容
为了解决现有技术中成本高、 污染严重、生产周期长的缺点, 本发明提 供了一种密封圏, 密封圏是所述反应设备有至关重要的部分, 其特点是容 易变形, 且在一定的高压条件下, 密封圏不会破裂, 现有技术中, 常用的 密封圏材料是橡胶, 作为密封圏气密性高但承受的压力和温度低的缺点, 为了解决这个技术问题, 本发明了提供了一种密封圏, 按重量百分比计, 铝: 8 0%- 85%;
钛: 1 0%- 15%;
铁屑: 0. 1%-1%;
氟铝酸钾: 4%_4. 9%。
其中, 铝的熔点为 660 °C , 钛的熔点为 1668 °C , 铁的熔点为 15 35 °C , 本发明采用以上技术特征, 其优点在于, 铝具有优秀耐腐蚀性能和加工性 能, 适用于制造双夹垫片; 钛在高温条件下, 具有优异的耐腐蚀性能, 调 节软化点。 铁可以用来调节垫圏的软硬度。 并且采用氟铝酸钾作为助熔剂 成分, 可以提高密封圏材料与铁的结合力。 并且, 之所以选用铝、 钛、 铁 作为密封圏的主要成分, 是因为铝和钛系反应过程的物料之一, 而铁与反 应器的主成分的一致, 解决了因垫圏熔化而对反应体系造成污染的问题。
本发明还提供了一种制备密封圏材料的方法, 包括以下几个步骤: 步骤 A: 将铝置于中频感应电炉内熔化, 熔化后加入氟铝酸钾, 熔融, 搅拌均匀;
步骤 B:于上述混合物中先后加入钛屑或者海绵钛,以及,铁屑,于 800 °C 至 1200 °C下使所述混合物完全熔融混合, 搅拌均匀后静置;
步骤 C:除去表面浮渣;
步骤 D:浇铸至模具中成型, 得到最终的密封圏。
优选的, 所述步骤 C中熔融的时间为 4至 6小时。
优选的, 所述步骤 D中的模具采用高铝水泥或者铜材料。
本发明的有益效果是: 采用本发明中的密封圏, 具有可调控的软化 点和熔点,可以用作不同反应器或蒸馏器的密封垫圏,保证了高压状态 下生产过程的顺利进行,解决了高温条件下反应器及蒸馏器的耐压密封 问题。
具体实施方式
下面对本发明的较优的实施例作进一步的详细说明:
实施例 1 :
将 80份铝置于中感应电炉内熔化,熔化后加入 4份氟铝酸钾,混 合, 搅拌均匀; 在上述混合物中先后加入 15份钛和 1份铁屑, 混合, 搅拌均匀; 于 800 °C至 1 200 °C下使所述混合物完全熔融 4小时后静置, 再除去表面浮渣;将得到的混合物浇铸至模具中成型,得到最终的密封 圏。
实施例 2 :
将 82份铝置于中感应电炉内熔化, 熔化后加入 4. 5份氟铝酸钾, 混合, 搅拌均匀; 在上述混合物中先后加入 1 3份钛和 0. 5份铁屑, 混 合,搅拌均匀; 于 800 °C至 1200 °C下使所述混合物完全熔融 5小时后静 置, 再除去表面浮渣; 将得到的混合物浇铸至模具中成型,得到最终的 密封圏。 实施例 3 :
将 85份铝置于中感应电炉内熔化, 熔化后加入 4. 9份氟铝酸钾, 混合, 搅拌均匀; 在上述混合物中先后加入 10份钛和 0. 1份铁屑, 混 合,搅拌均匀; 于 800 °C至 1200 °C下使所述混合物完全熔融 6小时后静 置, 再除去表面浮渣; 将得到的混合物浇铸至模具中成型,得到最终的 密封圏。
本发明中的密封圏的性能与现有技术中密封圏的性能对比:
Figure imgf000004_0001
从实施例可以看出, 根据各原料含量的不同, 可以制造不同熔点和变 软温度的密封圏。
将实施例 3所制成的密封圏应用在一种用于海绵钛生产的反应设备中, 该设备包括: 反应器和带有搅拌装置的反应器盖,所述反应器盖与所述反 应器之间设置有密封圏; 所述反应器盖的侧面设置有用于控制所述反应器 盖升降的升降装置, 所述反应器盖上方还设置有电阻炉, 所述电阻炉下方 设置有阀门, 所述反应器盖上方设置有抽真空管和充气管。
实施例 4:
所涉及到的化学方程式:
3K2TiF6+4Al = 3Ti+6KF+4AlF3
K2TiF6+2Mg=Ti+2MgF2+2KF
步骤 A: 将 36克铝和 36克镁放置在电阻炉中, 抽真空, 通氩气, 加热 至生成混合液;
步骤 B: 打开反应器盖, 加入计算量的氟钛酸钾于反应器中, 盖上反应 器盖后, 检漏, 緩慢升温至 150 °C后, 抽真空, 再加热至 250 °C。
步骤 C: 向反应器中通入氩气, 继续升温至 750 °C ;
步骤 D : 开启阀门, 调节速度, 滴入混合液, 并控制反应的温度为 750- 850 °C .
步骤 E: 打开反应器盖, 移出搅拌, 清除上层的 KA1 F4、 KF和 MgF2 , 得到海绵钛 45. 12克; 产物中含钛量为 96. 5%, 还原率为 90. 7%。
该反应设置采用本发明中的密封圏, 进一步提高了生产海绵钛过程中 的真实度, 提高了产率。
将本发明中的密封圏应用于一种专门用于生产海绵钛的蒸馏设备,该设 备包括: 加热炉和用于盛冷凝物的反应器, 所述加热炉上方设置有加热炉 盖, 所述反应器上方设置有反应器盖, 所述加热炉盖和反应器盖之间用管 道相连; 所述管道上设置有电阻丝; 所述加热炉盖和反应器盖上方各设置 有升降装置; 所述加热器盖上方设置有抽真空管; 所述管道的两端与所述 加热炉盖和反应器盖之间分别设置有第一金属密封圏和第二金属密封圏。
第一金属密封圏采用实施例 1中的金属密封圏,第一金属密封圏采用实 施例 2中的金属密封圏.
实施例 5 : 真空通氩气的条件下, 将 36克铝、 18克镁和 240克氟钛 酸钾在 800 °C下进行反应;
真空状态下, 在加热炉中 11 00 °C蒸馏; 将反应生成的 KF、 A1F3、 MgF2 和 Mg通过管道进入反应器内;
保持真空状态, 冷却后得到海绵钛 45. 45克; 产物中含钛量为 98% , 还原率为 92. 8%。 采用以上金属密封圏,可以进一步保证蒸馏过程中的密封性,提高蒸馏 的效率, 以及对生产出的海绵钛的纯度和还原率有 ^艮大的提高。
以上内容是结合具体的优选实施方式对本发明所作的进一步详细说 明, 不能认定本发明的具体实施只局限于这些说明。 对于本发明所属技术 领域的普通技术人员来说, 在不脱离本发明构思的前提下, 还可以做出若 干筒单推演或替换, 都应当视为属于本发明的保护范围。

Claims

权利要求书
1、 一种密封圏, 其特征在于, 按重量百分比计, 包括:
铝: 8 0%- 85%;
钛: 1 0%- 15%;
铁屑: 0. 1%-1%;
氟铝酸钾: 4%_4. 9%。
2、 一种制备如权利要求 1 所述的密封圏的方法, 其特征在于, 包括 以下几个步骤:
步骤 A: 将铝置于中频感应电炉内熔化, 熔化后加入氟铝酸钾, 熔融, 搅拌均匀;
步骤 B:于上述混合物中先后加入钛屑或者海绵钛,以及,铁屑,于 800 °C 至 1200 °C下使所述混合物完全熔融混合, 搅拌均匀后静置;
步骤 C:除去表面浮渣;
步骤 D:浇铸至模具中成型, 得到最终的密封圏。
3. 如权利要求 2所述的方法, 其特征在于, 所述步骤 C中熔融的时 间为 4至 6小时。
4. 如权利要求 3所述的方法, 其特征在于, 所述步骤 D中的模具采 用高铝水泥或者铜材料。
PCT/CN2012/073617 2012-01-18 2012-04-07 一种密封圈及其制备方法 WO2013013518A1 (zh)

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US9765887B2 (en) 2017-09-19
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