WO2019128142A1 - Method for preparing high-density basic nickel carbonate - Google Patents

Method for preparing high-density basic nickel carbonate Download PDF

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WO2019128142A1
WO2019128142A1 PCT/CN2018/091866 CN2018091866W WO2019128142A1 WO 2019128142 A1 WO2019128142 A1 WO 2019128142A1 CN 2018091866 W CN2018091866 W CN 2018091866W WO 2019128142 A1 WO2019128142 A1 WO 2019128142A1
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nickel
carbonate
solution
nickel carbonate
preparing
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PCT/CN2018/091866
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French (fr)
Chinese (zh)
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许开华
苏陶贵
张云河
陈龙
王超
吴伟
郭苗苗
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荆门市格林美新材料有限公司
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Publication of WO2019128142A1 publication Critical patent/WO2019128142A1/en

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/06—Carbonates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/02—Particle morphology depicted by an image obtained by optical microscopy
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/10—Solid density

Definitions

  • the invention belongs to the technical field of synthesis of basic nickel carbonate, and in particular relates to a preparation method of high-density basic nickel carbonate.
  • Basic nickel carbonate is an important inorganic fine chemical, mainly used in the preparation of various nickel salts, high-quality basic nickel carbonate, which can be used in the electronics industry and catalyst industry. In addition, basic nickel carbonate is also widely used. Electroplating, electroforming, enamel pigments, etc.
  • the basic nickel carbonate precipitating agent is generally sodium carbonate, ammonium carbonate (or ammonium hydrogencarbonate); using ammonium carbonate (or ammonium hydrogencarbonate) as a precipitating agent, the raw material is cheap, and the obtained nickel carbonate has a fine particle size, but the conversion rate of nickel is not high.
  • the mother liquor must be recovered, and the density of nickel carbonate is low; while sodium carbonate is used as a precipitant, the raw materials are easy to obtain cheap, the conversion rate of nickel salt is high, the cost is low, and the economic benefit is good.
  • the basic nickel carbonate has high requirements for Na, S and Cl content, and the Ni content of basic nickel carbonate is required to be 44% ⁇ 48%, and the bulk density is greater than 0.8g/cm 3 ;
  • the content of Ni in the basic nickel carbonate obtained by the prior art is more than 48%, and the ammonium salt is often used as a precipitant in the preparation process, which easily leads to many kinds of impurity elements, is not easy to be washed, has high impurity content, long washing process and high production cost. And the introduction of ammonia increases the cost of wastewater treatment.
  • the main object of the present invention is to provide a method for preparing high-density basic nickel carbonate, which solves the problems of the prior art basic nickel carbonate having many types of impurities, large content, difficulty in cleaning, and high production cost.
  • the technical solution of the present invention is achieved by a method for preparing high-density basic nickel carbonate, which is achieved by the following steps:
  • Step 1 Prepare a sodium carbonate solution having a carbonate ion concentration of 100 to 250 g/L and a nickel salt solution having a nickel ion concentration of 1 to 2 mol/L in the solution tank;
  • Step 2 feeding with a metering pump, adding the sodium carbonate solution and the nickel salt solution to the special reactor at the same time, keeping the flow rate of the nickel salt solution unchanged during the feeding process, and adjusting the pH value of the flow rate control system by adjusting the flow rate of the sodium carbonate solution And reacting at 70 to 99 ° C to obtain a mixture of nickel carbonate and mother liquor;
  • Step 3 the mixture of the nickel carbonate and the mother liquid obtained in the step 2 is driven into a centrifuge to remove the mother liquid to obtain a crude nickel carbonate;
  • step 4 the crude nickel carbonate obtained in the step 3 is rinsed and washed with lye, pure water having a mass fraction of 0.1 to 5.5%, dried, and sieved to obtain a high-density basic nickel carbonate.
  • the nickel salt is at least one of nickel chloride, nickel sulfate, and nickel nitrate.
  • the flow rate of the sodium carbonate solution is 5 ⁇ 1000 L/h
  • the flow rate of the nickel salt solution is 50 ⁇ 1000 L/h.
  • the pH is 8.0 ⁇ 8.3.
  • the reaction time is 8-18 h.
  • the temperature of the alkali liquid is 40 to 70 ° C; the temperature of the pure water is 70 to 85 ° C, and the conductivity of the pure water is ⁇ 100 ⁇ s / m.
  • the drying temperature is 95-105 ° C, and the drying time is 2 ⁇ 3 h.
  • the sieve is selected from 200 to 400 mesh.
  • the bulk density of the high-density basic nickel carbonate is 0.8-1.3 g/cm 3 .
  • the invention adopts a single sodium carbonate as a precipitating agent, and NH4+ is not introduced into the whole reaction system, so that the obtained basic nickel carbonate has few kinds of impurities; the temperature is 40-70 ° C and the quality is sequentially used.
  • the lye with a fraction of 0.1 to 5.5% and the pure water leaching and washing of the basic nickel carbonate with a temperature of 70-85 ° C and a conductivity of ⁇ 100 ⁇ s / m solve the problem that the prior art is difficult to clean and the production cost is high.
  • the obtained basic nickel carbonate has a small content of Na and Cl elements, and can be well applied to the hydrodesulfurization catalytic industry.
  • Figure 1 is a micrograph of a high-density basic nickel carbonate obtained in Example 1 of the present invention.
  • the present invention provides an embodiment to provide a method for preparing high-density basic nickel carbonate, which is achieved by the following steps:
  • Step 1 Prepare a sodium carbonate solution having a carbonate ion concentration of 100 to 250 g/L and a nickel salt solution having a nickel ion concentration of 1 to 2 mol/L in the solution tank; wherein the nickel salt is nickel chloride, nickel sulfate, and nitric acid. At least one of nickel;
  • Step 2 feeding with a metering pump, adding the sodium carbonate solution and the nickel salt solution to the special reactor at the same time, keeping the flow rate of the nickel salt solution unchanged during the feeding process is 50-1000 L/h, by adjusting the sodium carbonate solution.
  • the pH of the flow control system is 8.0 ⁇ 8.3, and the reaction is carried out at 70 ⁇ 99 °C for 8 ⁇ 18h to obtain a mixture of nickel carbonate and mother liquor; wherein the flow rate of the sodium carbonate solution is adjusted to range from 50 to 1000 L/h;
  • Step 3 the mixture of the nickel carbonate and the mother liquid obtained in the step 2 is driven into a centrifuge to remove the mother liquid to obtain a crude nickel carbonate;
  • Step 4 respectively, using the lye at a temperature of 40 to 70 ° C and having a mass fraction of 0.1 to 5.5%, the pure water leaching and washing step 3 obtained at a temperature of 70 to 85 ° C and a conductivity of ⁇ 100 ⁇ s/m.
  • the crude product is dried at 95-105 ° C for 2 ⁇ 3 hours and passed through a 200-400 mesh sieve to obtain a high-density basic nickel carbonate with a bulk density of 0.8-1.3 g/cm 3 .
  • the invention adopts a single sodium carbonate as a precipitating agent, and NH+4 is not introduced into the whole reaction system, so that the obtained basic nickel carbonate has few kinds of impurities; the temperature is 40-70° C. and the mass fraction is 0.1-5.5. % alkali solution and pure water rinsing and washing basic nickel carbonate with a temperature of 70-85 ° C and conductivity ⁇ 100 ⁇ s / m, solving the problem that the prior art is difficult to clean, high production cost, and the obtained alkali
  • the nickel carbonate type has a small content of Na and Cl, and can be well applied to the hydrodesulfurization catalytic industry.
  • a method for preparing high-density basic nickel carbonate which is achieved by the following steps:
  • Step 1 in the solution tank, respectively, a sodium carbonate solution having a carbonate ion concentration of 150 g/L and a nickel chloride solution having a nickel ion concentration of 1.5 mol/L;
  • Step 2 using a metering pump feed, the sodium carbonate solution and the nickel chloride solution are simultaneously added to a special reactor (the reactor can flow out of the mother liquor during the reaction, and ensure the solid content of the reaction system composed of nickel carbonate and mother liquor) Increasingly), the flow rate of the nickel salt solution is kept constant at 50 L/h during the feeding process, and the pH of the control system is controlled by adjusting the flow rate of the sodium carbonate solution (the flow rate of the sodium carbonate solution is adjusted to 50 to 1000 L/h) 8.1, and reacted at 80 ° C for 15 h to obtain a mixture of nickel carbonate and mother liquor;
  • Step 3 the mixture of the nickel carbonate and the mother liquid obtained in the step 2 is driven into a centrifuge to remove the mother liquid to obtain a crude nickel carbonate;
  • Step 4 respectively, using a lye having a temperature of 55 ° C and a mass fraction of 2.5%, a pure water having a temperature of 80 ° C and a conductivity of ⁇ 100 ⁇ s / m, and washing the crude nickel carbonate obtained in the step 3, and then at 100 ° C After drying for 2.5 h and passing through a 300 mesh sieve, a high density basic nickel carbonate having a bulk density of 1.0 g/cm 3 was obtained.
  • a method for preparing high-density basic nickel carbonate which is achieved by the following steps:
  • Step 1 in the solution tank, respectively, a sodium carbonate solution having a carbonate ion concentration of 150 g/L and a nickel chloride solution having a nickel ion concentration of 1.5 mol/L;
  • Step 2 using a metering pump feed, the sodium carbonate solution and the nickel chloride solution are simultaneously added to a special reactor (the reactor can flow out of the mother liquor during the reaction, and ensure the solid content of the reaction system composed of nickel carbonate and mother liquor) Increasingly), the flow rate of the nickel salt solution is kept constant at 50 L/h during the feeding process, and the pH of the control system is controlled by adjusting the flow rate of the sodium carbonate solution (the flow rate of the sodium carbonate solution is adjusted to 50 to 1000 L/h) 8.0, and reacted at 99 ° C for 8 h to obtain a mixture of nickel carbonate and mother liquor;
  • Step 3 the mixture of the nickel carbonate and the mother liquid obtained in the step 2 is driven into a centrifuge to remove the mother liquid to obtain a crude nickel carbonate;
  • a method for preparing high-density basic nickel carbonate which is achieved by the following steps:
  • Step 1 in the solution tank, respectively, a sodium carbonate solution having a carbonate ion concentration of 150 g/L and a nickel chloride solution having a nickel ion concentration of 1.5 mol/L;
  • Step 2 using a metering pump feed, the sodium carbonate solution and the nickel chloride solution are simultaneously added to a special reactor (the reactor can flow out of the mother liquor during the reaction, and ensure the solid content of the reaction system composed of nickel carbonate and mother liquor) Increasingly), the flow rate of the nickel salt solution is kept constant at 50 L/h during the feeding process, and the pH of the control system is controlled by adjusting the flow rate of the sodium carbonate solution (the flow rate of the sodium carbonate solution is adjusted to 50 to 1000 L/h) 8.3, and reacted at 70 ° C for 18 h to obtain a mixture of nickel carbonate and mother liquor;
  • Step 3 the mixture of the nickel carbonate and the mother liquid obtained in the step 2 is driven into a centrifuge to remove the mother liquid to obtain a crude nickel carbonate;
  • Step 4 respectively, using a lye solution having a temperature of 70 ° C and a mass fraction of 0.1%, a pure water having a temperature of 5 ° C and a conductivity of ⁇ 100 ⁇ s / m, and a crude nickel carbonate obtained by washing step 3, and then at 105 ° C. After drying for 2 hours and passing through a 300 mesh sieve, a high density basic nickel carbonate having a bulk density of 0.8 g/cm 3 was obtained.
  • a method for preparing high-density basic nickel carbonate which is achieved by the following steps:
  • Step 1 preparing a sodium carbonate solution having a carbonate ion concentration of 100 g/L and a nickel chloride solution having a nickel ion concentration of 1 mol/L in the solution tank;
  • Step 2 using a metering pump feed, the sodium carbonate solution and the nickel chloride solution are simultaneously added to a special reactor (the reactor can flow out of the mother liquor during the reaction, and ensure the solid content of the reaction system composed of nickel carbonate and mother liquor) Increasingly), the flow rate of the nickel salt solution is kept constant at 800 L/h during the feeding process, and the pH of the control system is controlled by adjusting the flow rate of the sodium carbonate solution (the flow rate of the sodium carbonate solution is adjusted to 50 to 1000 L/h) 8.1, and reacted at 80 ° C for 15 h to obtain a mixture of nickel carbonate and mother liquor;
  • Step 3 the mixture of the nickel carbonate and the mother liquid obtained in the step 2 is driven into a centrifuge to remove the mother liquid to obtain a crude nickel carbonate;
  • Step 4 respectively, using a lye having a temperature of 55 ° C and a mass fraction of 2.5%, a pure water having a temperature of 80 ° C and a conductivity of ⁇ 100 ⁇ s / m, and washing the crude nickel carbonate obtained in the step 3, and then at 100 ° C After drying for 2.5 hours and passing through a 300 mesh sieve, a high density basic nickel carbonate having a bulk density of 1.2 g/cm 3 was obtained.
  • a method for preparing high-density basic nickel carbonate which is achieved by the following steps:
  • Step 1 preparing a sodium carbonate solution having a carbonate ion concentration of 100 g/L and a nickel chloride solution having a nickel ion concentration of 1 mol/L in the solution tank;
  • Step 2 using a metering pump feed, the sodium carbonate solution and the nickel chloride solution are simultaneously added to a special reactor (the reactor can flow out of the mother liquor during the reaction, and ensure the solid content of the reaction system composed of nickel carbonate and mother liquor) Increasingly), the flow rate of the nickel salt solution is kept constant at 800 L/h during the feeding process, and the pH of the control system is controlled by adjusting the flow rate of the sodium carbonate solution (the flow rate of the sodium carbonate solution is adjusted to 50 to 1000 L/h) 8.0, and reacted at 99 ° C for 8 h to obtain a mixture of nickel carbonate and mother liquor;
  • Step 3 the mixture of the nickel carbonate and the mother liquid obtained in the step 2 is driven into a centrifuge to remove the mother liquid to obtain a crude nickel carbonate;
  • Step 4 respectively, using a lye solution having a temperature of 40 ° C and a mass fraction of 5.5%, a pure water having a temperature of 70 ° C and a conductivity of ⁇ 100 ⁇ s / m, and a crude nickel carbonate obtained by the washing step 3, and then at 95 ° C. After drying for 3 hours and passing through a 300 mesh sieve, a high density basic nickel carbonate having a bulk density of 1.1 g/cm 3 was obtained.
  • a method for preparing high-density basic nickel carbonate which is achieved by the following steps:
  • Step 1 preparing a sodium carbonate solution having a carbonate ion concentration of 100 g/L and a nickel chloride solution having a nickel ion concentration of 1 mol/L in the solution tank;
  • Step 2 using a metering pump feed, the sodium carbonate solution and the nickel chloride solution are simultaneously added to a special reactor (the reactor can flow out of the mother liquor during the reaction, and ensure the solid content of the reaction system composed of nickel carbonate and mother liquor) Increasingly), the flow rate of the nickel salt solution is kept constant at 800 L/h during the feeding process, and the pH of the control system is controlled by adjusting the flow rate of the sodium carbonate solution (the flow rate of the sodium carbonate solution is adjusted to 50 to 1000 L/h) 8.3, and reacted at 70 ° C for 18 h to obtain a mixture of nickel carbonate and mother liquor;
  • Step 3 the mixture of the nickel carbonate and the mother liquid obtained in the step 2 is driven into a centrifuge to remove the mother liquid to obtain a crude nickel carbonate;
  • Step 4 respectively, using a lye solution having a temperature of 70 ° C and a mass fraction of 0.1%, a pure water having a temperature of 5 ° C and a conductivity of ⁇ 100 ⁇ s / m, and a crude nickel carbonate obtained by washing step 3, and then at 105 ° C. After drying for 2 hours and passing through a 300 mesh sieve, a high density basic nickel carbonate having a bulk density of 1.3 g/cm 3 was obtained.
  • a method for preparing high-density basic nickel carbonate which is achieved by the following steps:
  • Step 1 preparing a sodium carbonate solution having a carbonate ion concentration of 250 g/L and a nickel nitrate solution having a nickel ion concentration of 2 mol/L in the solution tank;
  • Step 2 using a metering pump feed, the sodium carbonate solution and the nickel chloride solution are simultaneously added to a special reactor (the reactor can flow out of the mother liquor during the reaction, and ensure the solid content of the reaction system composed of nickel carbonate and mother liquor) Increasingly), the flow rate of the nickel salt solution is kept constant at 50 L/h during the feeding process, and the pH of the control system is controlled by adjusting the flow rate of the sodium carbonate solution (the flow rate of the sodium carbonate solution is adjusted to 50 to 1000 L/h) 8.0, and reacted at 99 ° C for 8 h to obtain a mixture of nickel carbonate and mother liquor;
  • Step 3 the mixture of the nickel carbonate and the mother liquid obtained in the step 2 is driven into a centrifuge to remove the mother liquid to obtain a crude nickel carbonate;
  • Step 4 respectively, using a lye solution having a temperature of 40 ° C and a mass fraction of 5.5%, a pure water having a temperature of 70 ° C and a conductivity of ⁇ 100 ⁇ s / m, and a crude nickel carbonate obtained by the washing step 3, and then at 95 ° C. After drying for 3 hours and passing through a 300 mesh sieve, a high density basic nickel carbonate having a bulk density of 1.0 g/cm 3 was obtained.
  • Example 1 The structure of the high-density basic nickel carbonate obtained in Example 1 was observed under a microscope, and the observation results are shown in FIG. 1; the basic nickel carbonate obtained in Example 1 - Example 7 was subjected to detection of Na, Ni, and CI contents, The test results are shown in Table 1:
  • Table 1 shows the physical property detection data of the basic nickel carbonate obtained in Example 1 to Example 7 of the present invention.
  • the basic nickel carbonate obtained by the present invention is spherical-like particles and wherein Na ⁇ 0.0200%, 44% ⁇ Ni ⁇ 48%, Cl ⁇ 0.0030%, it can be seen that the present invention
  • the properties of the obtained basic nickel carbonate are superior to those of the basic nickel carbonate obtained by the prior art.

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Abstract

Disclosed is a method for preparing high-density basic nickel carbonate. The method is implemented by the following steps: step 1, formulating a sodium carbonate solution and a nickel salt solution in solution tanks, respectively; step 2, simultaneously feeding, with a metering pump, the sodium carbonate solution and the nickel salt solution into a specially made reactor, keeping the flow rate of the nickel salt solution constant during the feeding process, controlling the pH value of a system by adjusting the flow rate of the sodium carbonate solution and reacting same at 70ºC-99ºC to obtain a mixture of nickel carbonate and a mother liquor; step 3, putting the above-mentioned mixture of nickel carbonate and a mother liquor into a centrifuge to remove the mother liquor so as to obtain a nickel carbonate crude product; and step 4, successively eluting and washing the above-mentioned nickel carbonate crude product with a base solution and pure water, respectively, and drying and sieving same to obtain the high-density basic nickel carbonate. In the present invention, by selecting single sodium carbonate as a precipitant, NH4+ is not introduced in the whole reaction system, reducing the kinds of impurities present in the obtained basic nickel carbonate.

Description

一种高密度碱式碳酸镍的制备方法Preparation method of high-density basic nickel carbonate 技术领域Technical field
本发明属于碱式碳酸镍的合成技术领域，具体涉及一种高密度碱式碳酸镍的制备方法。The invention belongs to the technical field of synthesis of basic nickel carbonate, and in particular relates to a preparation method of high-density basic nickel carbonate.
背景技术Background technique
碱式碳酸镍是一种重要的无机精细化学品，主要用于制备各种镍盐，高品质碱式碳酸镍，可应用于电子类行业、催化剂行业；此外，碱式碳酸镍还广泛用于电镀、电铸、瓷釉颜料等。Basic nickel carbonate is an important inorganic fine chemical, mainly used in the preparation of various nickel salts, high-quality basic nickel carbonate, which can be used in the electronics industry and catalyst industry. In addition, basic nickel carbonate is also widely used. Electroplating, electroforming, enamel pigments, etc.
碱式碳酸镍沉淀剂一般是碳酸钠、碳酸铵（或碳酸氢铵）；采用碳酸铵（或碳酸氢铵）为沉淀剂，原料便宜，得到的碳酸镍粒度细，但是镍的转化率不高，母液须回收，碳酸镍密度低；而采用碳酸钠为沉淀剂，原料易得价廉，镍盐转化率高，成本较低，具有很好的经济效益。The basic nickel carbonate precipitating agent is generally sodium carbonate, ammonium carbonate (or ammonium hydrogencarbonate); using ammonium carbonate (or ammonium hydrogencarbonate) as a precipitating agent, the raw material is cheap, and the obtained nickel carbonate has a fine particle size, but the conversion rate of nickel is not high. The mother liquor must be recovered, and the density of nickel carbonate is low; while sodium carbonate is used as a precipitant, the raw materials are easy to obtain cheap, the conversion rate of nickel salt is high, the cost is low, and the economic benefit is good.
加氢脱硫催化行业用碱式碳酸镍对Na、S、Cl含量有很高的要求，同时对碱式碳酸镍Ni含量要求在44%~48%，松装密度大于0.8g/cm 3；但现有技术获得的碱式碳酸镍中Ni含量均大于48%且制备过程中多选用铵盐作为沉淀剂，这样容易导致杂质元素种类多、不易洗涤、杂质含量高、洗涤流程长、生产成本高，且氨的引入增加了废水处理成本。 In the hydrodesulfurization catalytic industry, the basic nickel carbonate has high requirements for Na, S and Cl content, and the Ni content of basic nickel carbonate is required to be 44%~48%, and the bulk density is greater than 0.8g/cm 3 ; The content of Ni in the basic nickel carbonate obtained by the prior art is more than 48%, and the ammonium salt is often used as a precipitant in the preparation process, which easily leads to many kinds of impurity elements, is not easy to be washed, has high impurity content, long washing process and high production cost. And the introduction of ammonia increases the cost of wastewater treatment.
技术问题technical problem
有鉴于此，本发明的主要目的在于提供一种高密度碱式碳酸镍的制备方法，解决了现有技术碱式碳酸镍中杂质种类多、含量大、不易清洗、生产成本高的问题。In view of this, the main object of the present invention is to provide a method for preparing high-density basic nickel carbonate, which solves the problems of the prior art basic nickel carbonate having many types of impurities, large content, difficulty in cleaning, and high production cost.
技术解决方案Technical solution
为达到上述目的，本发明的技术方案是这样实现的：一种高密度碱式碳酸镍的制备方法，该方法通过如下步骤实现：In order to achieve the above object, the technical solution of the present invention is achieved by a method for preparing high-density basic nickel carbonate, which is achieved by the following steps:
步骤1，在溶液罐中分别配制碳酸离子浓度为100~250g/L的碳酸钠溶液和镍离子浓度为1~2moL/L的镍盐溶液；Step 1. Prepare a sodium carbonate solution having a carbonate ion concentration of 100 to 250 g/L and a nickel salt solution having a nickel ion concentration of 1 to 2 mol/L in the solution tank;
步骤2，用计量泵进料，将碳酸钠溶液和镍盐溶液同时加入特制的反应器中，进料过程中保持镍盐溶液的流量不变，通过调节碳酸钠溶液的流量控制体系的pH值，并在70~99℃下进行反应，获得碳酸镍与母液的混合物；Step 2, feeding with a metering pump, adding the sodium carbonate solution and the nickel salt solution to the special reactor at the same time, keeping the flow rate of the nickel salt solution unchanged during the feeding process, and adjusting the pH value of the flow rate control system by adjusting the flow rate of the sodium carbonate solution And reacting at 70 to 99 ° C to obtain a mixture of nickel carbonate and mother liquor;
步骤3，将步骤2获得的碳酸镍与母液的混合物打入离心机脱去母液，获得碳酸镍粗品；Step 3, the mixture of the nickel carbonate and the mother liquid obtained in the step 2 is driven into a centrifuge to remove the mother liquid to obtain a crude nickel carbonate;
步骤4，分别依次用质量分数为0.1~5.5%的碱液、纯水淋洗和洗涤步骤3获得的碳酸镍粗品，烘干、过筛，获得高密度碱式碳酸镍。In step 4, the crude nickel carbonate obtained in the step 3 is rinsed and washed with lye, pure water having a mass fraction of 0.1 to 5.5%, dried, and sieved to obtain a high-density basic nickel carbonate.
优选地，所述步骤1中，所述镍盐为氯化镍、硫酸镍、硝酸镍中的至少一种。Preferably, in the step 1, the nickel salt is at least one of nickel chloride, nickel sulfate, and nickel nitrate.
优选地，所述步骤2中，计量泵进料时，所述碳酸钠溶液的流量为5~1000L/h，所述镍盐溶液的流量为50~1000L/h。Preferably, in the step 2, when the metering pump is fed, the flow rate of the sodium carbonate solution is 5~1000 L/h, and the flow rate of the nickel salt solution is 50~1000 L/h.
优选地，所述步骤2中，所述pH值为8.0~8.3。Preferably, in the step 2, the pH is 8.0~8.3.
优选地，所述步骤2中，所述反应时间为8~18h。Preferably, in the step 2, the reaction time is 8-18 h.
优选地，所述步骤4中，所述碱液的温度为40~70℃；所述纯水的温度为70~85℃，所述纯水的电导率≤100μs/m。Preferably, in the step 4, the temperature of the alkali liquid is 40 to 70 ° C; the temperature of the pure water is 70 to 85 ° C, and the conductivity of the pure water is ≤ 100 μs / m.
优选地，所述步骤4中，所述烘干的温度为95~105℃，所述烘干的时间为2~3h。Preferably, in the step 4, the drying temperature is 95-105 ° C, and the drying time is 2~3 h.
优选地，所述步骤4中，所述过筛时选用200~400目的筛子。Preferably, in the step 4, the sieve is selected from 200 to 400 mesh.
优选地，所述步骤4中，所述高密度碱式碳酸镍的松装密度为 0.8~1.3g/cm 3。 Preferably, in the step 4, the bulk density of the high-density basic nickel carbonate is 0.8-1.3 g/cm 3 .
有益效果Beneficial effect
与现有技术相比，本发明通过选用单一的碳酸钠作为沉淀剂，整个反应体系中未引入NH4+，使得获得的碱式碳酸镍中杂质种类少；通过依次用温度为40~70℃且质量分数为0.1~5.5%的碱液和温度为70~85℃且电导率≤100μs/m的纯水淋洗和洗涤碱式碳酸镍粗品，解决了现有技术中不易清洗、生产成本高的问题，并且获得的碱式碳酸镍中Na、Cl元素含量少，能够很好的应用于加氢脱硫催化行业。Compared with the prior art, the invention adopts a single sodium carbonate as a precipitating agent, and NH4+ is not introduced into the whole reaction system, so that the obtained basic nickel carbonate has few kinds of impurities; the temperature is 40-70 ° C and the quality is sequentially used. The lye with a fraction of 0.1 to 5.5% and the pure water leaching and washing of the basic nickel carbonate with a temperature of 70-85 ° C and a conductivity of ≤ 100 μs / m solve the problem that the prior art is difficult to clean and the production cost is high. And the obtained basic nickel carbonate has a small content of Na and Cl elements, and can be well applied to the hydrodesulfurization catalytic industry.
附图说明DRAWINGS
图1为本发明实施例1获得的高密度碱式碳酸镍的显微镜图。BRIEF DESCRIPTION OF THE DRAWINGS Figure 1 is a micrograph of a high-density basic nickel carbonate obtained in Example 1 of the present invention.
本发明的最佳实施方式BEST MODE FOR CARRYING OUT THE INVENTION
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合附图及实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。The present invention will be further described in detail below with reference to the accompanying drawings and embodiments. It is understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
本发明提供了实施例提供了一种高密度碱式碳酸镍的制备方法，该方法通过如下步骤实现：The present invention provides an embodiment to provide a method for preparing high-density basic nickel carbonate, which is achieved by the following steps:
步骤1，在溶液罐中分别配制碳酸离子浓度为100~250g/L的碳酸钠溶液和镍离子浓度为1~2moL/L的镍盐溶液；其中，镍盐为氯化镍、硫酸镍、硝酸镍中的至少一种；Step 1. Prepare a sodium carbonate solution having a carbonate ion concentration of 100 to 250 g/L and a nickel salt solution having a nickel ion concentration of 1 to 2 mol/L in the solution tank; wherein the nickel salt is nickel chloride, nickel sulfate, and nitric acid. At least one of nickel;
步骤2，用计量泵进料，将碳酸钠溶液和镍盐溶液同时加入特制的反应器中，进料过程中保持镍盐溶液的流量为50~1000L/h不变，通过调节碳酸钠溶液的流量控制体系的pH值为8.0~8.3，并在70~99℃下反应8~18h，获得碳酸镍与母液的混合物；其中，碳酸钠溶液的流量的调节范围为50~1000L/h；Step 2, feeding with a metering pump, adding the sodium carbonate solution and the nickel salt solution to the special reactor at the same time, keeping the flow rate of the nickel salt solution unchanged during the feeding process is 50-1000 L/h, by adjusting the sodium carbonate solution. The pH of the flow control system is 8.0~8.3, and the reaction is carried out at 70~99 °C for 8~18h to obtain a mixture of nickel carbonate and mother liquor; wherein the flow rate of the sodium carbonate solution is adjusted to range from 50 to 1000 L/h;
步骤3，将步骤2获得的碳酸镍与母液的混合物打入离心机脱去母液，获得碳酸镍粗品；Step 3, the mixture of the nickel carbonate and the mother liquid obtained in the step 2 is driven into a centrifuge to remove the mother liquid to obtain a crude nickel carbonate;
步骤4，分别依次用温度为40~70℃且质量分数为0.1~5.5%的碱液、温度为70~85℃且电导率≤100μs/m的纯水淋洗和洗涤步骤3获得的碳酸镍粗品，再在95~105℃下干燥2~3h、过200~400目筛子，获得松装密度为 0.8~1.3g/cm 3高密度碱式碳酸镍。 Step 4, respectively, using the lye at a temperature of 40 to 70 ° C and having a mass fraction of 0.1 to 5.5%, the pure water leaching and washing step 3 obtained at a temperature of 70 to 85 ° C and a conductivity of ≤ 100 μs/m. The crude product is dried at 95-105 ° C for 2~3 hours and passed through a 200-400 mesh sieve to obtain a high-density basic nickel carbonate with a bulk density of 0.8-1.3 g/cm 3 .
本发明通过选用单一的碳酸钠作为沉淀剂，整个反应体系中未引入NH+4，使得获得的碱式碳酸镍中杂质种类少；通过依次用温度为40~70℃且质量分数为0.1~5.5%的碱液和温度为70~85℃且电导率≤100μs/m的纯水淋洗和洗涤碱式碳酸镍粗品，解决了现有技术中不易清洗、生产成本高的问题，并且获得的碱式碳酸镍中Na、Cl元素含量少，能够很好的应用于加氢脱硫催化行业。The invention adopts a single sodium carbonate as a precipitating agent, and NH+4 is not introduced into the whole reaction system, so that the obtained basic nickel carbonate has few kinds of impurities; the temperature is 40-70° C. and the mass fraction is 0.1-5.5. % alkali solution and pure water rinsing and washing basic nickel carbonate with a temperature of 70-85 ° C and conductivity ≤ 100 μs / m, solving the problem that the prior art is difficult to clean, high production cost, and the obtained alkali The nickel carbonate type has a small content of Na and Cl, and can be well applied to the hydrodesulfurization catalytic industry.
实施例1Example 1
一种高密度碱式碳酸镍的制备方法，该方法通过如下步骤实现：A method for preparing high-density basic nickel carbonate, which is achieved by the following steps:
步骤1，在溶液罐中分别配制碳酸离子浓度150g/L的碳酸钠溶液和镍离子浓度为1.5mol/L的氯化镍溶液；Step 1, in the solution tank, respectively, a sodium carbonate solution having a carbonate ion concentration of 150 g/L and a nickel chloride solution having a nickel ion concentration of 1.5 mol/L;
步骤2，用计量泵进料，将碳酸钠溶液和氯化镍溶液同时加入特制的反应器中（该反应器在反应过程中可流出母液，并保证碳酸镍与母液构成的反应体系的固含量不断增加），进料过程中保持镍盐溶液的流量为50L/h不变，通过调节碳酸钠溶液的流量（碳酸钠溶液的流量的调节范围为50~1000L/h）控制体系的pH值为8.1，并在80℃下反应15h，获得碳酸镍与母液的混合物；Step 2, using a metering pump feed, the sodium carbonate solution and the nickel chloride solution are simultaneously added to a special reactor (the reactor can flow out of the mother liquor during the reaction, and ensure the solid content of the reaction system composed of nickel carbonate and mother liquor) Increasingly), the flow rate of the nickel salt solution is kept constant at 50 L/h during the feeding process, and the pH of the control system is controlled by adjusting the flow rate of the sodium carbonate solution (the flow rate of the sodium carbonate solution is adjusted to 50 to 1000 L/h) 8.1, and reacted at 80 ° C for 15 h to obtain a mixture of nickel carbonate and mother liquor;
步骤3，将步骤2获得的碳酸镍与母液的混合物打入离心机脱去母液，获得碳酸镍粗品；Step 3, the mixture of the nickel carbonate and the mother liquid obtained in the step 2 is driven into a centrifuge to remove the mother liquid to obtain a crude nickel carbonate;
步骤4，分别依次用温度为55℃且质量分数为2.5%的碱液、温度为80℃且电导率≤100μs/m的纯水淋洗和洗涤步骤3获得的碳酸镍粗品，再在100℃下干燥2.5h、过300目筛子，获得松装密度为1.0g/cm 3高密度碱式碳酸镍。 Step 4, respectively, using a lye having a temperature of 55 ° C and a mass fraction of 2.5%, a pure water having a temperature of 80 ° C and a conductivity of ≤ 100 μs / m, and washing the crude nickel carbonate obtained in the step 3, and then at 100 ° C After drying for 2.5 h and passing through a 300 mesh sieve, a high density basic nickel carbonate having a bulk density of 1.0 g/cm 3 was obtained.
实施例2Example 2
一种高密度碱式碳酸镍的制备方法，该方法通过如下步骤实现：A method for preparing high-density basic nickel carbonate, which is achieved by the following steps:
步骤1，在溶液罐中分别配制碳酸离子浓度150g/L的碳酸钠溶液和镍离子浓度为1.5mol/L的氯化镍溶液；Step 1, in the solution tank, respectively, a sodium carbonate solution having a carbonate ion concentration of 150 g/L and a nickel chloride solution having a nickel ion concentration of 1.5 mol/L;
步骤2，用计量泵进料，将碳酸钠溶液和氯化镍溶液同时加入特制的反应器中（该反应器在反应过程中可流出母液，并保证碳酸镍与母液构成的反应体系的固含量不断增加），进料过程中保持镍盐溶液的流量为50L/h不变，通过调节碳酸钠溶液的流量（碳酸钠溶液的流量的调节范围为50~1000L/h）控制体系的pH值为8.0，并在99℃下反应8h，获得碳酸镍与母液的混合物；Step 2, using a metering pump feed, the sodium carbonate solution and the nickel chloride solution are simultaneously added to a special reactor (the reactor can flow out of the mother liquor during the reaction, and ensure the solid content of the reaction system composed of nickel carbonate and mother liquor) Increasingly), the flow rate of the nickel salt solution is kept constant at 50 L/h during the feeding process, and the pH of the control system is controlled by adjusting the flow rate of the sodium carbonate solution (the flow rate of the sodium carbonate solution is adjusted to 50 to 1000 L/h) 8.0, and reacted at 99 ° C for 8 h to obtain a mixture of nickel carbonate and mother liquor;
步骤3，将步骤2获得的碳酸镍与母液的混合物打入离心机脱去母液，获得碳酸镍粗品；Step 3, the mixture of the nickel carbonate and the mother liquid obtained in the step 2 is driven into a centrifuge to remove the mother liquid to obtain a crude nickel carbonate;
4，分别依次用温度为40℃且质量分数为5.5%的碱液、温度为70℃且电导率≤100μs/m的纯水淋洗和洗涤步骤3获得的碳酸镍粗品，再在95℃下干燥3h、过300目筛子，获得松装密度为0.9g/cm 3高密度碱式碳酸镍。 4, respectively, using a lye solution having a temperature of 40 ° C and a mass fraction of 5.5%, a pure water rinse at a temperature of 70 ° C and a conductivity of ≤ 100 μs / m, and a crude nickel carbonate obtained in the washing step 3, and then at 95 ° C After drying for 3 hours and passing through a 300 mesh sieve, a high density basic nickel carbonate having a bulk density of 0.9 g/cm 3 was obtained.
步骤实施例3Step embodiment 3
一种高密度碱式碳酸镍的制备方法，该方法通过如下步骤实现：A method for preparing high-density basic nickel carbonate, which is achieved by the following steps:
步骤1，在溶液罐中分别配制碳酸离子浓度150g/L的碳酸钠溶液和镍离子浓度为1.5mol/L的氯化镍溶液；Step 1, in the solution tank, respectively, a sodium carbonate solution having a carbonate ion concentration of 150 g/L and a nickel chloride solution having a nickel ion concentration of 1.5 mol/L;
步骤2，用计量泵进料，将碳酸钠溶液和氯化镍溶液同时加入特制的反应器中（该反应器在反应过程中可流出母液，并保证碳酸镍与母液构成的反应体系的固含量不断增加），进料过程中保持镍盐溶液的流量为50L/h不变，通过调节碳酸钠溶液的流量（碳酸钠溶液的流量的调节范围为50~1000L/h）控制体系的pH值为8.3，并在70℃下反应18h，获得碳酸镍与母液的混合物；Step 2, using a metering pump feed, the sodium carbonate solution and the nickel chloride solution are simultaneously added to a special reactor (the reactor can flow out of the mother liquor during the reaction, and ensure the solid content of the reaction system composed of nickel carbonate and mother liquor) Increasingly), the flow rate of the nickel salt solution is kept constant at 50 L/h during the feeding process, and the pH of the control system is controlled by adjusting the flow rate of the sodium carbonate solution (the flow rate of the sodium carbonate solution is adjusted to 50 to 1000 L/h) 8.3, and reacted at 70 ° C for 18 h to obtain a mixture of nickel carbonate and mother liquor;
步骤3，将步骤2获得的碳酸镍与母液的混合物打入离心机脱去母液，获得碳酸镍粗品；Step 3, the mixture of the nickel carbonate and the mother liquid obtained in the step 2 is driven into a centrifuge to remove the mother liquid to obtain a crude nickel carbonate;
步骤4，分别依次用温度为70℃且质量分数为0.1%的碱液、温度为5℃且电导率≤100μs/m的纯水淋洗和洗涤步骤3获得的碳酸镍粗品，再在105℃下干燥2h、过300目筛子，获得松装密度为0.8g/cm 3高密度碱式碳酸镍。 Step 4, respectively, using a lye solution having a temperature of 70 ° C and a mass fraction of 0.1%, a pure water having a temperature of 5 ° C and a conductivity of ≤ 100 μs / m, and a crude nickel carbonate obtained by washing step 3, and then at 105 ° C. After drying for 2 hours and passing through a 300 mesh sieve, a high density basic nickel carbonate having a bulk density of 0.8 g/cm 3 was obtained.
实施例4Example 4
一种高密度碱式碳酸镍的制备方法，该方法通过如下步骤实现：A method for preparing high-density basic nickel carbonate, which is achieved by the following steps:
步骤1，在溶液罐中分别配制碳酸离子浓度为100g/L的碳酸钠溶液和镍离子浓度为1mol/L的氯化镍溶液；Step 1, preparing a sodium carbonate solution having a carbonate ion concentration of 100 g/L and a nickel chloride solution having a nickel ion concentration of 1 mol/L in the solution tank;
步骤2，用计量泵进料，将碳酸钠溶液和氯化镍溶液同时加入特制的反应器中（该反应器在反应过程中可流出母液，并保证碳酸镍与母液构成的反应体系的固含量不断增加），进料过程中保持镍盐溶液的流量为800L/h不变，通过调节碳酸钠溶液的流量（碳酸钠溶液的流量的调节范围为50~1000L/h）控制体系的pH值为8.1，并在80℃下反应15h，获得碳酸镍与母液的混合物；Step 2, using a metering pump feed, the sodium carbonate solution and the nickel chloride solution are simultaneously added to a special reactor (the reactor can flow out of the mother liquor during the reaction, and ensure the solid content of the reaction system composed of nickel carbonate and mother liquor) Increasingly), the flow rate of the nickel salt solution is kept constant at 800 L/h during the feeding process, and the pH of the control system is controlled by adjusting the flow rate of the sodium carbonate solution (the flow rate of the sodium carbonate solution is adjusted to 50 to 1000 L/h) 8.1, and reacted at 80 ° C for 15 h to obtain a mixture of nickel carbonate and mother liquor;
步骤3，将步骤2获得的碳酸镍与母液的混合物打入离心机脱去母液，获得碳酸镍粗品；Step 3, the mixture of the nickel carbonate and the mother liquid obtained in the step 2 is driven into a centrifuge to remove the mother liquid to obtain a crude nickel carbonate;
步骤4，分别依次用温度为55℃且质量分数为2.5%的碱液、温度为80℃且电导率≤100μs/m的纯水淋洗和洗涤步骤3获得的碳酸镍粗品，再在100℃下干燥2.5h、过300目筛子，获得松装密度为1.2g/cm 3高密度碱式碳酸镍。 Step 4, respectively, using a lye having a temperature of 55 ° C and a mass fraction of 2.5%, a pure water having a temperature of 80 ° C and a conductivity of ≤ 100 μs / m, and washing the crude nickel carbonate obtained in the step 3, and then at 100 ° C After drying for 2.5 hours and passing through a 300 mesh sieve, a high density basic nickel carbonate having a bulk density of 1.2 g/cm 3 was obtained.
实施例5Example 5
一种高密度碱式碳酸镍的制备方法，该方法通过如下步骤实现：A method for preparing high-density basic nickel carbonate, which is achieved by the following steps:
步骤1，在溶液罐中分别配制碳酸离子浓度为100g/L的碳酸钠溶液和镍离子浓度为1mol/L的氯化镍溶液；Step 1, preparing a sodium carbonate solution having a carbonate ion concentration of 100 g/L and a nickel chloride solution having a nickel ion concentration of 1 mol/L in the solution tank;
步骤2，用计量泵进料，将碳酸钠溶液和氯化镍溶液同时加入特制的反应器中（该反应器在反应过程中可流出母液，并保证碳酸镍与母液构成的反应体系的固含量不断增加），进料过程中保持镍盐溶液的流量为800L/h不变，通过调节碳酸钠溶液的流量（碳酸钠溶液的流量的调节范围为50~1000L/h）控制体系的pH值为8.0，并在99℃下反应8h，获得碳酸镍与母液的混合物；Step 2, using a metering pump feed, the sodium carbonate solution and the nickel chloride solution are simultaneously added to a special reactor (the reactor can flow out of the mother liquor during the reaction, and ensure the solid content of the reaction system composed of nickel carbonate and mother liquor) Increasingly), the flow rate of the nickel salt solution is kept constant at 800 L/h during the feeding process, and the pH of the control system is controlled by adjusting the flow rate of the sodium carbonate solution (the flow rate of the sodium carbonate solution is adjusted to 50 to 1000 L/h) 8.0, and reacted at 99 ° C for 8 h to obtain a mixture of nickel carbonate and mother liquor;
步骤3，将步骤2获得的碳酸镍与母液的混合物打入离心机脱去母液，获得碳酸镍粗品；Step 3, the mixture of the nickel carbonate and the mother liquid obtained in the step 2 is driven into a centrifuge to remove the mother liquid to obtain a crude nickel carbonate;
步骤4，分别依次用温度为40℃且质量分数为5.5%的碱液、温度为70℃且电导率≤100μs/m的纯水淋洗和洗涤步骤3获得的碳酸镍粗品，再在95℃下干燥3h、过300目筛子，获得松装密度为1.1g/cm 3高密度碱式碳酸镍。 Step 4, respectively, using a lye solution having a temperature of 40 ° C and a mass fraction of 5.5%, a pure water having a temperature of 70 ° C and a conductivity of ≤ 100 μs / m, and a crude nickel carbonate obtained by the washing step 3, and then at 95 ° C. After drying for 3 hours and passing through a 300 mesh sieve, a high density basic nickel carbonate having a bulk density of 1.1 g/cm 3 was obtained.
实施例6Example 6
一种高密度碱式碳酸镍的制备方法，该方法通过如下步骤实现：A method for preparing high-density basic nickel carbonate, which is achieved by the following steps:
步骤1，在溶液罐中分别配制碳酸离子浓度为100g/L的碳酸钠溶液和镍离子浓度为1mol/L的氯化镍溶液；Step 1, preparing a sodium carbonate solution having a carbonate ion concentration of 100 g/L and a nickel chloride solution having a nickel ion concentration of 1 mol/L in the solution tank;
步骤2，用计量泵进料，将碳酸钠溶液和氯化镍溶液同时加入特制的反应器中（该反应器在反应过程中可流出母液，并保证碳酸镍与母液构成的反应体系的固含量不断增加），进料过程中保持镍盐溶液的流量为800L/h不变，通过调节碳酸钠溶液的流量（碳酸钠溶液的流量的调节范围为50~1000L/h）控制体系的pH值为8.3，并在70℃下反应18h，获得碳酸镍与母液的混合物；Step 2, using a metering pump feed, the sodium carbonate solution and the nickel chloride solution are simultaneously added to a special reactor (the reactor can flow out of the mother liquor during the reaction, and ensure the solid content of the reaction system composed of nickel carbonate and mother liquor) Increasingly), the flow rate of the nickel salt solution is kept constant at 800 L/h during the feeding process, and the pH of the control system is controlled by adjusting the flow rate of the sodium carbonate solution (the flow rate of the sodium carbonate solution is adjusted to 50 to 1000 L/h) 8.3, and reacted at 70 ° C for 18 h to obtain a mixture of nickel carbonate and mother liquor;
步骤3，将步骤2获得的碳酸镍与母液的混合物打入离心机脱去母液，获得碳酸镍粗品；Step 3, the mixture of the nickel carbonate and the mother liquid obtained in the step 2 is driven into a centrifuge to remove the mother liquid to obtain a crude nickel carbonate;
步骤4，分别依次用温度为70℃且质量分数为0.1%的碱液、温度为5℃且电导率≤100μs/m的纯水淋洗和洗涤步骤3获得的碳酸镍粗品，再在105℃下干燥2h、过300目筛子，获得松装密度为1.3g/cm 3高密度碱式碳酸镍。 Step 4, respectively, using a lye solution having a temperature of 70 ° C and a mass fraction of 0.1%, a pure water having a temperature of 5 ° C and a conductivity of ≤ 100 μs / m, and a crude nickel carbonate obtained by washing step 3, and then at 105 ° C. After drying for 2 hours and passing through a 300 mesh sieve, a high density basic nickel carbonate having a bulk density of 1.3 g/cm 3 was obtained.
实施例7Example 7
一种高密度碱式碳酸镍的制备方法，该方法通过如下步骤实现：A method for preparing high-density basic nickel carbonate, which is achieved by the following steps:
步骤1，在溶液罐中分别配制碳酸离子浓度为250g/L的碳酸钠溶液和镍离子浓度为2mol/L的硝酸镍溶液；Step 1, preparing a sodium carbonate solution having a carbonate ion concentration of 250 g/L and a nickel nitrate solution having a nickel ion concentration of 2 mol/L in the solution tank;
步骤2，用计量泵进料，将碳酸钠溶液和氯化镍溶液同时加入特制的反应器中（该反应器在反应过程中可流出母液，并保证碳酸镍与母液构成的反应体系的固含量不断增加），进料过程中保持镍盐溶液的流量为50L/h不变，通过调节碳酸钠溶液的流量（碳酸钠溶液的流量的调节范围为50~1000L/h）控制体系的pH值为8.0，并在99℃下反应8h，获得碳酸镍与母液的混合物；Step 2, using a metering pump feed, the sodium carbonate solution and the nickel chloride solution are simultaneously added to a special reactor (the reactor can flow out of the mother liquor during the reaction, and ensure the solid content of the reaction system composed of nickel carbonate and mother liquor) Increasingly), the flow rate of the nickel salt solution is kept constant at 50 L/h during the feeding process, and the pH of the control system is controlled by adjusting the flow rate of the sodium carbonate solution (the flow rate of the sodium carbonate solution is adjusted to 50 to 1000 L/h) 8.0, and reacted at 99 ° C for 8 h to obtain a mixture of nickel carbonate and mother liquor;
步骤3，将步骤2获得的碳酸镍与母液的混合物打入离心机脱去母液，获得碳酸镍粗品；Step 3, the mixture of the nickel carbonate and the mother liquid obtained in the step 2 is driven into a centrifuge to remove the mother liquid to obtain a crude nickel carbonate;
步骤4，分别依次用温度为40℃且质量分数为5.5%的碱液、温度为70℃且电导率≤100μs/m的纯水淋洗和洗涤步骤3获得的碳酸镍粗品，再在95℃下干燥3h、过300目筛子，获得松装密度为1.0g/cm 3高密度碱式碳酸镍。 Step 4, respectively, using a lye solution having a temperature of 40 ° C and a mass fraction of 5.5%, a pure water having a temperature of 70 ° C and a conductivity of ≤ 100 μs / m, and a crude nickel carbonate obtained by the washing step 3, and then at 95 ° C. After drying for 3 hours and passing through a 300 mesh sieve, a high density basic nickel carbonate having a bulk density of 1.0 g/cm 3 was obtained.
对实施例1获得的高密度碱式碳酸镍用显微镜观察其结构，观察结果如图1所示；对实施例1-实施例7获得的碱式碳酸镍进行Na、Ni、CI含量的检测，检测结果如表1所示：The structure of the high-density basic nickel carbonate obtained in Example 1 was observed under a microscope, and the observation results are shown in FIG. 1; the basic nickel carbonate obtained in Example 1 - Example 7 was subjected to detection of Na, Ni, and CI contents, The test results are shown in Table 1:
表1为本发明实施例1-实施例7获得的碱式碳酸镍的物理性能检测数据Table 1 shows the physical property detection data of the basic nickel carbonate obtained in Example 1 to Example 7 of the present invention.
  Na离子含量/%Na ion content /% CI离子含量/%CI ion content /% Ni离子含量/%Ni ion content /% 松装密度/g/cm 3 Bulk density / g / cm 3
实施1Implementation 1 0.015%0.015% 0.0026%0.0026% 45%45% 1.0g/cm 3 1.0g/cm 3
实施2Implementation 2 0.018%0.018% 0.0024%0.0024% 44%44% 0.9g/cm 3 0.9g/cm 3
实施3Implementation 3 0.016%0.016% 0.0027%0.0027% 46%46% 0.8g/cm 3 0.8g/cm 3
实施4Implementation 4 0.015%0.015% 0.0025%0.0025% 47%47% 1.2g/cm 3 1.2g/cm 3
实施5Implementation 5 0.017%0.017% 0.0028%0.0028% 43%43% 1.1g/cm 3 1.1g/cm 3
实施6Implementation 6 0.016%0.016% 0.0029%0.0029% 45%45% 1.3g/cm 3 1.3g/cm 3
实施7Implementation 7 0.018%0.018% 0.0027%0.0027% 44%44% 1.0g/cm 3 1.0g/cm 3
常规conventional 0.025%0.025% 0.0036%0.0036% 41%41% 0.5g/cm 3 0.5g/cm 3
从图1以及表1中可以看出，本发明获得的碱式碳酸镍呈类球状颗粒且其中的Na≤0.0200%、44%≤Ni≤48%、Cl≤0.0030%，由此可见，本发明获得的碱式碳酸镍的各项性能均优于现有方法获得的碱式碳酸镍的各项性能。It can be seen from FIG. 1 and Table 1 that the basic nickel carbonate obtained by the present invention is spherical-like particles and wherein Na≤0.0200%, 44%≤Ni≤48%, Cl≤0.0030%, it can be seen that the present invention The properties of the obtained basic nickel carbonate are superior to those of the basic nickel carbonate obtained by the prior art.
以上所述，仅为本发明的较佳实施例而已，并非用于限定本发明的保护范围。The above is only the preferred embodiment of the present invention and is not intended to limit the scope of the present invention.

Claims (9)

  1. 一种高密度碱式碳酸镍的制备方法，其特征在于，该方法通过如下步骤实现：步骤1，在溶液罐中分别配制碳酸离子浓度为100~250g/L的碳酸钠溶液和镍离子浓度为1~2moL/L的镍盐溶液；步骤2，用计量泵进料，将碳酸钠溶液和镍盐溶液同时加入特制的反应器中，进料过程中保持镍盐溶液的流量不变，通过调节碳酸钠溶液的流量控制体系的pH值，并在70~99℃下进行反应，获得碳酸镍与母液的混合物；步骤3，将步骤2获得的碳酸镍与母液的混合物打入离心机脱去母液，获得碳酸镍粗品；步骤4，分别依次用质量分数为0.1~5.5%的碱液、纯水淋洗和洗涤步骤3获得的碳酸镍粗品，烘干、过筛，获得高密度碱式碳酸镍。The invention relates to a method for preparing high-density basic nickel carbonate, which is characterized in that: the method comprises the steps of: preparing a sodium carbonate solution having a carbonate ion concentration of 100-250 g/L and a nickel ion concentration in a solution tank; 1~2moL/L nickel salt solution; Step 2, feed with a metering pump, add sodium carbonate solution and nickel salt solution to the special reactor at the same time, keep the flow rate of the nickel salt solution unchanged during the feeding process, and adjust The flow rate of the sodium carbonate solution is controlled by the pH of the system, and the reaction is carried out at 70 to 99 ° C to obtain a mixture of nickel carbonate and the mother liquid; in step 3, the mixture of the nickel carbonate and the mother liquid obtained in the step 2 is centrifuged to remove the mother liquor. Obtaining crude nickel carbonate; step 4, sequentially rinsing and washing the crude nickel carbonate obtained in step 3 with lye, pure water having a mass fraction of 0.1 to 5.5%, drying and sieving to obtain high-density basic nickel carbonate .
  2. 根据权利要求1所述的一种高密度碱式碳酸镍的制备方法，其特征在于，所述步骤1中，所述镍盐为氯化镍、硫酸镍、硝酸镍中的至少一种。The method for preparing a high-density basic nickel carbonate according to claim 1, wherein in the step 1, the nickel salt is at least one of nickel chloride, nickel sulfate, and nickel nitrate.
  3. 根据权利要求2所述的一种高密度碱式碳酸镍的制备方法，其特征在于，所述步骤2中，计量泵进料时，所述碳酸钠溶液的流量为5~1000L/h，所述镍盐溶液的流量为50~1000L/h。The method for preparing high-density basic nickel carbonate according to claim 2, wherein in the step 2, when the metering pump is fed, the flow rate of the sodium carbonate solution is 5 to 1000 L/h. The flow rate of the nickel salt solution is 50 to 1000 L/h.
  4. 根据权利要求3所述的一种高密度碱式碳酸镍的制备方法，其特征在于，所述步骤2中，所述pH值为8.0~8.3。The method for preparing high-density basic nickel carbonate according to claim 3, wherein in the step 2, the pH is 8.0 to 8.3.
  5. 根据权利要求4所述的一种高密度碱式碳酸镍的制备方法，其特征在于，所述步骤2中，所述反应时间为8~18h。The method for preparing high-density basic nickel carbonate according to claim 4, wherein in the step 2, the reaction time is 8 to 18 hours.
  6. 根据权利要求5所述的一种高密度碱式碳酸镍的制备方法，其特征在于，所述步骤4中，所述碱液的温度为40~70℃；所述纯水的温度为70~85℃，所述纯水的电导率≤100μs/m。The method for preparing high-density basic nickel carbonate according to claim 5, wherein in the step 4, the temperature of the alkali liquid is 40 to 70 ° C; and the temperature of the pure water is 70 to At 85 ° C, the conductivity of the pure water is ≤ 100 μs / m.
  7. 根据权利要求6所述的种高密度碱式碳酸镍的制备方法，其特征在于，所述步骤4中，所述烘干的温度为95~105℃，所述烘干的时间为2~3h。The method for preparing a high-density basic nickel carbonate according to claim 6, wherein in the step 4, the drying temperature is 95 to 105 ° C, and the drying time is 2 to 3 hours. .
  8. 根据权利要求7任意一项所述的种高密度碱式碳酸镍的制备方法，其特征在于，所述步骤4中，所述过筛时选用200~400目的筛子。The method for preparing a high-density basic nickel carbonate according to any one of claims 7 to 4, wherein in the step 4, a sieve of 200 to 400 mesh is used for the sieving.
  9. 根据权利要求1-8任意一项所述的种高密度碱式碳酸镍的制备方法，其特征在于，所述步骤4中，所述高密度碱式碳酸镍的松装密度为 0.8~1.3g/cm 3。 The method for preparing a high-density basic nickel carbonate according to any one of claims 1 to 8, wherein in the step 4, the bulk density of the high-density basic nickel carbonate is 0.8 to 1.3 g. /cm 3 .
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CN110564977A (en) * 2019-08-15 2019-12-13 广州科城环保科技有限公司 Method for recovering nickel resource from chemical nickel waste liquid
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