WO2014201752A1 - 一种高效制备氢氧化镁的制备方法及装置 - Google Patents

一种高效制备氢氧化镁的制备方法及装置 Download PDF

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Publication number
WO2014201752A1
WO2014201752A1 PCT/CN2013/080196 CN2013080196W WO2014201752A1 WO 2014201752 A1 WO2014201752 A1 WO 2014201752A1 CN 2013080196 W CN2013080196 W CN 2013080196W WO 2014201752 A1 WO2014201752 A1 WO 2014201752A1
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Prior art keywords
linkage unit
pressure control
control linkage
reactor
pressure
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PCT/CN2013/080196
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English (en)
French (fr)
Inventor
朱益民
唐晓佳
郭琳
刘全
陈晨
李铁
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Dalian Maritime University
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Dalian Maritime University
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Priority claimed from CN201310248358.1A external-priority patent/CN103303947B/zh
Priority claimed from CN2013203542385U external-priority patent/CN203284218U/zh
Application filed by Dalian Maritime University filed Critical Dalian Maritime University
Priority to JP2016520234A priority Critical patent/JP6212211B2/ja
Priority to KR1020167001340A priority patent/KR101795974B1/ko
Priority to US14/900,334 priority patent/US9776882B2/en
Priority to EP13887283.3A priority patent/EP3012222A4/en
Publication of WO2014201752A1 publication Critical patent/WO2014201752A1/zh
Anticipated expiration legal-status Critical
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00—Compounds of magnesium
    • C01F5/14—Magnesium hydroxide
    • C01F5/16—Magnesium hydroxide by treating magnesia, e.g. calcined dolomite, with water or solutions of salts not containing magnesium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/008—Details of the reactor or of the particulate material; Processes to increase or to retard the rate of reaction

Definitions

  • the invention relates to a preparation method and device for efficiently preparing magnesium hydroxide. Background technique
  • magnesium hydroxide As a green material, magnesium hydroxide is widely used in fireproof materials, agriculture, and environmental protection. There are usually five ways to obtain magnesium hydroxide industrially: 1. Producing magnesium hydroxide by reacting limestone with brine; 2. Producing magnesium hydroxide by reacting sodium hydroxide with brine and halogen block; 3. Using calcined magnesite Minerals, dolomite and brine, halogen block reaction to produce magnesium hydroxide; 4, using ammonia and brine, halogen block reaction to produce magnesium hydroxide; 5, using magnesium oxide hydration to form magnesium hydroxide, where the magnesium oxide must be light burnt products To ensure the hydration activity. The most common method is to obtain magnesium hydroxide by hydration of lightly burned magnesia.
  • the hydration is usually carried out under stirring conditions.
  • the hydration conditions are basically: hydration temperature 30 ⁇ 60 ° C; magnesium oxide slurry Concentration 5 ⁇ 20% (w/w); hydration time l ⁇ 24h, hydration rate 60 ⁇ 80%.
  • the invention aims to stably and efficiently prepare a magnesium hydroxide slurry by controlling pressure and temperature to react magnesium oxide with water vapor.
  • the invention provides a device for efficiently preparing magnesium hydroxide, comprising a mixing tank, a pressure control linkage unit I, a reactor, a pressure control linkage unit II, a condenser, a two-position three-way valve, a storage tank, and a pressure control linkage.
  • Unit III, steam generator, the mixing tank discharge port and the pressure control linkage unit I are connected by a pump at one end, the other end of the pressure control linkage unit I is connected with the reactor inlet, and the reactor discharge port is linked with the pressure control.
  • One end of the unit II is connected, the other end of the pressure control linkage unit II is connected with one end of the condenser, the other end of the condenser is connected with the first interface of the two-position three-way valve, and the second interface of the two-position three-way valve is connected with the return port of the mixing tank.
  • the third port of the two-way three-way valve is connected to the storage tank, the steam inlet of the reactor is connected to one end of the pressure control linkage unit III, and the other end of the pressure control linkage unit III is connected to the steam generator.
  • the pressure control linkage unit of the present invention preferably consists of a pressure sensor and a solenoid valve.
  • magnesium hydroxide In the prior art, water molecules are adsorbed onto the surface of the magnesium oxide particles, and the magnesium hydroxide formed by the reaction is covered with magnesium oxide particles. On the surface of the granule, the progress of the further hydration reaction is hindered.
  • the magnesium hydroxide is prepared by the apparatus of the present invention, the high pressure steam is directly contacted with the solid, and a gas-solid reaction occurs, and the magnesium hydroxide formed on the surface of the magnesium oxide particle is rapidly stripped. The magnesium oxide particles are continuously hydrated, and after cooling, a magnesium hydroxide slurry is obtained.
  • Another object of the present invention is to provide a method for efficiently preparing magnesium hydroxide, which comprises the following steps:
  • the magnesium oxide accounts for 5 to 15% of the total weight
  • the magnesium oxide slurry is added to the reactor through a pump, the steam generator is turned on, steam is introduced into the reactor, the reactor is heated, the pressure of the pressure control linkage unit I is controlled to be 0.2 to 0.5 MPa, and the pressure of the pressure control linkage unit II is 0.2 ⁇ 0.5MPa, the pressure control linkage unit III pressure is 0.2 ⁇ 0.5MPa, the reaction temperature is 90 ⁇ 150°C, and the liquid in the reaction is returned from the second interface of the two-position three-way valve to the mixing tank, and then the mixing tank Returning to the reactor to form a circulation loop;
  • the feed pressure is controlled by the pressure control linkage unit I, and the steam generated by the steam generator is reacted with the magnesium oxide slurry through the pressure control linkage unit III, and the water hammer phenomenon during the reaction is controlled by the pressure control linkage unit II.
  • the magnesium oxide of the present invention is preferably 15% by weight based on the total weight.
  • the pressure of the pressure control linkage unit I of the present invention is preferably 0.3 to 0.5 MPa.
  • the pressure of the pressure control linkage unit II of the present invention is preferably 0.3 to 0.5 MPa.
  • the pressure of the pressure control linkage unit III of the present invention is preferably 0.3 to 0.5 MPa.
  • the reaction temperature of the present invention is preferably from 120 to 150 °C.
  • the above preferred ratio of magnesium oxide, the pressure control linkage unit I pressure, the pressure control linkage unit II pressure, the pressure control linkage unit III pressure and the reaction temperature bring the magnesium hydroxide reaction conversion ratio to 90% or more.
  • Figure 1 of the present invention is a schematic view showing the structure of a high-efficiency preparation of a magnesium hydroxide device
  • a device for efficiently preparing magnesium hydroxide comprising a mixing tank 1, a pressure control linkage unit 1, a reactor 3, a pressure control linkage unit 114, a condenser 5, a two-position three-way valve 6, a storage tank 7, and a pressure Control the linkage unit 1118, the steam generator 9, the mixing tank discharge port 11 and the pressure control linkage unit I 2 - end are connected by a pressure water pump, and the other end of the pressure control linkage unit I 2 is connected with the reactor feed port 31,
  • the reactor discharge port 32 is connected to the pressure control linkage unit ⁇ 4-terminal, the other end of the pressure control linkage unit ⁇ 4 is connected to the condenser 5-end, and the other end of the condenser 5 is connected to the two-position three-way valve first interface 61, two The three-way valve second port 62 is connected to the mixing tank return port 12, the two-position three-way valve third port 63 is connected to the storage tank 7, and the reactor steam inlet 33 is connected to the pressure control linkage unit ⁇
  • a preparation method for efficiently preparing magnesium hydroxide comprising the following steps:
  • the magnesium oxide slurry is added to the reactor 3 through a pump, the steam generator 9 is turned on, steam is introduced into the reactor 3, the reactor 3 is heated, and the pressure of the pressure control linkage unit is controlled to be 0.2 to 0.3 MPa, and the pressure is controlled.
  • the pressure of the linkage unit II 4 is 0.2 to 0.3 MPa
  • the pressure of the pressure control linkage unit ⁇ 8 is 0.2 to 0.3 MPa
  • the reaction temperature is raised to 90 to 120 ° C
  • the liquid in the reaction is returned from the two-position three-way valve second interface 62 to the mixture.
  • the tank 1 is returned to the reactor 3 by the mixing tank 1 to form a circulation loop, and the circulation flow rate is 1.95 L/min;
  • Example 1 After 3 cycles of 35 minutes, the two-position three-way valve second port 62 is closed, the two-position three-way valve third port 63 is opened, and the reacted liquid is added to the storage tank 7.
  • Table 1 The experimental results of Example 1 are shown in Table 1:
  • Embodiment 1 The difference from Embodiment 1 is:
  • a preparation method for efficiently preparing magnesium hydroxide comprising the following steps:
  • the magnesium oxide slurry is added to the reactor 3 through a pump, the steam generator 9 is turned on, steam is introduced into the reactor 3, the reactor 3 is heated, and the pressure of the pressure control linkage unit is controlled to be 0.3 to 0.5 MPa, and the pressure is controlled.
  • the pressure of the linkage unit II 4 is 0.3 ⁇ 0.5MPa
  • the pressure of the pressure control linkage unit ⁇ 8 is 0.3 ⁇ 0.5MPa
  • the reaction temperature is raised to 120 ⁇ 150°C
  • the liquid in the reaction is returned from the two-position three-way valve second interface 62 to the mixing.
  • the tank 1 is returned from the mixing tank 1 to the reactor 3 to form a circulation loop, and the circulation flow rate is 1.55 L/min;
  • the second port 3 of the three-way valve is closed, the third port 63 of the three-way valve is opened, and the liquid after the reaction is added to the storage tank 7.
  • Embodiment 1 The difference from Embodiment 1 is:
  • a preparation method for efficiently preparing magnesium hydroxide comprising the following steps:
  • the magnesium oxide slurry is added to the reactor 3 through a pump, the steam generator 9 is turned on, steam is introduced into the reactor 3, the reactor 3 is heated, and the pressure of the pressure control linkage unit is controlled to be 0.2 to 0.3 MPa, and the pressure is controlled.
  • the pressure of the linkage unit II 4 is 0.2 to 0.3 MPa
  • the pressure of the pressure control linkage unit ⁇ 8 is 0.2 to 0.3 MPa
  • the reaction temperature is raised to 90 to 120 ° C
  • the liquid in the reaction is returned from the two-position three-way valve second interface 62 to the mixture.
  • the tank 1 is returned to the reactor 3 by the mixing tank 1 to form a circulation loop, and the circulation flow rate is 1.2 L/min;
  • the second port 3 of the three-way valve is closed, the third port 63 of the three-way valve is opened, and the liquid after the reaction is added to the storage tank 7.
  • Embodiment 1 The difference from Embodiment 1 is:
  • a preparation method for efficiently preparing magnesium hydroxide comprising the following steps:
  • the magnesium oxide slurry is added to the reactor 3 through a pump, the steam generator 9 is turned on, steam is introduced into the reactor 3, the reactor 3 is heated, and the pressure of the pressure control linkage unit is controlled to be 0.3 to 0.5 MPa, and the pressure is controlled.
  • the pressure of the linkage unit II 4 is 0.3 ⁇ 0.5MPa
  • the pressure of the pressure control linkage unit ⁇ 8 is 0.3 ⁇ 0.5MPa
  • the reaction temperature is raised to 120 ⁇ 150°C
  • the liquid in the reaction is returned from the two-position three-way valve second interface 62 to the mixing.
  • the tank 1 is returned to the reactor 3 by the mixing tank 1 to form a circulation loop, and the circulation flow rate is 2.9 L/min;
  • the second port 3 of the three-way valve is closed, the third port 63 of the three-way valve is opened, and the liquid after the reaction is added to the storage tank 7.
  • Embodiment 1 The difference from Embodiment 1 is:
  • a preparation method for efficiently preparing magnesium hydroxide comprising the following steps:
  • the magnesium oxide slurry is added to the reactor 3 through a pump, the steam generator 9 is turned on, steam is introduced into the reactor 3, the reactor 3 is heated, and the pressure of the pressure control linkage unit is controlled to be 0.2 to 0.3 MPa, and the pressure is controlled.
  • the pressure of the linkage unit II 4 is 0.2 to 0.3 MPa
  • the pressure of the pressure control linkage unit ⁇ 8 is 0.2 to 0.3 MPa
  • the reaction temperature is raised to 90 to 120 ° C
  • the liquid in the reaction is returned from the two-position three-way valve second interface 62 to the mixture.
  • the tank 1 is returned to the reactor 3 by the mixing tank 1 to form a circulation loop, and the circulation flow rate is 3.1 L/min;
  • the second port 3 of the three-way valve is closed, the third port 63 of the three-way valve is opened, and the liquid after the reaction is added to the storage tank 7.
  • Embodiment 1 The difference from Embodiment 1 is:
  • a preparation method for efficiently preparing magnesium hydroxide comprising the following steps:
  • the magnesium oxide slurry is added to the reactor 3 through a pump, the steam generator 9 is turned on, steam is introduced into the reactor 3, the reactor 3 is heated, and the pressure of the pressure control linkage unit is controlled to be 0.3 to 0.5 MPa, and the pressure is controlled.
  • the pressure of the linkage unit II 4 is 0.3 ⁇ 0.5MPa
  • the pressure of the pressure control linkage unit ⁇ 8 is 0.3 ⁇ 0.5MPa
  • the reaction temperature is raised to 120 ⁇ 150°C
  • the liquid in the reaction is returned from the two-position three-way valve second interface 62 to the mixing.
  • Tank 1 and then mix The tank 1 is returned to the reactor 3 to form a circulation loop, and the circulation flow rate is 2.75 L/min;
  • the second port 3 of the three-way valve is closed, the third port 63 of the three-way valve is opened, and the liquid after the reaction is added to the storage tank 7.
  • the reaction conversion rate tends to be stable at lOmin, and the reaction conversion rate changes little with time after lOmin;
  • the experiment of the present invention was compared using a cup and can experiment
  • the conversion conversion rate of magnesium oxide is only 77.7%.
  • the preparation method of the present invention obtains a reaction conversion rate of more than 80% at the same reaction temperature and 10 minutes after the reaction.
  • the present invention has a significant advantage of being fast and efficient, and at the same time, the apparatus of the present invention has a much smaller footprint than the conventional apparatus due to the shortened reaction rate.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Inorganic Chemistry (AREA)
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  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

本发明涉及一种高效制备氢氧化镁的装置，包括混料罐、压力控制联动单元Ⅰ、反应器、压力控制联动单元Ⅱ、冷凝器、两位三通阀、储料罐、压力控制联动单元Ⅲ、蒸汽发生器，所述混料罐出料口与压力控制联动单元Ⅰ一端通过泵连接，压力控制联动单元Ⅰ另一端与反应器进料口连接，反应器出料口与压力控制联动单元Ⅱ一端连接，压力控制联动单元Ⅱ另一端与冷凝器一端连接，冷凝器另一端与两位三通阀第一接口连接，两位三通阀第二接口与混料罐返料口连接，两位三通阀第三接口与储料罐连接，反应器蒸汽入口与压力控制联动单元Ⅲ一端连接，压力控制联动单元Ⅲ另一端与蒸汽发生器连接，本发明有益效果为高效快速的制备氢氧化镁浆料。

Description

一种高效制备氢氧化镁的制备方法及装置 技术领域
本发明涉及一种高效制备氢氧化镁的制备方法及装置。 背景技术
氢氧化镁作为一种绿色材料， 被广泛应用于防火材料、 农业、 环保方面。 工业上 获得氢氧化镁的方式通常为 5种： 1、 用石灰石和卤水反应生产氢氧化镁； 2、 用氢氧 化钠和卤水、 卤块反应制氢氧化镁； 3、 利用煅烧过的菱镁矿、 白云石和卤水、 卤块反 应生产氢氧化镁； 4、 用氨水和卤水、 卤块反应制氢氧化镁； 5、 利用氧化镁水化生成 氢氧化镁， 这里的氧化镁必须是轻烧产品以保证水化的活性。 最常用的是采用水化轻 烧氧化镁的方式获取氢氧化镁， 水化通常都是在搅拌的条件下完成的， 水化的条件基 本为： 水化温度 30〜60°C ; 氧化镁浆液浓度 5〜20% (w/w); 水化时间 l〜24h， 水化 率 60〜80%。
综上所述，氧化镁水化制备氢氧化镁技术领域存在的问题： 由于较长的停留时间， 传统的氧化镁水化制备氢氧化镁均为间歇式工艺、 反应容器的体积较大、 水化效率不 高、 水化率较低。 发明内容
本发明通过控制压力与温度， 使氧化镁与水蒸汽反应， 达到稳定、 高效制备氢氧 化镁浆料的目的。
本发明提供了一种高效制备氢氧化镁的装置，包括混料罐、压力控制联动单元 I、 反应器、 压力控制联动单元 II、 冷凝器、 两位三通阀、 储料罐、 压力控制联动单元 III、 蒸汽发生器， 所述混料罐出料口与压力控制联动单元 I一端通过泵连接， 压力控制联 动单元 I另一端与反应器进料口连接，反应器出料口与压力控制联动单元 II一端连接， 压力控制联动单元 II另一端与冷凝器一端连接， 冷凝器另一端与两位三通阀第一接口 连接，两位三通阀第二接口与混料罐返料口连接，两位三通阀第三接口与储料罐连接， 反应器蒸汽入口与压力控制联动单元 III一端连接， 压力控制联动单元 III另一端与蒸汽 发生器连接。
本发明所述压力控制联动单元优选为由压力传感器和电磁阀组成。
现有技术中水分子吸附到氧化镁颗粒表面， 反应形成的氢氧化镁覆盖在氧化镁颗 粒表面上， 阻碍了进一步水化反应的进行， 本发明所述的装置制备氢氧化镁时， 高压 蒸汽直接与固体接触， 发生气固反应，氧化镁颗粒表面上生成的氢氧化镁被迅速剥离， 氧化镁颗粒持续被水化， 冷却后得到氢氧化镁浆料。
本发明另一目的提供了一种高效制备氢氧化镁的制备方法， 所述方法包括如下步 骤：
①将氧化镁与水加入到混料罐中混匀， 得到氧化镁浆液；
所述氧化镁占总重量的 5〜15%；
②将氧化镁浆液通过泵加入到反应器中， 开启蒸汽发生器，往反应器中通入蒸汽， 加热反应器， 控制压力控制联动单元 I压力为 0.2〜0.5MPa、 压力控制联动单元 II压 力为 0.2〜0.5MPa、压力控制联动单元 III压力为 0.2〜0.5MPa， 反应温度为 90〜150°C， 将反应中液体由两位三通阀第二接口返回到混料罐， 再由混料罐返回到反应器中构成 循环回路；
③循环 10〜35min后关闭两位三通阀第二接口， 开启两位三通阀第三接口， 将反 应后液体加入到储料罐。
本发明所述步骤②为通过压力控制联动单元 I控制进料压力， 蒸汽发生器产生的 蒸汽通过压力控制联动单元 III与氧化镁浆料反应， 通过压力控制联动单元 II控制反应 时的水击现象带来的压力剧烈变化。
本发明所述氧化镁优选为占总重量的 15%。
本发明所述压力控制联动单元 I压力优选为 0.3〜0.5MPa。
本发明所述压力控制联动单元 II压力优选为 0.3〜0.5MPa。
本发明所述压力控制联动单元 III压力优选为 0.3〜0.5MPa。
本发明所述反应温度优选为 120〜150°C。
上述优选氧化镁的比例、 压力控制联动单元 I压力、 压力控制联动单元 II压力、 压力控制联动单元 III压力和反应温度使氢氧化镁反应转化率达到 90%以上。
本发明有益效果为：
①提高制备氢氧化镁的反应速率；
②提高制备氢氧化镁的反应转化率；
③极大缩小了反应器的体积。 附图说明
本发明附图 1幅， 图 1为高效制备氢氧化镁装置的结构示意图；
其中， 1、 混料罐， 11、 混料罐出料口， 12、 混料罐返料口， 2、 压力控制联动单 元 I， 3、 反应器， 31、 反应器进料口， 32、 反应器出料口， 33、 反应器蒸汽入口， 4、 压力控制联动单元 II， 5、 冷凝器， 6、 两位三通阀， 61、 两位三通阀第一接口， 62、 两位三通阀第二接口， 63、 两位三通阀第三接口， 7、 储料罐， 8、 压力控制联动单元 III， 9、 蒸汽发生器。 具体实施方式
下述非限制性实施例可以使本领域的普通技术人员更全面地理解本发明， 但不以 任何方式限制本发明。 实施例 1
一种高效制备氢氧化镁的装置， 包括混料罐 1、压力控制联动单元 1 2、 反应器 3、 压力控制联动单元 114、 冷凝器 5、 两位三通阀 6、 储料罐 7、 压力控制联动单元 1118、 蒸汽发生器 9，所述混料罐出料口 11与压力控制联动单元 I 2—端通过压力水泵连接， 压力控制联动单元 I 2另一端与反应器进料口 31连接， 反应器出料口 32与压力控制 联动单元 Π 4—端连接， 压力控制联动单元 Π4另一端与冷凝器 5—端连接， 冷凝器 5 另一端与两位三通阀第一接口 61连接， 两位三通阀第二接口 62与混料罐返料口 12 连接， 两位三通阀第三接口 63与储料罐 7连接， 反应器蒸汽入口 33与压力控制联动 单元 ΙΠ8—端连接， 压力控制联动单元 ΙΠ8另一端与蒸汽发生器 9连接，所述压力控制 联动单元由压力传感器和电磁阀组成。
一种高效制备氢氧化镁的制备方法， 所述方法包括如下步骤：
①将氧化镁与水加入到混料罐 1 中混匀， 所述氧化镁占总重量的 5%， 得到氧化 镁浆液；
②将氧化镁浆液通过泵加入到反应器 3中， 开启蒸汽发生器 9， 往反应器 3中通 入蒸汽， 加热反应器 3， 控制压力控制联动单元 1 2压力为 0.2〜0.3MPa、 压力控制联 动单元 II 4压力为 0.2〜0.3MPa、 压力控制联动单元 ΙΠ8压力为 0.2〜0.3MPa， 反应温 度升至 90〜120°C， 将反应中液体由两位三通阀第二接口 62返回到混料罐 1， 再由混 料罐 1返回到反应器 3中构成循环回路， 循环流量为 1.95L/min;
③循环 35min后关闭两位三通阀第二接口 62，开启两位三通阀第三接口 63，将反 应后液体加入到储料罐 7。 实施例 1的实验结果见表 1 :
表 1实施例 1的水化率
Figure imgf000006_0001
实施例 2
与实施例 1区别在于：
一种高效制备氢氧化镁的制备方法， 所述方法包括如下步骤：
①将氧化镁与水加入到混料罐 1 中混匀， 所述氧化镁占总重量的 5%， 得到氧化 镁浆液；
②将氧化镁浆液通过泵加入到反应器 3中， 开启蒸汽发生器 9， 往反应器 3中通 入蒸汽， 加热反应器 3， 控制压力控制联动单元 1 2压力为 0.3〜0.5MPa、 压力控制联 动单元 II 4压力为 0.3〜0.5MPa、 压力控制联动单元 ΙΠ8压力为 0.3〜0.5MPa， 反应温 度升至 120〜150°C，将反应中液体由两位三通阀第二接口 62返回到混料罐 1，再由混 料罐 1返回到反应器 3中构成循环回路， 循环流量为 1.55L/min;
③循环 35min后关闭两位三通阀第二接口 62，开启两位三通阀第三接口 63，将反 应后液体加入到储料罐 7。
实施例 2的实验结果见表 2:
表 2实施例 2的水化率
Figure imgf000006_0002
实施例 3
与实施例 1区别在于：
一种高效制备氢氧化镁的制备方法， 所述方法包括如下步骤：
①将氧化镁与水加入到混料罐 1中混匀， 所述氧化镁占总重量的 10%， 得到氧化 镁浆液； ②将氧化镁浆液通过泵加入到反应器 3中， 开启蒸汽发生器 9， 往反应器 3中通 入蒸汽， 加热反应器 3， 控制压力控制联动单元 1 2压力为 0.2〜0.3MPa、 压力控制联 动单元 II 4压力为 0.2〜0.3MPa、 压力控制联动单元 ΙΠ8压力为 0.2〜0.3MPa， 反应温 度升至 90〜120°C， 将反应中液体由两位三通阀第二接口 62返回到混料罐 1， 再由混 料罐 1返回到反应器 3中构成循环回路， 循环流量为 1.2L/min;
③循环 35min后关闭两位三通阀第二接口 62，开启两位三通阀第三接口 63，将反 应后液体加入到储料罐 7。
实施例 3的实验结果见表 3:
表 3实施例 3的水化率
Figure imgf000007_0001
实施例 4
与实施例 1区别在于：
一种高效制备氢氧化镁的制备方法， 所述方法包括如下步骤：
①将氧化镁与水加入到混料罐 1中混匀， 所述氧化镁占总重量的 10%， 得到氧化 镁浆液；
②将氧化镁浆液通过泵加入到反应器 3中， 开启蒸汽发生器 9， 往反应器 3中通 入蒸汽， 加热反应器 3， 控制压力控制联动单元 1 2压力为 0.3〜0.5MPa、 压力控制联 动单元 II 4压力为 0.3〜0.5MPa、 压力控制联动单元 ΙΠ8压力为 0.3〜0.5MPa， 反应温 度升至 120〜150°C，将反应中液体由两位三通阀第二接口 62返回到混料罐 1，再由混 料罐 1返回到反应器 3中构成循环回路， 循环流量为 2.9L/min;
③循环 35min后关闭两位三通阀第二接口 62，开启两位三通阀第三接口 63，将反 应后液体加入到储料罐 7。
实施例 4的实验结果见表 4:
表 4实施例 4的水化率
反应时间 （min)
10 15 20 25 30 35 水化率 （％) 83.7 82.6 84.7 83.4 84.9 82.1
实施例 5
与实施例 1区别在于：
一种高效制备氢氧化镁的制备方法， 所述方法包括如下步骤：
①将氧化镁与水加入到混料罐 1中混匀， 所述氧化镁占总重量的 15%， 得到氧化 镁浆液；
②将氧化镁浆液通过泵加入到反应器 3中， 开启蒸汽发生器 9， 往反应器 3中通 入蒸汽， 加热反应器 3， 控制压力控制联动单元 1 2压力为 0.2〜0.3MPa、 压力控制联 动单元 II 4压力为 0.2〜0.3MPa、 压力控制联动单元 ΙΠ8压力为 0.2〜0.3MPa， 反应温 度升至 90〜120°C， 将反应中液体由两位三通阀第二接口 62返回到混料罐 1， 再由混 料罐 1返回到反应器 3中构成循环回路， 循环流量为 3.1L/min;
③循环 35min后关闭两位三通阀第二接口 62，开启两位三通阀第三接口 63，将反 应后液体加入到储料罐 7。
实施例 5的实验结果见表 5:
表 5实施例 5的水化率
Figure imgf000008_0001
实施例 6
与实施例 1区别在于：
一种高效制备氢氧化镁的制备方法， 所述方法包括如下步骤：
①将氧化镁与水加入到混料罐 1中混匀， 所述氧化镁占总重量的 15%， 得到氧化 镁浆液；
②将氧化镁浆液通过泵加入到反应器 3中， 开启蒸汽发生器 9， 往反应器 3中通 入蒸汽， 加热反应器 3， 控制压力控制联动单元 1 2压力为 0.3〜0.5MPa、 压力控制联 动单元 II 4压力为 0.3〜0.5MPa、 压力控制联动单元 ΙΠ8压力为 0.3〜0.5MPa， 反应温 度升至 120〜150°C，将反应中液体由两位三通阀第二接口 62返回到混料罐 1，再由混 料罐 1返回到反应器 3中构成循环回路， 循环流量为 2.75L/min;
③循环 35min后关闭两位三通阀第二接口 62，开启两位三通阀第三接口 63，将反 应后液体加入到储料罐 7。
实施例 6的实验结果见表 6:
表 6实施例 6的水化率
Figure imgf000009_0001
实验结论：
①采用本发明所述制备氢氧化镁的方法， lOmin 时反应转化率趋于稳定， lOmin 后反应转化率随时间变化较小；
②氧化镁质量百分浓度为 10〜15%时， lOmin时反应转化率达到 80〜90%。
对比例 1
采用杯罐实验对比本发明实验；
对比例 1的实验条件见表 7。
表 7对比例 1的实验条件
Figure imgf000009_0002
对比例 1的实验结果见表 8。
表 8对比例 1的实验结论
Figure imgf000009_0003
结论： 杯罐实验的水化时间为 120min时， 氧化镁的反应转化率仅为 77.7%， 本发 明所述的制备方法在相同反应温度下，反应 lOmin获得 80%以上的反应转化率，因此， 与传统方法相比， 本发明具有快速、 高效的显著优势， 同时由于反应速率缩短， 使本 发明所述装置较传统装置占地面积极大减小。

Claims

权 利 要 求 书
1、 一种高效制备氢氧化镁的装置， 包括混料罐 （1 )、 压力控制联动单元 I (2)、 反应器 （3)、 压力控制联动单元 II (4)、 冷凝器 （5)、 两位三通阀 （6)、 储料罐 （7)、 压力控制联动单元 III (8)、 蒸汽发生器 （9)， 所述混料罐出料口 （11 ) 与压力控制联 动单元 I (2)—端通过泵连接，压力控制联动单元 I (2)另一端与反应器进料口（31 ) 连接， 反应器出料口 （32) 与压力控制联动单元 II (4)一端连接， 压力控制联动单元 II (4)另一端与冷凝器（5)—端连接，冷凝器（5)另一端与两位三通阀第一接口（61 ) 连接， 两位三通阀第二接口 （62) 与混料罐返料口 （12) 连接， 两位三通阀第三接口
(63) 与储料罐 （7) 连接， 反应器蒸汽入口 （33) 与压力控制联动单元 III (8) 一端 连接， 压力控制联动单元 III (8) 另一端与蒸汽发生器 （9) 连接。
2、根据权利要求 1所述的装置， 其特征在于： 所述压力控制联动单元由压力传感 器和电磁阀组成。
3、 一种高效制备氢氧化镁的制备方法， 其特征在于： 所述方法包括如下步骤：
①将氧化镁与水加入到混料罐 （1 ) 中混匀， 得到氧化镁浆液；
所述氧化镁占总重量的 5〜15%；
②将氧化镁浆液通过泵加入到反应器（3)中，开启蒸汽发生器（9)，往反应器（3) 中通入蒸汽， 加热反应器 （3)， 控制压力控制联动单元 I (2) 压力为 0.2〜0.5MPa、 压力控制联动单元 II (4)压力为 0.2〜0.5MPa、压力控制联动单元 III (8)压力为 0.2〜 0.5MPa, 反应温度为 90〜150°C， 将反应中液体由两位三通阀第二接口 （62) 返回到 混料罐 （1 )， 再由混料罐 （1 ) 返回到反应器 （3) 中构成循环回路；
③循环 10〜35min 后关闭两位三通阀第二接口 （62)， 开启两位三通阀第三接口 (63), 将反应后液体加入到储料罐 （7)。
4、 根据权利要求 3所述的制备方法， 其特征在于： 所述氧化镁占总重量的 15%。
5、 根据权利要求 3所述的制备方法， 其特征在于： 所述压力控制联动单元 I (2) 压力为 0.3〜0.5MPa。
6、 根据权利要求 3所述的制备方法， 其特征在于： 所述压力控制联动单元 II (4) 压力为 0.3〜0.5MPa。
7、 根据权利要求 3所述的制备方法， 其特征在于： 所述压力控制联动单元 III (8) 压力为 0.3〜0.5MPa。
8、 根据权利要求 3所述的制备方法， 其特征在于： 所述反应温度为 120〜150°C。
PCT/CN2013/080196 2013-06-19 2013-07-26 一种高效制备氢氧化镁的制备方法及装置 Ceased WO2014201752A1 (zh)

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