CN111517341A - Water-saving and efficient washing method and device for reducing chloride content in magnesium carbonate - Google Patents

Water-saving and efficient washing method and device for reducing chloride content in magnesium carbonate Download PDF

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CN111517341A
CN111517341A CN202010527384.8A CN202010527384A CN111517341A CN 111517341 A CN111517341 A CN 111517341A CN 202010527384 A CN202010527384 A CN 202010527384A CN 111517341 A CN111517341 A CN 111517341A
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washing
water
magnesium carbonate
slurry
washing tank
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尹全义
邢煊
翟立强
孙孟勇
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Hebei Meishen Technology Co ltd
Hebei Xingtai Metallurgical Magnesium Industry Co ltd
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Hebei Meishen Technology Co ltd
Hebei Xingtai Metallurgical Magnesium Industry Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00Compounds of magnesium
    • C01F5/24Magnesium carbonates

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Abstract

The invention discloses a water-saving and efficient washing method and device for reducing chloride content in magnesium carbonate, and relates to the technical field of chemical impurity removal; the method comprises the following steps: the method comprises the following steps: mixing and washing raw materials; step two: mixing and washing magnesium carbonate; step three: solid-liquid separation and drying are carried out, and after filtrate is collected, the filtrate is used as water for size mixing in the synthesis reaction: the invention can ensure that chloride ions can be fully contacted with water and dissolved in the water, thereby improving the washing effect and effectively reducing the chloride content; the slurry is circularly washed by the ultrasonic, so that the slurry is thoroughly and fully washed, the power of ultrasonic equipment is reduced, and the energy consumption is effectively reduced; the washing water and the filtrate are recycled, and the washing water is recycled after ion exchange, so that the water consumption is greatly reduced, and the environment is protected.

Description

降低碳酸镁中氯化物含量的节水高效的洗涤方法及装置Water-saving and efficient washing method and device for reducing chloride content in magnesium carbonate

技术领域technical field

本发明属于化工除杂技术领域,具体涉及一种降低碳酸镁中氯化物含量的节水高效的洗涤方法及装置。The invention belongs to the technical field of chemical impurity removal, and in particular relates to a water-saving and efficient washing method and device for reducing chloride content in magnesium carbonate.

背景技术Background technique

化学法合成碳酸镁时,使用的原料中或多或少都夹带杂质氯离子,这对碳酸镁的应用影响很大,甚至限制了在一些尖端精密行业的使用,为此必须在生产过程中予以除去。目前,主要是采用水洗脱除的方法,此种方法效率低、效果不甚良好,而且耗水量巨大,造成水资源浪费。When chemically synthesizing magnesium carbonate, the raw materials used contain more or less impurity chloride ions, which has a great impact on the application of magnesium carbonate, and even limits the use in some cutting-edge precision industries. remove. At present, the method of water elution is mainly used, which has low efficiency, poor effect, and huge water consumption, resulting in waste of water resources.

发明内容SUMMARY OF THE INVENTION

为解决现有采用水洗脱除的方法效率低、效果不甚良好,而且耗水量巨大,造成水资源浪费的技术的问题;本发明的目的在于提供一种降低碳酸镁中氯化物含量的节水高效的洗涤方法及装置。In order to solve the technical problem that the existing method of using water elution is low in efficiency, not very good in effect, huge in water consumption, and causes waste of water resources; the object of the present invention is to provide a water-saving method that reduces chloride content in magnesium carbonate Efficient washing method and device.

本发明的降低碳酸镁中氯化物含量的节水高效的洗涤方法,它的方法如下:The water-saving and efficient washing method that reduces chloride content in the magnesium carbonate of the present invention, its method is as follows:

步骤一:原料的调浆、洗涤:Step 1: Sizing and washing of raw materials:

将生产碳酸镁的原料和水按照一定的比例调浆、混合,浓度控制为5-50g/L,开启加热装置,控制浆液温度在40-90℃,开启搅拌和循环装置,搅拌30-150min;搅拌结束后,采用离心脱水或板框压滤机设备对浆液进行固液分离;将分离出的半固体原料,输送至合成反应釜中;滤液收集后经离子交换树脂处理,用于再次洗涤;The raw materials for producing magnesium carbonate and water are slurried and mixed according to a certain proportion, the concentration is controlled to 5-50g/L, the heating device is turned on, the temperature of the slurry is controlled at 40-90°C, the stirring and circulation device is turned on, and the stirring is 30-150min; After the stirring, centrifugal dehydration or plate and frame filter press equipment is used to separate the slurry from solid and liquid; the separated semi-solid raw materials are transported to the synthesis reactor; the filtrate is collected and treated with ion exchange resin for washing again;

步骤二:碳酸镁的调浆、洗涤:Step 2: Sizing and washing of magnesium carbonate:

碳酸镁合成结束后,进行固液分离,滤液收集后经离子交换树脂处理,用于再次洗涤;After the synthesis of magnesium carbonate, solid-liquid separation is carried out, and the filtrate is collected and processed by ion exchange resin for washing again;

将分离出的碳酸镁转移至洗涤罐中,加适量水调浆,控制浆液浓度为5-50g/L;开启加热装置,控制浆液温度在40-90℃,开启循环装置,在循环泵的作用下,使浆液在两个洗涤罐内循环,调整循环泵的参数和流量调节阀,控制流量为5-10m³/h,保持浆液充满洗涤罐二;开启洗涤罐二中的超声装置,调整超声频率及功率至额定功率的60%-95%;洗涤20-100min后结束;Transfer the separated magnesium carbonate to the washing tank, add an appropriate amount of water to adjust the slurry, and control the concentration of the slurry to be 5-50g/L; turn on the heating device, control the temperature of the slurry to be 40-90 °C, and open the circulation device. Then, make the slurry circulate in the two washing tanks, adjust the parameters of the circulating pump and the flow control valve, control the flow rate to 5-10m³/h, and keep the slurry full of the second washing tank; open the ultrasonic device in the second washing tank, adjust the ultrasonic frequency And the power reaches 60%-95% of the rated power; the washing ends after 20-100min;

步骤三:固液分离、干燥:Step 3: Solid-liquid separation and drying:

结束洗涤后,对浆液进行固液分离,干燥分离后的碳酸镁即得产品;滤液收集后,作为合成反应中调浆用水。After washing, the slurry is subjected to solid-liquid separation, and the separated magnesium carbonate is dried to obtain a product; after the filtrate is collected, it is used as water for slurrying in the synthesis reaction.

作为优选,所述步骤二中两次固液分离的水混合后温度为40-90℃。Preferably, in the second step, the temperature of the water after the two solid-liquid separations is mixed is 40-90°C.

作为优选,所述两个洗涤罐为一大一小,均内置搅拌装置。Preferably, the two washing tanks are one large and one small, and both have built-in stirring devices.

作为优选,所述洗涤罐二中安装有超声装置,以较小的设备功率和设备投入,满足洗涤要求。Preferably, an ultrasonic device is installed in the second washing tank, which meets the washing requirements with less equipment power and equipment investment.

一种降低碳酸镁中氯化物含量的节水高效的洗涤装置,包括洗涤罐一、洗涤罐二、搅拌装置、超声装置、循环泵、回流管道、加热装置、流量调节阀;洗涤罐一的右下端通过管道与洗涤罐二的上侧连接,且管道上安装有循环泵5,洗涤罐一内安装有搅拌装置、加热装置,洗涤罐二的底部通过回流管道与洗涤罐一的上侧连接,回流管道上设有流量调节阀,洗涤罐二的内部安装有超声装置,洗涤罐一依次与脱水设备、离子交换设备、收集池相连,形成水循环通路。A water-saving and efficient washing device for reducing chloride content in magnesium carbonate, comprising a washing tank 1, a washing tank 2, a stirring device, an ultrasonic device, a circulating pump, a return pipeline, a heating device, and a flow regulating valve; The lower end is connected with the upper side of the second washing tank through a pipeline, and a circulating pump 5 is installed on the pipeline. A stirring device and a heating device are installed in the first washing tank, and the bottom of the second washing tank is connected with the upper side of the washing tank 1 through a return pipeline. A flow regulating valve is arranged on the return pipeline, an ultrasonic device is installed inside the second washing tank, and the first washing tank is connected with the dehydration equipment, the ion exchange equipment and the collecting tank in sequence to form a water circulation path.

与现有技术相比,本发明的有益效果为:Compared with the prior art, the beneficial effects of the present invention are:

一、能够使氯离子能够充分与水接触,并溶解于水中,提高洗涤效果,降低氯化物含量;1. It can make chloride ions fully contact with water and dissolve in water to improve washing effect and reduce chloride content;

二、浆液循环经过超声洗涤,有效的降低了能耗和减少设备投入;2. The slurry circulation is ultrasonically washed, which effectively reduces energy consumption and equipment investment;

三、可将洗涤和生产反应操作合二为一,不增加劳动量和生产周期,效率高;3. Washing and production reaction operations can be combined into one, without increasing labor and production cycle, and high efficiency;

四、调浆水、洗涤水反复循环利用,大大降低了生产用水消耗,同时基本无废水排放,保护环境。4. The sizing water and washing water are recycled and reused, which greatly reduces the consumption of production water, and at the same time, there is basically no waste water discharge, which protects the environment.

附图说明Description of drawings

为了易于说明,本发明由下述的具体实施及附图作以详细描述。For ease of description, the present invention is described in detail by the following specific implementations and accompanying drawings.

图1为本发明的结构示意图。FIG. 1 is a schematic structural diagram of the present invention.

图中: 1-洗涤罐一;2-洗涤罐二;3-搅拌装置;4-超声装置;5-循环泵;6-回流管道;7-加热装置;8-流量调节阀;9-脱水设备;10-离子交换设备;11-收集池。In the figure: 1-washing tank one; 2-washing tank two; 3-stirring device; 4-ultrasonic device; 5-circulating pump; 6-return pipeline; 7-heating device; 8-flow regulating valve; 9-dehydration equipment ; 10-ion exchange equipment; 11-collection pool.

具体实施方式Detailed ways

为使本发明的目的、技术方案和优点更加清楚明了,下面通过附图中示出的具体实施例来描述本发明。但是应该理解,这些描述只是示例性的,而并非要限制本发明的范围。此外,在以下说明中,省略了对公知结构和技术的描述,以避免不必要地混淆本发明的概念。In order to make the objectives, technical solutions and advantages of the present invention clearer, the present invention will be described below through the specific embodiments shown in the accompanying drawings. It should be understood, however, that these descriptions are exemplary only, and are not intended to limit the scope of the present invention. Also, in the following description, descriptions of well-known structures and techniques are omitted to avoid unnecessarily obscuring the concepts of the present invention.

在此,还需要说明的是,为了避免因不必要的细节而模糊了本发明,在附图中仅仅示出了与根据本发明的方案密切相关的结构和/或处理步骤,而省略了与本发明关系不大的其他细节。Here, it should also be noted that, in order to avoid obscuring the present invention due to unnecessary details, only the structures and/or processing steps closely related to the solution according to the present invention are shown in the drawings, and the related structures and/or processing steps are omitted. Other details not relevant to the invention.

如图1所示,本具体实施方式采用以下技术方案:它的洗涤方法如下:As shown in Figure 1, this specific embodiment adopts the following technical solutions: its washing method is as follows:

步骤一:原料的调浆、洗涤:Step 1: Sizing and washing of raw materials:

将生产碳酸镁的原料和水按照一定的比例调浆、混合,浓度控制为5-50g/L,开启加热装置,控制浆液温度在40-90℃,开启搅拌和循环装置,搅拌30-150min;搅拌结束后,采用离心脱水或板框压滤机设备等对浆液进行固液分离;将分离出的半固体原料,输送至合成反应釜中;滤液收集后经离子交换树脂处理,用于再次洗涤;The raw materials for producing magnesium carbonate and water are slurried and mixed according to a certain proportion, the concentration is controlled to 5-50g/L, the heating device is turned on, the temperature of the slurry is controlled at 40-90°C, the stirring and circulation device is turned on, and the stirring is 30-150min; After stirring, use centrifugal dehydration or plate and frame filter press equipment to separate the slurry from solid and liquid; the separated semi-solid raw materials are transported to the synthesis reactor; after the filtrate is collected, it is treated with ion exchange resin for washing again. ;

这一步的洗涤中,能有效降低原料中的氯离子含量,从而降低在反应过程中结合到晶体内的氯离子的比例,减小洗涤难度;In this step of washing, the chloride ion content in the raw material can be effectively reduced, thereby reducing the proportion of chloride ions bound to the crystal during the reaction process, and reducing the difficulty of washing;

步骤二:碳酸镁的调浆、洗涤:Step 2: Sizing and washing of magnesium carbonate:

碳酸镁合成结束后,进行固液分离,滤液收集后经离子交换树脂处理,用于再次洗涤;After the synthesis of magnesium carbonate, solid-liquid separation is carried out, and the filtrate is collected and processed by ion exchange resin for washing again;

将分离出的碳酸镁转移至洗涤罐中,加适量水调浆,控制浆液浓度为5-50g/L;开启加热装置,控制浆液温度在40-90℃,开启循环装置,在循环泵的作用下,使浆液在两个洗涤罐内循环,调整循环泵的参数和流量调节阀,控制流量为5-10m³/h,保持浆液充满洗涤罐二;开启洗涤罐二中的超声装置,调整超声频率及功率至额定功率的60%-95%;洗涤20-100min后结束;Transfer the separated magnesium carbonate to the washing tank, add an appropriate amount of water to adjust the slurry, and control the concentration of the slurry to be 5-50g/L; turn on the heating device, control the temperature of the slurry to be 40-90 °C, and open the circulation device. Then, make the slurry circulate in the two washing tanks, adjust the parameters of the circulating pump and the flow control valve, control the flow rate to 5-10m³/h, and keep the slurry full of the second washing tank; open the ultrasonic device in the second washing tank, adjust the ultrasonic frequency And the power reaches 60%-95% of the rated power; the washing ends after 20-100min;

步骤三:固液分离、干燥:Step 3: Solid-liquid separation and drying:

结束洗涤后,对浆液进行固液分离,干燥分离后的碳酸镁即得产品,滤液收集后,作为合成反应中调浆用水。After washing, the slurry is subjected to solid-liquid separation, and the separated magnesium carbonate is dried to obtain a product. After the filtrate is collected, it is used as water for slurrying in the synthesis reaction.

进一步的,所述步骤二中两次固液分离的水混合后温度为40-90℃。Further, in the second step, the temperature of the water after the two solid-liquid separations is mixed is 40-90°C.

如图1所示,降低碳酸镁中氯化物含量的节水高效的洗涤装置,包括洗涤罐一1、洗涤罐二2、搅拌装置3、超声装置4、循环泵5、回流管道6、加热装置7、流量调节阀8;洗涤罐一1的右下端通过管道与洗涤罐二2的上侧连接,且管道上安装有循环泵5,洗涤罐一1内安装有搅拌装置3、加热装置7,洗涤罐二2的底部通过回流管道6与洗涤罐一1的上侧连接,回流管道6上设有流量调节阀8,洗涤罐二2的内部安装有超声装置4,洗涤罐一1依次与脱水设备9、离子交换设备10、收集池11相连,形成水循环通路。As shown in Figure 1, the water-saving and efficient washing device for reducing chloride content in magnesium carbonate includes washing tank 1 1, washing tank 2 2, stirring device 3, ultrasonic device 4, circulating pump 5, return pipeline 6, heating device 7. Flow regulating valve 8; the lower right end of washing tank one 1 is connected to the upper side of washing tank two 2 through a pipeline, and a circulating pump 5 is installed on the pipeline, and a stirring device 3 and a heating device 7 are installed in washing tank one 1, The bottom of the washing tank two 2 is connected with the upper side of the washing tank one 1 through the return pipe 6, the return pipe 6 is provided with a flow regulating valve 8, and an ultrasonic device 4 is installed inside the washing tank two 2. The equipment 9, the ion exchange equipment 10, and the collection tank 11 are connected to form a water circulation path.

本具体实施方式中第2步中两次固液分离的水混合后温度约为40-90℃,事宜的温度,可以增大氯离子在水中的溶解度,提高洗涤效果,这对氯化物洗涤有较大帮助。In this specific embodiment, the temperature of the water after the two solid-liquid separations in the second step is about 40-90 ° C. The temperature of the matter can increase the solubility of chloride ions in water and improve the washing effect, which is beneficial to chloride washing. Great help.

第2步中所涉及的洗涤罐,分为一大一小两个部分,均内置搅拌装置。所不同的是,洗涤罐二小罐内设有超声装置,洗涤罐一、洗涤罐二之间设有循环泵和回流管。碳酸镁和水充分搅拌下,循环进入带有超声的洗涤罐二中,超声震荡使得碳酸镁晶体结构伸展或震动,氯离子能够充分与水接触,并溶解于水中,提高洗涤效果,降低氯化物含量。The washing tank involved in the second step is divided into two parts, one large and one small, and both have built-in stirring devices. The difference is that an ultrasonic device is arranged in the second small tank of the washing tank, and a circulating pump and a return pipe are arranged between the first washing tank and the second washing tank. Magnesium carbonate and water are fully stirred and circulated into the second washing tank with ultrasonic. Ultrasonic vibration makes the crystal structure of magnesium carbonate stretch or vibrate, and chloride ions can fully contact with water and dissolve in water to improve washing effect and reduce chloride. content.

第2步中,为减小超声设备的功率,在洗涤罐二进行部分浆液分次超声洗涤,浆液循环经过超声洗涤,有效的降低了能耗。In the second step, in order to reduce the power of the ultrasonic equipment, part of the slurry is ultrasonically washed in batches in the second washing tank, and the slurry is circulated through ultrasonic cleaning, which effectively reduces the energy consumption.

对于本领域技术人员而言,显然本发明不限于上述示范性实施例的细节,而且在不背离本发明的精神或基本特征的情况下,能够以其他的具体形式实现本发明。因此,无论从哪一点来看,均应将实施例看作是示范性的,而且是非限制性的,本发明的范围由所附权利要求而不是上述说明限定,因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。It will be apparent to those skilled in the art that the present invention is not limited to the details of the above-described exemplary embodiments, but that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments are to be regarded in all respects as illustrative and not restrictive, and the scope of the invention is to be defined by the appended claims rather than the foregoing description, which are therefore intended to fall within the scope of the claims. All changes within the meaning and scope of the equivalents of , are included in the present invention.

此外,应当理解,虽然本说明书按照实施方式加以描述,但并非每个实施方式仅包含一个独立的技术方案,说明书的这种叙述方式仅仅是为清楚起见,本领域技术人员应当将说明书作为一个整体,各实施例中的技术方案也可以经适当组合,形成本领域技术人员可以理解的其他实施方式。In addition, it should be understood that although this specification is described in terms of embodiments, not each embodiment only includes an independent technical solution, and this description in the specification is only for the sake of clarity, and those skilled in the art should take the specification as a whole , the technical solutions in each embodiment can also be appropriately combined to form other implementations that can be understood by those skilled in the art.

Claims (4)

1. The water-saving and efficient washing method for reducing the chloride content in magnesium carbonate is characterized in that: the method comprises the following steps:
the method comprises the following steps: mixing and washing raw materials:
mixing the raw material for producing magnesium carbonate and water according to a certain proportion, mixing, controlling the concentration to be 5-50g/L, starting a heating device, controlling the temperature of the slurry to be 40-90 ℃, starting a stirring and circulating device, and stirring for 30-150 min; after stirring, performing solid-liquid separation on the slurry by adopting centrifugal dehydration or plate-and-frame filter press equipment; conveying the separated semi-solid raw material to a synthesis reaction kettle; collecting the filtrate, treating with ion exchange resin, and washing again;
step two: slurry mixing and washing of magnesium carbonate:
after the synthesis of magnesium carbonate is finished, carrying out solid-liquid separation, collecting filtrate, treating the filtrate by ion exchange resin, and washing again;
transferring the separated magnesium carbonate into a washing tank, adding a proper amount of water to mix slurry, and controlling the concentration of the slurry to be 5-50 g/L; starting the heating device, controlling the temperature of the slurry to be 40-90 ℃, starting the circulating device, circulating the slurry in the two washing tanks under the action of the circulating pump, adjusting the parameters of the circulating pump and a flow regulating valve, controlling the flow to be 5-10m for carrying out the cultivation/h, and keeping the second washing tank full of the slurry; opening an ultrasonic device in the second washing tank, and adjusting the ultrasonic frequency and the power to 60% -95% of the rated power; washing for 20-100 min;
step three: solid-liquid separation and drying:
and after washing is finished, carrying out solid-liquid separation on the slurry, drying the separated magnesium carbonate to obtain a product, and collecting filtrate to be used as water for size mixing in the synthesis reaction.
2. The water-saving and efficient washing method for reducing the chloride content in magnesium carbonate according to claim 1, characterized in that: and in the second step, the temperature of the mixed water after the two solid-liquid separations is 40-90 ℃.
3. The water-saving and efficient washing method for reducing the chloride content in magnesium carbonate according to claim 1, characterized in that: the two washing tanks are respectively provided with a large stirring device and a small stirring device.
4. Reduce water conservation high efficiency washing device of chloride content in magnesium carbonate, its characterized in that: comprises a first washing tank, a second washing tank, a stirring device, a heating device, an ultrasonic device, a circulating pump and a backflow pipeline; the right lower end of the first washing tank is connected with the upper side of the second washing tank through a pipeline, a circulating pump is installed on the pipeline, a stirring device and a heating device are installed in the first washing tank, the bottom of the second washing tank is connected with the upper side of the first washing tank through a backflow pipeline, a flow regulating valve is arranged on the backflow pipeline, an ultrasonic device is installed inside the second washing tank, and the first washing tank is sequentially connected with a dewatering device, an ion exchange device and a collecting pool to form a water circulation passage.
CN202010527384.8A 2020-06-11 2020-06-11 Water-saving and efficient washing method and device for reducing chloride content in magnesium carbonate Pending CN111517341A (en)

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Application publication date: 20200811