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CN111704176A - A kind of short-flow preparation method of nickel carbonate - Google Patents

A kind of short-flow preparation method of nickel carbonate Download PDF

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Publication number
CN111704176A
CN111704176A CN202010530269.6A CN202010530269A CN111704176A CN 111704176 A CN111704176 A CN 111704176A CN 202010530269 A CN202010530269 A CN 202010530269A CN 111704176 A CN111704176 A CN 111704176A
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nickel
sodium carbonate
nickel sulfate
synthesis
solution
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郭廷彪
陈琴
丁雨田
胡勇
贾智
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Lanzhou University of Technology
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Lanzhou University of Technology
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00Compounds of nickel
    • C01G53/06Carbonates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00Compounds of nickel
    • C01G53/04Oxides

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Abstract

A short-flow process for preparing nickel carbonate features that the low mole ratio of sodium carbonate to nickel sulfate is used, the low pH value is used, and the low-pH-value nickel carbonate flows in parallel into synthesizing reactor at 80-85 deg.C. In the continuous synthesis process, the blade of the stirrer is used for continuously stirring the synthetic liquid, so that the synthesis process is accelerated. And after the synthesis is finished, continuing stirring for 10-30 min, then performing filter pressing, then performing slurrying and washing on the filter cake again, repeatedly cleaning the filter cake for 3-4 times, and then performing filter pressing and air drying to obtain the nickel carbonate with qualified quality, wherein the nickel carbonate is used as a raw material for preparing nickel protoxide.

Description

一种碳酸镍的短流程制备方法A kind of short-flow preparation method of nickel carbonate

技术领域technical field

本发明涉及碳酸镍的制备技术。The present invention relates to the preparation technology of nickel carbonate.

背景技术Background technique

合成碳酸镍的方法有好几种,一种是在合成釜中先加一定量的水并通入蒸汽,通过蒸汽使水加热到70-80度,然后并联通入硫酸镍溶液和碳酸钠溶液,确保合成过程中PH值为6.9-7.0,对合成后的浆液进行过滤并对滤饼进行桨化,然后通入碳酸钠溶液,高PH值(9.2-9.5)进行碱浸脱硫,同时通入蒸汽,确保碱浸温度达到85℃以上,再进行压滤再次洗钠吹干这样一种工艺;第二种合成碳酸镍的工艺为高PH值合成后进行除钙除镁,且合成过程中碳酸钠与硫酸镍的浓度系数摩尔比为2.3:1,由于碳酸钠与硫酸镍的摩尔系数比大,造成碳酸钠的过度浪费和水洗钠时的难度增加,进而导致水洗过程中的水耗量增加,因而利用该工艺生产碳酸镍存在两点弊端,第一是碳酸钠消耗量大,第二是水洗量大,因而导致生产成本增加,能耗增加;第三种合成碳酸镍的工艺为合成过程中的PH控制在8.3-8.6,合成过程通过控制PH值,使合成液显示碱性,也是碳酸钠投入量增加,因而也造成一定成本上的浪费。There are several methods for synthesizing nickel carbonate. One is to add a certain amount of water to the synthesis kettle and pass steam, heat the water to 70-80 degrees through steam, and then feed nickel sulfate solution and sodium carbonate solution in parallel. , to ensure that the pH value in the synthesis process is 6.9-7.0, filter the synthesized slurry and paddle the filter cake, and then introduce sodium carbonate solution, high pH value (9.2-9.5) for alkali leaching desulfurization, and at the same time Steam to ensure that the alkali leaching temperature reaches above 85 ° C, and then carry out a process such as pressure filtration and sodium washing and drying; the second process for synthesizing nickel carbonate is to remove calcium and magnesium after high pH synthesis, and carbonic acid during the synthesis process. The molar ratio of the concentration coefficient of sodium to nickel sulfate is 2.3:1. Due to the large molar coefficient ratio of sodium carbonate to nickel sulfate, the excessive waste of sodium carbonate and the difficulty in washing sodium with water increase, which in turn leads to an increase in water consumption during the washing process. Therefore, there are two drawbacks in using this process to produce nickel carbonate. The first is that the consumption of sodium carbonate is large, and the second is that the amount of water washing is large, which leads to an increase in production costs and an increase in energy consumption; the third technology for synthesizing nickel carbonate is a synthesis process. The PH in the liquid is controlled at 8.3-8.6, and the synthetic liquid is made alkaline by controlling the pH value in the synthesis process, and the input amount of sodium carbonate is also increased, thus causing a certain waste of cost.

发明内容SUMMARY OF THE INVENTION

本发明的目的是提供一种碳酸镍的短流程制备方法。The purpose of this invention is to provide a kind of short-flow preparation method of nickel carbonate.

本发明是一种碳酸镍的短流程制备方法,其步骤为:The present invention is a kind of short-flow preparation method of nickel carbonate, and its steps are:

步骤1:向储罐中硫酸镍溶液中通入蒸汽,进行加热,使其达到80℃~85℃;Step 1: Pour steam into the nickel sulfate solution in the storage tank, and heat it to make it reach 80°C to 85°C;

步骤2:在碳酸钠溶解釜的水中通入蒸汽,进行加热至40~50℃,加入碳酸钠,碳酸钠的摩尔数是硫酸镍的1.2~1.25倍,继续通入蒸汽,使碱液的温度达到80℃~85℃;Step 2: Pour steam into the water in the sodium carbonate dissolving kettle, heat it to 40~50°C, add sodium carbonate, the mole number of sodium carbonate is 1.2~1.25 times that of nickel sulfate, continue to pass steam to make the temperature of the lye solution Reach 80℃~85℃;

步骤3:硫酸镍溶液与碳酸钠溶液并联进入合成釜,碳酸钠溶液的流速与硫酸镍溶液的流速比(为1.2~1.25):1;Step 3: The nickel sulfate solution and the sodium carbonate solution enter the synthesis kettle in parallel, and the ratio of the flow rate of the sodium carbonate solution to the flow rate of the nickel sulfate solution (1.2 to 1.25): 1;

步骤4:并联进入合成釜时硫酸镍的流速为1.2~1.8m3/h,连续合成过程中,利用搅拌的桨叶不断对合成液进行搅拌,加速合成过程;Step 4: when entering the synthesis kettle in parallel, the flow rate of nickel sulfate is 1.2~1.8 m 3 /h, and in the continuous synthesis process, the synthesis solution is continuously stirred by stirring paddles to accelerate the synthesis process;

步骤5:当合成完成后,继续搅拌10~30min,然后进行压滤,然后把滤饼再次进行桨化,洗涤,反复对滤饼清洗3~4次,然后压滤风干,将制得质量合格的碳酸镍,然后取样化验,用作制备氧化亚镍的原料。Step 5: After the synthesis is completed, continue to stir for 10-30 minutes, then carry out pressure filtration, then paddle the filter cake again, wash the filter cake repeatedly, wash the filter cake for 3 to 4 times, and then filter and air-dry, and the obtained quality will be qualified. The nickel carbonate is then sampled and used as a raw material for the preparation of nickelous oxide.

本发明的有益之处是:采取控制碳酸钠与硫酸镍的摩尔系数比,低PH值进行合成,低温度进行洗钠和洗硫,达到节能降耗且低成本生产制备碳酸镍。利用低的碳酸钠与硫酸镍的摩尔比,低PH值合成,对合成后的碳酸镍进行低温洗涤除钠,降低生产成本,降低能耗,提高生产效率。The present invention has the advantages that the molar coefficient ratio of sodium carbonate and nickel sulfate is controlled, the synthesis is performed at a low pH value, and the sodium and sulfur are washed at a low temperature, so as to achieve energy saving, consumption reduction and low-cost production and preparation of nickel carbonate. Utilizing the low molar ratio of sodium carbonate and nickel sulfate to synthesize at low pH value, the synthesized nickel carbonate is washed at low temperature to remove sodium, so as to reduce production cost, reduce energy consumption and improve production efficiency.

具体实施方式Detailed ways

本发明是一种碳酸镍的短流程制备方法,其步骤为:The present invention is a kind of short-flow preparation method of nickel carbonate, and its steps are:

步骤1:向储罐中硫酸镍溶液中通入蒸汽,进行加热,使其达到80℃~85℃;Step 1: Pour steam into the nickel sulfate solution in the storage tank, and heat it to make it reach 80°C to 85°C;

步骤2:在碳酸钠溶解釜的水中通入蒸汽,进行加热至40~50℃,加入碳酸钠,碳酸钠的摩尔数是硫酸镍的1.2~1.25倍,继续通入蒸汽,使碱液的温度达到80℃~85℃;Step 2: Pour steam into the water in the sodium carbonate dissolving kettle, heat it to 40~50°C, add sodium carbonate, the mole number of sodium carbonate is 1.2~1.25 times that of nickel sulfate, continue to pass steam to make the temperature of the lye solution Reach 80℃~85℃;

步骤3:硫酸镍溶液与碳酸钠溶液并联进入合成釜,碳酸钠溶液的流速与硫酸镍溶液的流速比(为1.2~1.25):1;Step 3: The nickel sulfate solution and the sodium carbonate solution enter the synthesis kettle in parallel, and the ratio of the flow rate of the sodium carbonate solution to the flow rate of the nickel sulfate solution (1.2 to 1.25): 1;

步骤4:并联进入合成釜时硫酸镍的流速为1.2~1.8m3/h,连续合成过程中,利用搅拌的桨叶不断对合成液进行搅拌,加速合成过程;Step 4: when entering the synthesis kettle in parallel, the flow rate of nickel sulfate is 1.2~1.8 m 3 /h, and in the continuous synthesis process, the synthesis solution is continuously stirred by stirring paddles to accelerate the synthesis process;

步骤5:当合成完成后,继续搅拌10~30min,然后进行压滤,然后把滤饼再次进行桨化,洗涤,反复对滤饼清洗3~4次,然后压滤风干,将制得质量合格的碳酸镍,然后取样化验,用作制备氧化亚镍的原料。下面用更为具体的实施例进一步展开本发明。Step 5: After the synthesis is completed, continue to stir for 10-30 minutes, then carry out pressure filtration, then paddle the filter cake again, wash the filter cake repeatedly, wash the filter cake for 3 to 4 times, and then filter and air-dry, and the obtained quality will be qualified. The nickel carbonate is then sampled and used as a raw material for the preparation of nickelous oxide. The present invention is further developed with more specific embodiments below.

实施例1:Example 1:

将140.34g/L的硫酸镍溶液(溶液成分如下表4所示)5m3加入到硫酸镍储罐中,然后对硫酸镍储罐通入蒸汽,使储罐中的硫酸镍溶液温度达到80-85℃;在碱液储罐中加入6m3的水,然后再通入蒸汽,对碱液储罐中的水进行加热,当其温度达到40-50℃后,加入698kg的碳酸钠(碳酸钠与硫酸镍的摩尔系数比为1.22:1),加入后进行不断搅拌,等碳酸钠充分溶解后,取样进行杂质含量分析,分析结果如表2所示。同时进行蒸汽加热,将碱液持续加热使其温度达到80-85℃。然后并联使硫酸镍溶液和碳酸钠溶液同时通往合成釜中,硫酸镍溶液的流速为1.5m3/h,碳酸钠溶液的流速为1.8m3/h。在合成过程中不断搅拌,且通过调节蒸汽阀调节蒸汽流量,控制合成温度,确保合成温度控制在80℃。当溶液合成时间达到2h后,停止向合成釜中加入并联溶液,继续搅拌30min。然后对合成的浆液进行压滤,然后利用40-50℃的水对滤饼进行洗涤,反复洗涤3-4次后,压滤吹干,取样检测化验。Add 5m3 of 140.34g/L nickel sulfate solution (the solution composition is shown in Table 4 below) into the nickel sulfate storage tank, and then pass steam to the nickel sulfate storage tank, so that the temperature of the nickel sulfate solution in the storage tank reaches 80- 85°C; add 6m 3 of water in the lye storage tank, and then pass steam to heat the water in the lye storage tank. When the temperature reaches 40-50°C, add 698kg of sodium carbonate (sodium carbonate). The ratio of molar coefficient to nickel sulfate is 1.22:1). After adding, continue stirring. After the sodium carbonate is fully dissolved, sampling is carried out for impurity content analysis. The analysis results are shown in Table 2. At the same time, steam heating is performed, and the lye is continuously heated to make the temperature reach 80-85 °C. Then the nickel sulfate solution and the sodium carbonate solution are connected in parallel to the synthesis kettle at the same time, the flow rate of the nickel sulfate solution is 1.5m 3 /h, and the flow rate of the sodium carbonate solution is 1.8m 3 /h. During the synthesis process, stirring was continued, and the steam flow was adjusted by adjusting the steam valve, and the synthesis temperature was controlled to ensure that the synthesis temperature was controlled at 80 °C. When the solution synthesis time reaches 2h, stop adding the parallel solution to the synthesis kettle, and continue stirring for 30min. Then the synthesized slurry is filtered by pressure, and then the filter cake is washed with water at 40-50° C. After repeated washing for 3-4 times, pressure-filtered and dried, and sampled for testing.

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从实施例1制备碳酸镍取样的检测结果可以看出:利用该工艺制备的碳酸镍镍含量较高,杂质含量非常低,完全满足制备氧化亚镍所需要的原料的需求规定。It can be seen from the detection result of preparing nickel carbonate sampling in Example 1: the nickel carbonate nickel content prepared by this process is relatively high, and the impurity content is very low, which fully meets the requirements of the raw materials required for the preparation of nickelous oxide.

实施例2Example 2

将142.63g/L的硫酸镍溶液(溶液成分如下表4所示)5m3加入到硫酸镍储罐中,然后对硫酸镍储罐通入蒸汽,使储罐中的硫酸镍溶液温度达到80-85℃;在碱液储罐中加入6m3的水,然后再通入蒸汽,对碱液储罐中的水进行加热,当其温度达到40-50℃后,加入720kg的碳酸钠(碳酸钠与硫酸镍的摩尔系数比为1.23:1),加入后进行不断搅拌,等碳酸钠充分溶解后,取样进行杂质含量分析,分析结果如表5所示。同时进行蒸汽加热,将碱液持续加热使其温度达到80-85℃。然后并联使硫酸镍溶液和碳酸钠溶液同时通往合成釜中,硫酸镍溶液的流速为1.2m3/h,碳酸钠溶液的流速为1.5m3/h。在合成过程中不断搅拌,且通过调节蒸汽阀调节蒸汽流量,控制合成温度,确保合成温度控制在83℃。当溶液合成时间达到2h后,停止向合成釜中加入并联溶液,继续搅拌30min。然后对合成的浆液进行压滤,然后利用40-50℃的水对滤饼进行洗涤,反复洗涤3-4次后,压滤吹干,取样检测化验,化验结果如下表6所示。Add 5m 3 of 142.63g/L nickel sulfate solution (the solution composition is shown in Table 4 below) into the nickel sulfate storage tank, and then pass steam to the nickel sulfate storage tank, so that the temperature of the nickel sulfate solution in the storage tank reaches 80- 85°C; add 6m3 of water to the lye storage tank, and then pass in steam to heat the water in the lye storage tank. When the temperature reaches 40-50°C, add 720kg of sodium carbonate (sodium carbonate and The molar coefficient ratio of nickel sulfate is 1.23:1). After adding, it is continuously stirred. After the sodium carbonate is fully dissolved, sampling is carried out for impurity content analysis. The analysis results are shown in Table 5. At the same time, steam heating is performed, and the lye is continuously heated to make the temperature reach 80-85 °C. Then the nickel sulfate solution and the sodium carbonate solution are connected in parallel to the synthesis kettle at the same time, the flow rate of the nickel sulfate solution is 1.2m 3 /h, and the flow rate of the sodium carbonate solution is 1.5m 3 /h. During the synthesis process, stirring was continued, and the steam flow was adjusted by adjusting the steam valve, and the synthesis temperature was controlled to ensure that the synthesis temperature was controlled at 83 °C. When the solution synthesis time reaches 2h, stop adding the parallel solution to the synthesis kettle, and continue stirring for 30min. Then the synthesized slurry is filtered by pressure, and then the filter cake is washed with water at 40-50° C. After repeated washing for 3-4 times, pressure filtration is dried, and sampling is performed for testing. The test results are shown in Table 6 below.

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从实施例2制备碳酸镍取样的检测结果可以看出:利用该工艺制备的碳酸镍镍含量较高,杂质含量非常低,完全满足制备氧化亚镍所需要的原料的需求规定。It can be seen from the detection results of the preparation of nickel carbonate sampling in Example 2: the nickel carbonate nickel content prepared by this process is relatively high, and the impurity content is very low, which fully meets the requirements of the raw materials required for the preparation of nickelous oxide.

实施例3Example 3

将144.12g/L的硫酸镍溶液(溶液成分如下表7所示)5m3加入到硫酸镍储罐中,然后对硫酸镍储罐通入蒸汽,使储罐中的硫酸镍溶液温度达到80-85℃;在碱液储罐中加入6m3的水,然后再通入蒸汽,对碱液储罐中的水进行加热,当其温度达到40-50℃后,加入738kg的碳酸钠(碳酸钠与硫酸镍的摩尔系数比为1.25:1),加入后进行不断搅拌,等碳酸钠充分溶解后,取样进行杂质含量分析,分析结果如表8所示。同时进行蒸汽加热,将碱液持续加热使其温度达到80-85℃。然后并联使硫酸镍溶液和碳酸钠溶液同时通往合成釜中,硫酸镍溶液的流速为1.8m3/h,碳酸钠溶液的流速为2.16m3/h。在合成过程中不断搅拌,且通过调节蒸汽阀调节蒸汽流量,控制合成温度,确保合成温度控制在85℃。当溶液合成时间达到2h后,停止向合成釜中加入并联溶液,继续搅拌30min。然后对合成的浆液进行压滤,然后利用40-50℃的水对滤饼进行洗涤,反复洗涤3-4次后,压滤吹干,取样检测化验,化验结果如下表9所示。Add 5m3 of 144.12g /L nickel sulfate solution (the solution composition is shown in Table 7 below) into the nickel sulfate storage tank, and then pass steam to the nickel sulfate storage tank, so that the temperature of the nickel sulfate solution in the storage tank reaches 80- 85°C; add 6m 3 of water in the lye storage tank, and then pass steam to heat the water in the lye storage tank. When the temperature reaches 40-50°C, add 738kg of sodium carbonate (sodium carbonate). The ratio of molar coefficient to nickel sulfate is 1.25:1), stirring continuously after adding, and after the sodium carbonate is fully dissolved, sampling is carried out for impurity content analysis, and the analysis results are shown in Table 8. At the same time, steam heating is performed, and the lye is continuously heated to make the temperature reach 80-85 °C. Then the nickel sulfate solution and the sodium carbonate solution are connected in parallel to the synthesis kettle at the same time, the flow rate of the nickel sulfate solution is 1.8m 3 /h, and the flow rate of the sodium carbonate solution is 2.16m 3 /h. During the synthesis process, stirring was continued, and the steam flow was adjusted by adjusting the steam valve, and the synthesis temperature was controlled to ensure that the synthesis temperature was controlled at 85°C. When the solution synthesis time reaches 2h, stop adding the parallel solution to the synthesis kettle, and continue stirring for 30min. Then the synthesized slurry is filtered by pressure, and then the filter cake is washed with water at 40-50° C. After repeated washing for 3-4 times, pressure filtration is dried, and sampling is performed for testing. The test results are shown in Table 9 below.

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从实施例3制备碳酸镍取样的检测结果可以看出:利用该工艺制备的碳酸镍镍含量较高,杂质含量非常低,完全满足制备氧化亚镍所需要的原料的需求规定。且利用该工艺制备碳酸镍时,所消耗的碳酸钠量较低,水洗时的加热温度也较低,利用该工艺生产碳酸镍,既节省成本,又节能降耗,且通过检测,压滤后的废水中的镍含量非常低,因而金属回收率也非常高。It can be seen from the detection results of the preparation of nickel carbonate sampling in Example 3: the nickel carbonate nickel content prepared by this process is relatively high, and the impurity content is very low, which fully meets the requirements of the raw materials required for the preparation of nickelous oxide. And when using this process to prepare nickel carbonate, the amount of sodium carbonate consumed is low, and the heating temperature during washing is also low. Using this process to produce nickel carbonate not only saves costs, but also saves energy and reduces consumption. The nickel content of the wastewater is very low, so the metal recovery rate is also very high.

Claims (1)

1. A short-process preparation method of nickel carbonate is characterized by comprising the following steps:
step 1: introducing steam into the nickel sulfate solution in the storage tank, and heating to reach 80-85 ℃;
step 2: introducing steam into water in a sodium carbonate dissolving kettle, heating to 40-50 ℃, adding sodium carbonate, wherein the mole number of the sodium carbonate is 1.2-1.25 times that of nickel sulfate, and continuously introducing the steam to enable the temperature of alkali liquor to reach 80-85 ℃;
and step 3: the nickel sulfate solution and the sodium carbonate solution are connected in parallel and enter a synthesis kettle, and the ratio of the flow speed of the sodium carbonate solution to the flow speed of the nickel sulfate solution (1.2-1.25) is 1;
and 4, step 4: the flow velocity of the nickel sulfate is 1.2-1.8 m when the nickel sulfate enters the synthesis kettle in parallel3In the continuous synthesis process, continuously stirring the synthetic liquid by using a stirring blade to accelerate the synthesis process;
and 5: and after the synthesis is finished, continuing stirring for 10-30 min, then performing filter pressing, then performing slurrying and washing on the filter cake again, repeatedly cleaning the filter cake for 3-4 times, then performing filter pressing and air drying, preparing the nickel carbonate with qualified quality, and then sampling and testing to be used as a raw material for preparing nickel protoxide.
CN202010530269.6A 2020-06-11 2020-06-11 A kind of short-flow preparation method of nickel carbonate Pending CN111704176A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101016173A (en) * 2006-12-29 2007-08-15 金川集团有限公司 Method of preparing electronic grade nickel carbonate by sodium carbonate deposition
CN101519229A (en) * 2009-03-19 2009-09-02 金川集团有限公司 Method for continuously synthesizing nickel carbonate
CN105645482A (en) * 2016-02-26 2016-06-08 金川集团股份有限公司 Synthesis method of nickel protoxide precursor nickel carbonate

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101016173A (en) * 2006-12-29 2007-08-15 金川集团有限公司 Method of preparing electronic grade nickel carbonate by sodium carbonate deposition
CN101519229A (en) * 2009-03-19 2009-09-02 金川集团有限公司 Method for continuously synthesizing nickel carbonate
CN105645482A (en) * 2016-02-26 2016-06-08 金川集团股份有限公司 Synthesis method of nickel protoxide precursor nickel carbonate

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