WO2010148983A1 - 一种硝酸钠球形细颗粒的造粒方法 - Google Patents

一种硝酸钠球形细颗粒的造粒方法 Download PDF

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WO2010148983A1
WO2010148983A1 PCT/CN2010/074011 CN2010074011W WO2010148983A1 WO 2010148983 A1 WO2010148983 A1 WO 2010148983A1 CN 2010074011 W CN2010074011 W CN 2010074011W WO 2010148983 A1 WO2010148983 A1 WO 2010148983A1
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sodium nitrate
tower
spherical fine
fine particles
granulation
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PCT/CN2010/074011
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English (en)
French (fr)
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戴良玉
吴望发
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Dai Liangyu
Wu Wangfa
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Priority to US13/379,335 priority Critical patent/US8465680B2/en
Publication of WO2010148983A1 publication Critical patent/WO2010148983A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D9/00—Nitrates of sodium, potassium or alkali metals in general
    • C01D9/16—Purification
    • 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
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
    • B01J2/04—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops in a gaseous medium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D9/00—Nitrates of sodium, potassium or alkali metals in general
    • C01D9/18—Preparation in the form of shaped products, e.g. granules

Definitions

  • the present invention relates to a process for producing spherical fine particles of sodium nitrate.
  • CN1205125C provides a method for producing sodium nitrate particles, which is melted in industrial sodium nitrate and pumped into a high-position tank, and then ejected from the low-position prilling tower nozzle by the difference in position.
  • the small droplets are cooled into a granular body in contact with the air flowing in the counterflow process, and the water is reduced. Content, the purpose of improving the dispersion.
  • the spherical or ovoid droplets formed after ejecting from the nozzle will naturally deform during the falling process. Therefore, after cooling, the granules of all possible shapes are obtained, the shape of the particles is irregular, and the roundness of the product particles cannot be obtained. When it reaches 0.8 or more, the number of spherical particles is much lower than 80%, and its dispersibility needs to be further improved;
  • the sodium nitrate droplets have a large specific surface area and strong hygroscopicity, and the method uses a room temperature air having a large water content to cool the sodium nitrate droplets, so that the sodium nitrate particles absorb a large amount of water again;
  • the technique of dispersing droplets by reciprocating vibration can only keep the particle size of the sodium nitrate particles in the range of 0.3 to 3 mm, and the yield of the product of 0.5 mm to 1 mm is extremely low, and the particle size of the product particles cannot be obtained. Controlled below 0.5mm;
  • the granulation method can obtain sodium nitrate particles having a lower water content, a higher roundness, and a smaller particle size than the existing particles.
  • a granulation method for spherical fine particles of sodium nitrate comprising the following steps:
  • the dew point of the lyophilized high-pressure air is lower than that of the normal-temperature air, the use of the high-pressure air as the medium for cooling the sodium nitrate particles is advantageous for reducing the water content of the particles, and the dew point of the high-pressure air used in the step 2 is lowered.
  • the temperature is below -60 °C, the water content of the sodium nitrate particles is less than 0.05%; meanwhile, the method also passes lyophilized high-pressure air in a tangential direction to make the sodium nitrate particles spiral along the wall of the tower in the granulation tower. Decrease to obtain sodium nitrate particles with extremely high roundness.
  • the lyophilized high-pressure air pressure used in the step 2 is generally 0.005 to 5 MPa, and the temperature is usually selected to be normal temperature.
  • the molten industrial sodium nitrate liquid can also be fed directly into the atomizing device without the need for continuous production.
  • an air intake pipe is also disposed in the lower portion of the prilling tower, and the lyophilized high-pressure air from the bottom to the top is introduced into the prilling tower through the air intake pipe to extend the sodium nitrate.
  • the sodium nitrate granules are spirally moved in the granulating tower, the sodium nitrate granules with higher roundness are obtained.
  • the sodium nitrate granules are spirally moved in the granulating tower for about 5 minutes, at least 80% of the sodium nitrate granules are rounded. It reached 0.8 or more.
  • the high-pressure air entering the prilling tower from the lower intake pipe and the high-pressure air entering the prilling tower from the upper intake pipe are generated by the same freeze-drying air compressor, and the technical parameters such as pressure, temperature and dew point are exactly the same. .
  • Suitable atomizing devices in the present invention include, but are not limited to, rotary atomizers, pressure nozzle atomizers, and two-fluid nozzle atomizers well known to those skilled in the art.
  • rotary atomizers can produce fine particles.
  • the pressure nozzle atomizer and the two-fluid nozzle atomizer produce larger particles.
  • the particle size of the sodium nitrate droplet can be adjusted by the technical parameters such as the gas flow rate of the compressed air, the nozzle diameter and the nozzle rotation speed, so that the particle size is mainly distributed between 30 ⁇ m and 0.5 mm.
  • the atomization device uses high-pressure air atomization at a temperature of 280 to 310 ° C and a pressure of 0.9 to 1.0 MPa, and a preferential use temperature of 300 to 308 ° C and a pressure of 1.0 Mpa. High pressure air atomization.
  • the industrial sodium nitrate raw material in the step 1 is melted into a liquid by electric heating in a molten salt furnace, and the water contained in the raw material is evaporated and discharged.
  • a return pipe can be arranged between the high-level heat preservation buffer tank and the molten salt furnace to limit the liquid level in the high-position tank, realize continuous melting and continuous production, thereby reducing production cost and obtaining a more stable quality product.
  • the air in the tower and the sodium nitrate powder suspended therein are discharged from the air guiding pipe disposed at the lower part of the granulation tower, and then separated into a cyclone separator, and the obtained powder is collected and packaged by the outlet of the cyclone separator.
  • the air containing a very small amount of powdered sodium nitrate is introduced into the water absorption tank through the exhaust pipe and then discharged into the atmosphere.
  • the air guiding duct is located below the lower air intake pipe.
  • the method passes through the lyophilized high-pressure air in the tangential direction at the upper position of the granulation tower, and the sodium nitrate droplets spirally descend along the tower wall in the granulation tower, so that the roundness of the obtained sodium nitrate particles reaches 0.8.
  • the contact between the individual particles is point contact, and it is less likely to agglomerate than the product with insufficient roundness in the past, and the dispersibility is better;
  • An intake pipe is also arranged in the lower part of the prilling tower, and the lyophilized high-pressure air from the bottom to the top is introduced into the prilling tower through the intake pipe to extend the droplets of the sodium nitrate or the particles in the prilling tower. The time of exercise to obtain more rounded sodium nitrate particles;
  • the present invention introduces molten sodium nitrate into a high-level heat preservation buffer tank, and provides a return pipe between the high-position heat preservation buffer tank and the molten salt furnace.
  • the above structure is arranged such that the molten salt process and the atomization process are independently performed. To achieve continuous production of industry;
  • the lyophilized high pressure air is used to cool the sodium nitrate droplets, thereby reducing the water content of the obtained sodium nitrate granule product.
  • FIG. 1 is a schematic view showing a production process of an embodiment of the present invention
  • Figure 2 is a cumulative distribution curve of volume (weight) of sodium nitrate particles.
  • the industrial sodium nitrate raw material is melted into a liquid by electric heating in a molten salt furnace to evaporate water contained in the raw material.
  • the molten sodium nitrate liquid is introduced into a high-level heat preservation buffer tank by using a high-temperature pump in the molten salt furnace, and then sent to the atomizing device at the top of a granulation tower by using the difference, and atomized to a maximum particle diameter of 0.5 mm.
  • the gas used in the atomization device spray was high-pressure air having a temperature of 300 ° C and a pressure of 1.0 MPa to prevent the molten sodium nitrate from condensing upon spraying.
  • the upper and lower intake pipes are respectively arranged on the granulating tower, and the dew point obtained by the lyophilized air compressor is -80 ° C, and the normal temperature and high pressure air at a pressure of 1.0 MPa is respectively from the upper intake pipe and the lower portion at a flow ratio of 1:3.
  • the air is fed into the prilling tower, wherein the high-pressure air entering from the upper intake pipe enters the tower in a tangential direction, so that the sodium nitrate droplet entering from the top of the tower spirals down along the tower wall in the prilling tower, from the lower part
  • the high-pressure air entering the intake pipe enters the prilling tower from bottom to top, so that the time for each sodium nitrate particle to spiral in the prilling tower is kept at about 5 minutes.
  • the granulation tower is provided with an air guiding pipe which is arranged below the lower air inlet pipe, and the high-pressure air entering the tower and the sodium nitrate powder suspended therein are led out from the air guiding pipe provided at the lower part of the granulation tower, and then Into the cyclone separation, the separated powder is collected from the outlet of the cyclone, packaged to obtain the product; the air with a very small amount of powdered sodium nitrate is discharged through the exhaust pipe of the cyclone, introduced into the water absorption tank, and the rear Into the atmosphere.
  • the cooled spherical fine particles of sodium nitrate are collected at the bottom of the granulation tower and packaged to obtain a product.
  • the physical and chemical parameters of the sodium nitrate granule product are as follows:
  • the particle size of the particles having a particle diameter of less than 1 mm mm is 99.9%, and the sieve residue ratio is 0.01%, which is detected by a JL-1155 laser particle size tester;
  • the water content of the granules is determined by the Karl Fischer method, and the water content is 0.03%;

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Description

一种硝酸钠球形细颗粒的造粒方法 技术领域
本发明涉及硝酸钠球形细颗粒的制造方法。
背景技术
普通的工业硝酸钠（国家标准GB/T4553）为不规则非球形粉末结晶、水份含量高、易吸潮而结块、流散性差，不便于使用。为改善现有硝酸钠颗粒的上述特性，CN1205125C提供了一种硝酸钠颗粒的制造方法，将工业硝酸钠熔融后泵入高位槽内，而后利用位差从处于低位的造粒塔喷头喷出，并利用分散装置的上下、左右往复振动将其分散成较为均匀的小液滴，小液滴在造粒塔内下落过程中与逆流而上的空气接触而被冷却成颗粒状体，达到降低水份含量，改善流散性的目的。
但是，上述制造方法还存在如下的不足：
一、从喷头喷出后形成的球形或卵形小液滴会在下落过程中自然变形，因此，冷却后得到的是一切可能形状的颗粒状体，颗粒形状不规则，产品颗粒的圆度无法达到0.8以上，球形颗粒的数量远低于80%，其流散性有待于进一步改善；
二、硝酸钠液滴比表面积大，吸湿性强，而该方法使用含水量较大的常温空气冷却硝酸钠液滴，导致硝酸钠颗粒重又吸收大量的水份；
三、利用往复振动分散液滴的技术仅能将硝酸钠颗粒的粒径基本保持在0.3～3mm的范围内，0.5mm～1mm粒径产品的得率极低，更无法将产品颗粒的粒径控制在0.5mm以下；
四、不能连续生产。
发明内容
本发明的目的在于提供一种硝酸钠球形细颗粒的造粒方法，以解决现有技术中存在的上述问题。该造粒方法可得到较现有颗粒含水量更低、圆度更高和颗粒更小的硝酸钠颗粒。
本发明提供的技术方案如下：
一种硝酸钠球形细颗粒的造粒方法，包括以下步骤：
1）将工业硝酸钠在熔盐炉内熔融后，导入一高位保温缓冲槽，而后送至位于一造粒塔顶部的雾化装置，将其雾化成粒径主要分布的30µm～0.5mm之间的雾滴；
2）将经过冷冻干燥的高压空气从所述造粒塔的上部进气管位置沿切线方向进入塔内，使步骤1中获得的硝酸钠雾滴在造粒塔内沿塔壁作螺旋下降，使其进一步球形化，得到球形细颗粒状的硝酸钠；
3）收集位于造粒塔底的冷却硝酸钠球形细颗粒，包装获得产品。
本方法中，由于经过冷冻干燥的高压空气的露点较常温空气低，使用上述高压空气作为硝酸钠颗粒冷却的介质，有利于降低颗粒的含水量，在步骤2中所使用的高压空气的露点降至-60℃以下时，硝酸钠颗粒的含水量至0.05%以下；同时，该方法还沿切线方向通入冷冻干燥的高压空气，使硝酸钠颗料在造粒塔内沿塔壁作螺旋状下降，得到圆度极高的硝酸钠颗粒。另外，步骤2中所使用的经过冷冻干燥的高压空气压力一般为0.005～5MPa，温度通常选择常温。
当然，在不需要进行连续生产的情况下，也可以将熔融的工业硝酸钠液体直接送入到雾化装置中。
本发明的一较佳实施例中，所述造粒塔的下部也设置一进气管，并通过该进气管向造粒塔内导入从下往上的经过冷冻干燥的高压空气，以延长硝酸钠颗粒在造粒塔作螺旋运动的时间，获得圆度更高的硝酸钠颗粒，在硝酸钠颗粒在造粒塔内作螺旋运动的时间在5min左右时，至少有80%的硝酸钠颗粒圆度达到0.8以上。优选地，从下部进气管进入造粒塔内的高压空气与从所述上部进气管进入造粒塔内的高压空气由同一冷冻干燥空气压缩机产生，其压力、温度和露点等技术参数完全相同。
本发明中适合的雾化装置包括但不限于本领域普通技术人员公知的转轮雾化器、压力喷嘴雾化器和双流体喷嘴雾化器，通常，转轮雾化器可制备出细颗粒，而压力喷嘴雾化器和双流体喷嘴雾化器则制备出较大的颗粒。硝酸钠雾滴的粒径可通过压缩空气的气体流量、喷嘴口径和喷嘴转速等技术参数调整，使其粒径主要分布在30µm～0.5mm之间。
本发明的一较佳实施例中，所述的雾化装置使用温度为280～310℃、压力为0.9～1.0Mpa的高压空气雾化，更优先使用温度为300～308℃、压力为1.0Mpa的高压空气雾化。
本发明的一较佳实施例中，步骤1中的工业硝酸钠原料在一熔盐炉中通过电加热方式熔融成液体，原料中含有的水份则被蒸发和排出。在高位保温缓冲槽和熔盐炉之间可设置一条回流管，用以限制高位槽内的液位，实现连续熔融和连续生产，从而降低生产成本，并获得质量更加稳定的产品。
本发明的一较佳实施例中，塔内空气和悬浮在其中的硝酸钠粉末从造粒塔下部设置的引风管导出后进入旋风分离器分离，得到的粉末由旋风分离器出口收集包装，含有极少量粉状硝酸钠的空气则经由排风管引入水吸收槽吸收后，排入大气。所述的引风管位于所述下部进气管的下方。
除非特别指名，这里所使用的所有技术和科学术语的含义与本发明所属技术领域一般技术人员通常所理解的含义相同。同样，所有在此提及的出版物、专利申请、专利及其他参考资料均可以引入本发明作为参考。
综上，与现有技术相比，本发明的有益效果可列举如下：
1）该方法在造粒塔上部位置沿切线方向通入冷冻干燥的高压空气，硝酸钠雾滴在造粒塔内沿塔壁作螺旋状下降，使获得的硝酸钠颗粒的圆度大都达到0.8以上，各个颗粒之间的接触为点接触，相对于以往圆度不足的产品更不易结块，流散性更好；
2）造粒塔的下部也设置一进气管，并通过该进气管向造粒塔内导入从下往上的经过冷冻干燥的高压空气，以延长硝酸钠雾滴或颗粒在造粒塔作螺旋运动的时间，获得圆度更高的硝酸钠颗粒；
3）采用雾化方法，可得到粒度极小、粒度分布可以按要求调节的产品；
4）本发明将熔融的硝酸钠导入一高位保温缓冲槽，并在高位保温缓冲槽和熔盐炉之间设置一条回流管，上述结构的设置可以使熔盐过程和雾化过程各自独立地进行，实现工业的连续生产；
5）使用经过冷冻干燥的高压空气来冷却硝酸钠液滴，以此来降低所获得的硝酸钠颗粒产品的含水量。
附图说明
图1为本发明实施的生产流程示意图；
图2为硝酸钠颗粒的体积（重量）累计分布曲线。
具体实施方式
实施例1
如图1中所示，将工业硝酸钠原料在一熔盐炉中通过电加热方式熔融成液体，蒸发原料中含有的水份。将熔融的硝酸钠液体利用熔盐炉内的高温泵导入一高位保温缓冲槽，而后利用位差将其送至位于一造粒塔顶部的雾化装置，将其雾化成最大粒径为0.5mm，平均粒径30微米的雾滴。
雾化装置喷雾时所使用的气体为温度达300℃、压力为1.0Mpa的高压空气，以防止熔融的硝酸钠在喷雾时冷凝。
造粒塔上分设有上部进气管和下部进气管，由冷冻干燥空气压缩机获得的露点为-80℃、压力为1.0MPa的常温高压空气以1:3的流量比分别从上部进气管和下部进气送入造粒塔内，其中，从上部进气管进入的高压空气沿切线方向进入塔内，使从塔顶进入的硝酸钠雾滴在造粒塔内沿塔壁作螺旋下降，从下部进气管进入的高压空气则从下往上进入造粒塔内，使每一硝酸钠颗粒在造粒塔内作螺旋运动的时间基本保持在5min左右。
造粒塔上设有一引风管，该引风管设置在上述下部进气管的下方，进入塔内的高压空气和悬浮在其中的硝酸钠粉末从造粒塔下部设置的引风管导出，而后进入旋风分离器分离，分离得到的粉末从旋风分离器出口收集，包装获得产品；带有极少量粉状硝酸钠的空气则经由旋风分离器的排风管排出，引入水吸收槽吸收，而后排入大气。
收集位于造粒塔底的冷却硝酸钠球形细颗粒，包装获得产品。
硝酸钠颗粒产品的理化参数如下所示：
1）用JL-1155型激光粒度测试仪检测新获得的硝酸钠细颗粒，如图2中所示，粒径小于1mm毫米的颗粒含量为100%；
2）将上述硝酸钠细颗粒在常规储存条件下存放半年后，用JL-1155型激光粒度测试仪检测，粒径小于1mm毫米的颗粒含量为99.9%，筛余率为0.01%；
3）颗粒含水量用卡尔费休法检测，含水量为0.03%；
4）占总数量85%的硝酸钠颗粒圆度达到0.8。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。

Claims (7)

1、一种硝酸钠球形细颗粒的造粒方法，其特征在于，包括以下步骤：
1）将工业硝酸钠在熔盐炉内熔融后，导入一高位保温缓冲槽，而后送至位于一造粒塔顶部的雾化装置，将其雾化成粒径主要分布在30µm～0.5mm之间的雾滴；
2）将经过冷冻干燥的高压空气从所述造粒塔的上部进气管位置沿切线方向进入塔内，使步骤1中获得的硝酸钠雾滴在造粒塔内沿塔壁作螺旋下降，使其进一步球形化，得到球形细颗粒状的硝酸钠；
3）收集位于造粒塔底的冷却硝酸钠球形细颗粒，包装获得产品。
2、根据权利要求1中所述的一种硝酸钠球形细颗粒的造粒方法，其特征在于：步骤2中所使用的高压空气的露点在-60℃以下。
3、根据权利要求2中所述的一种硝酸钠球形细颗粒的造粒方法，其特征在于：所述造粒塔的下部也设置一进气管，并通过该进气管向造粒塔内导入从下往上的经过冷冻干燥的高压空气。
4、根据权利要求3中所述的一种硝酸钠球形细颗粒的造粒方法，其特征在于：所述的经过冷冻干燥的高压空气通过同一冷冻干燥空气压缩机产生，并分别流入造粒塔的下部进气管和上部进气管。
5、根据权利要求4中所述的一种硝酸钠球形细颗粒的造粒方法，其特征在于：所述雾化装置雾化时使用的是温度为280～310℃、压力为0.9～1.0Mpa的高压空气。
6、根据权利要求1或2或3或4或5中所述的一种硝酸钠球形细颗粒的造粒方法，其特征在于：塔内空气和悬浮在其中的硝酸钠粉末通过造粒塔下部设置的引风管导出，进入旋风分离器分离，得到的粉末由旋风分离器出口收集包装，含有极少量粉状硝酸钠的空气则经由排风管引入水吸收槽吸收后，排入大气。
7、根据权利要求6中所述的一种硝酸钠球形细颗粒的造粒方法，其特征在于：所述的引风管位于所述下部进气管的下方。
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CN109384251A (zh) * 2018-12-12 2019-02-26 青海盐湖工业股份有限公司 一种硝酸钾的造粒方法及其制备的硝酸钾颗粒
CN109692621A (zh) * 2019-01-29 2019-04-30 青海爱能森新材料科技有限公司 一种太阳能熔盐熔融造粒装置
CN114314610A (zh) * 2022-01-18 2022-04-12 三明科飞产气新材料股份有限公司 一种复合改性硝酸盐生产工艺

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