WO2020244181A1 - 一种高分散高导热白炭黑的制备方法 - Google Patents

一种高分散高导热白炭黑的制备方法 Download PDF

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WO2020244181A1
WO2020244181A1 PCT/CN2019/122964 CN2019122964W WO2020244181A1 WO 2020244181 A1 WO2020244181 A1 WO 2020244181A1 CN 2019122964 W CN2019122964 W CN 2019122964W WO 2020244181 A1 WO2020244181 A1 WO 2020244181A1
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sodium silicate
value
mother liquor
preparation
gradient
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French (fr)
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王永庆
毛善兵
于方琪
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确成硅化学股份有限公司
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • C01B33/187—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
    • C01B33/193—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates of aqueous solutions of silicates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/309—Combinations of treatments provided for in groups C09C1/3009 - C09C1/3081
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06—Treatment with inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/10—Treatment with macromolecular organic compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
    • 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
    • C01P2006/32—Thermal properties
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2217—Oxides; Hydroxides of metals of magnesium
    • C08K2003/2224—Magnesium hydroxide
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium

Definitions

  • the invention relates to a preparation method of highly dispersed and highly thermally conductive white carbon black.
  • White carbon black is a colorless, non-toxic, and amorphous fine powder. It has excellent properties such as small particle size, high specific surface area, high chemical purity, good dispersion performance, high temperature resistance and good electrical insulation. , Plastics, coatings and many other fields are widely used.
  • Michelin used white carbon black as a raw material to reduce the rolling resistance of tires by 35%, while also reducing automobile fuel consumption by 3% to 5%.
  • the dispersibility and thermal conductivity of silica play an important role in improving the "greening" of tires. Among them, the high thermal conductivity can quickly and efficiently dissipate the heat generated by the tire when the friction resistance is generated, so as to maintain the shape of the tire, reduce the resistance, and improve the safety.
  • silica with high dispersibility and high thermal conductivity there is little research on silica with high dispersibility and high thermal conductivity.
  • CN108439414A discloses a method for preparing highly dispersed large pore volume precipitated silica by a pH pendulum method. This method uses liquid sodium silicate and dilute sulfuric acid as raw materials, controls the pH value to swing back and forth from 11 ⁇ 1 to 5 ⁇ 1 for a total of 5 times, and then performs filter press washing, spray drying, and material manufacturing to obtain a dispersion/grade up to 9.5-10 high dispersion and large pore volume precipitated silica, due to the existence of a large number of pores, the thermal conductivity of the silica is poor.
  • the purpose of the present invention is to provide a method for preparing highly dispersed and highly thermally conductive silica.
  • a preparation method of high dispersion and high thermal conductivity white carbon black includes the following steps:
  • step (2) the mass percentage concentration of the surfactant in the mother liquor is 0.2-2%.
  • the surface active agent is a non-ionic surface active agent.
  • the non-ionic surfactant is octylphenol polyoxyethylene ether, nonylphenol polyoxyethylene ether and/or laureth polyoxyethylene ether.
  • step (2) aluminum salt is added at 0.2-2% of the mass of sodium silicate, and magnesium salt is added at 0.2-2% of the mass of sodium silicate.
  • the aluminum salt is aluminum sulfate or aluminum chloride
  • the magnesium salt is magnesium sulfate or magnesium chloride
  • the density of the sodium silicate solution is 1.1 to 1.25 g/cm 3
  • the modulus of sodium silicate is 2 to 4;
  • the acid solution is sulfuric acid with a concentration of 1 to 3 mol/L;
  • the pH value of the system is adjusted in a gradient from 5 to 11 according to the gradient of pH value 5 ⁇ 7 ⁇ 9 ⁇ 11, and react for 5-15 minutes after each adjustment;
  • the gradient adjustment of the pH value of the system from 11 to 5 is performed according to the gradient of pH value 11 ⁇ 9 ⁇ 7 ⁇ 5, and the reaction is 5-15 minutes after each adjustment.
  • a surfactant is added to the reaction system to prevent excessive agglomeration of primary particles and make the particle size of the aggregate produced uniform; at the same time, the purpose of adjusting the dispersion level of white carbon black is achieved through pH gradient adjustment.
  • the aluminum salt and magnesium salt are converted into aluminum hydroxide and magnesium hydroxide (after drying, it is further dehydrated and converted into aluminum oxide and magnesium oxide) and filled in the voids of the white carbon black aggregate by layer adsorption, so that the white carbon black can obtain high Dispersibility and high thermal conductivity, the thermal conductivity of the white carbon black of the present invention is above 15w/m ⁇ k, and the degree of dispersion is >9.7.
  • a preparation method of high dispersion and high thermal conductivity white carbon black includes the following steps:
  • step (2) the mass percentage concentration of the surfactant in the mother liquor is 0.2-2%.
  • the surfactant is a nonionic surfactant.
  • the non-ionic surfactant is octylphenol polyoxyethylene ether, nonylphenol polyoxyethylene ether and/or laureth polyoxyethylene ether.
  • step (2) aluminum salt is added at 0.2-2% of the mass of sodium silicate, and magnesium salt is added at 0.2-2% of the mass of sodium silicate.
  • the aluminum salt is aluminum sulfate or aluminum chloride
  • the magnesium salt is magnesium sulfate or magnesium chloride
  • the density of the sodium silicate solution is 1.1 to 1.25 g/cm 3 , and the modulus of the sodium silicate is 2 to 4;
  • the acid solution is sulfuric acid with a concentration of 1 to 3 mol/L;
  • the pH value of the system is adjusted in a gradient from 5 to 11 according to the gradient of pH value 5 ⁇ 7 ⁇ 9 ⁇ 11, and react for 5-15 minutes after each adjustment;
  • the gradient adjustment of the pH value of the system from 11 to 5 is performed according to the gradient of pH value 11 ⁇ 9 ⁇ 7 ⁇ 5, and the reaction is 5-15 minutes after each adjustment;
  • the reaction temperature is 70-90°C.
  • the drying temperature is 200 to 500°C.
  • the separation method can be filtration, pressure filtration, centrifugation, sedimentation, etc. In the separation process with washing to remove impurities.
  • the drying method can be spray drying and other conventional drying methods.
  • the present invention prepares vulcanized rubber filled with white carbon black according to HG/T 2404-2008, and evaluates the dispersion degree of white carbon black in rubber according to method D of GB/T 6030-2006.
  • the present invention measures the thermal conductivity of silica in accordance with GB/T 20671.10-2006.
  • a preparation method of high dispersion and high thermal conductivity white carbon black includes the following steps:
  • step (3) Add sodium silicate solution to the mother liquor of step (2), adjust the pH value of the system to 7, after reacting for 10 minutes, continue to add sodium silicate solution to adjust the pH value to 9, after reacting for 10 minutes, continue to add Adjust the pH value of sodium silicate solution to 11 and react for 10 minutes;
  • step (3) Add dilute sulfuric acid to the mother liquor treated in step (3), adjust the pH value of the system to 9, after reacting for 10 minutes, continue to add dilute sulfuric acid to adjust the pH to 7, and after reacting for 10 minutes, continue to add dilute sulfuric acid. Adjust the pH to 5 and react for 10 minutes;
  • Step (4) After the reaction is completed, the mother liquor is filtered and washed with a plate and frame filter, and then spray-dried (inlet temperature 300°C) to obtain high-dispersion and high-thermal-conductivity silica with thermal conductivity above 15w/m ⁇ k and dispersed Degree rating>9.7.
  • a preparation method of high dispersion and high thermal conductivity white carbon black includes the following steps:
  • step (3) Add sodium silicate solution to the mother liquor of step (2), adjust the pH value of the system to 7, after reacting for 10 minutes, continue to add sodium silicate solution to adjust the pH value to 9, after reacting for 10 minutes, continue to add Adjust the pH value of sodium silicate solution to 11 and react for 10 minutes;
  • step (3) Add dilute sulfuric acid to the mother liquor treated in step (3), adjust the pH value of the system to 9, after reacting for 10 minutes, continue to add dilute sulfuric acid to adjust the pH to 7, and after reacting for 10 minutes, continue to add dilute sulfuric acid. Adjust the pH to 5 and react for 10 minutes;
  • Step (4) After the reaction, the mother liquor is filtered and washed with a plate and frame filter, and then spray-dried (at an inlet temperature of 400°C) to obtain high-dispersion and high-conductivity silica with a thermal conductivity of 15w/m ⁇ k or more. Degree rating>9.7.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

本发明公开了一种高分散高导热白炭黑的制备方法，该方法包括以下步骤：(1)配制硅酸钠溶液和酸溶液；(2)向硅酸钠溶液中加入表面活性剂、铝盐、镁盐和酸溶液，至体系的pH值为5，得到母液；(3)向母液中加入硅酸钠溶液，将体系的pH值由5梯度调节至11，然后向母液中加入酸溶液，将体系的pH值由11梯度调节至5；(4)母液经分离、干燥，得到白炭黑。与现有技术相比，采用本发明方法制备的白炭黑导热系数在15w/m·k以上，分散度等级＞9.7。

Description

一种高分散高导热白炭黑的制备方法 技术领域
本发明涉及一种高分散高导热白炭黑的制备方法。
背景技术
白炭黑是一种无色、无毒、无定形的微细粉状物，具有粒径小，比表面积达、化学纯度高、分散性能好、耐高温和电绝缘性好等优异性能，在橡胶、塑料、涂料等诸多领域广泛应用。1992年米其林公司通过使用白炭黑为原料，使轮胎的滚动阻力降低了35％，同时还使汽车燃油消耗量降低了3％-5％。在上述应用中，白炭黑的分散性、导热性对提高轮胎的“绿色化”起着重要的作用。其中高导热性可使轮胎在产生摩擦阻力生成的热量被快速高效的散发掉，以保持轮胎的形状，降低阻力，提高安全性。但同时具有高分散性和高导热性的白炭黑研究较少。
CN108439414A公开了一种pH值摆法制备高分散大孔容沉淀二氧化硅的方法。该方法以液体硅酸钠和稀硫酸为原料，控制pH值从11±1至5±1之间来回摆动共5次，然后进行压滤洗涤、喷雾干燥、造料，得到分散度/级达9.5-10的高分散大孔容沉淀二氧化硅，由于大量孔隙的存在，使得该二氧化硅的导热性较差。
现有技术有通过添加导热性较好的Al 2O 3、ZnO、SiC填料等来提高橡胶的散热性能，但不同填料在橡胶中的分散性存在明显差异，与白炭黑的配合性差。
发明内容
根据上述现有技术的不足，本发明的目的在于提供一种高分散高导热白炭黑的制备方法。
为实现上述目的，本发明采用的技术方案如下：
一种高分散高导热白炭黑的制备方法，包括以下步骤：
(1)配制硅酸钠溶液和酸溶液；
(2)向硅酸钠溶液中加入表面活性剂、铝盐、镁盐和酸溶液，至体系的pH值为5，得到母液；
(3)向母液中加入硅酸钠溶液，将体系的pH值由5梯度调节至11，然后向母液中加入酸溶液，将体系的pH值由11梯度调节至5；
(4)母液经分离、干燥，得到白炭黑。
作为优选技术方案之一，步骤(2)中，所述的表面活性剂在母液中的质量百分比浓度为0.2～2％。
作为更进一步的优选技术方案之一，所述的表面活性剂为非离子型表面活性剂。
作为更进一步的优选技术方案之一，所述的非离子型表面活性剂为辛基酚聚氧乙烯醚、壬基酚聚氧乙烯醚和/或月桂醇聚氧乙烯醚。
作为优选技术方案之一，步骤(2)中，按硅酸钠质量的0.2～2％加入铝盐，按硅酸钠质量的0.2～2％加入镁盐。
作为更进一步的优选技术方案之一，所述铝盐为硫酸铝或氯化铝，所述镁盐为硫酸镁或氯化镁。
作为优选技术方案之一，所述的硅酸钠溶液的密度为1.1～1.25g/cm 3，硅酸钠的模数为2～4；
所述的酸溶液为浓度为1～3mol/L的硫酸；
所述的体系的pH值由5梯度调节至11是按pH值为5→7→9→11的梯度进行调节，每次调节后反应5～15min；
所述的体系的pH值由11梯度调节至5是按pH值为11→9→7→5的梯度进行调节，每次调节后反应5～15min。
本发明在反应体系中加入表面活性剂，防止原始粒子过度聚集，使生产的聚集体粒径均匀；同时通过pH值的梯度调节来达到调控白炭黑分散等级的目的，在pH梯度调节过程中，铝盐和镁盐转化成氢氧化铝和氢氧化镁(干燥后进一步脱水转化成氧化铝和氧化镁)并被层次吸附填充在白炭黑聚集体的空隙， 从而使得白炭黑同时获得高分散性和高导热性，本发明的白炭黑导热系数在15w/m·k以上，分散度等级＞9.7。
具体实施方式
下面通过具体实施例对本发明的具体技术方案作进一步地详细说明。
一种高分散高导热白炭黑的制备方法，包括以下步骤：
(1)配制硅酸钠溶液和酸溶液；
(2)向硅酸钠溶液中加入表面活性剂、铝盐、镁盐和酸溶液，至体系的pH值为5，得到母液；
(3)向母液中加入硅酸钠溶液，将体系的pH值由5梯度调节至11，然后向母液中加入酸溶液，将体系的pH值由11梯度调节至5；
(4)母液经分离、干燥，得到白炭黑。
在另一优选的技术方案中，步骤(2)中，所述的表面活性剂在母液中的质量百分比浓度为0.2～2％。
在另一优选的技术方案中，所述的表面活性剂为非离子型表面活性剂。
在另一优选的技术方案中，所述的非离子型表面活性剂为辛基酚聚氧乙烯醚、壬基酚聚氧乙烯醚和/或月桂醇聚氧乙烯醚。
在另一优选的技术方案中，步骤(2)中，按硅酸钠质量的0.2～2％加入铝盐，按硅酸钠质量的0.2～2％加入镁盐。
在另一优选的技术方案中，所述铝盐为硫酸铝或氯化铝，所述镁盐为硫酸镁或氯化镁。
在另一优选的技术方案中，所述的硅酸钠溶液的密度为1.1～1.25g/cm 3，硅酸钠的模数为2～4；
所述的酸溶液为浓度为1～3mol/L的硫酸；
所述的体系的pH值由5梯度调节至11是按pH值为5→7→9→11的梯度进行调节，每次调节后反应5～15min；
所述的体系的pH值由11梯度调节至5是按pH值为11→9→7→5的梯度进行调节，每次调节后反应5～15min；
反应温度为70～90℃。
干燥温度为200～500℃。
分离方式可采取过滤、压滤、离心、沉降等。在分离的过程中配合洗涤，以除去杂质。
干燥方式可采取喷雾干燥等常规的干燥方式。
本发明依HG/T 2404-2008制备填充有白炭黑的硫化橡胶，并依GB/T 6030-2006的方法D评估白炭黑在橡胶中的分散度等级。
本发明依GB/T 20671.10-2006测定白炭黑的导热系数。
实施例1
一种高分散高导热白炭黑的制备方法，包括以下步骤：
(1)将模数为2.2的硅酸钠用水溶解，配制成密度为1.17g/cm 3的硅酸钠溶液，将浓硫酸用水稀释配制成浓度为1mol/L的稀硫酸；
(2)将硅酸钠溶液加热至80℃后，在搅拌下，先向硅酸钠溶液中加入辛基酚聚氧乙烯醚、硫酸铝和硫酸镁，混匀后，再加入稀硫酸，至体系的pH值为5，反应10min，得到母液，辛基酚聚氧乙烯醚的质量浓度为0.5％，硫酸铝的用量为硅酸钠质量的1％，硫酸镁的用量为硅酸钠质量的1％；
(3)向步骤(2)的母液中加入硅酸钠溶液，将体系的pH值调节至7，反应10min后，继续加入硅酸钠溶液将pH值调节至9，反应10min后，再继续加入硅酸钠溶液将pH值调节至11，反应10min；
(4)向经步骤(3)处理的母液中加入稀硫酸，将体系的pH值调节至9，反应10min后，继续加稀硫酸将pH调节至7，反应10min后，再继续加稀硫酸将pH调节至5，反应10min；
(5)步骤(4)反应完毕后的母液用板框过滤机过滤洗涤，然后喷雾干燥(入口温度300℃)，得到高分散高导热白炭黑，导热系数在15w/m·k以上，分散度等级＞9.7。
实施例2
一种高分散高导热白炭黑的制备方法，包括以下步骤：
(1)将模数为3.7的硅酸钠用水溶解，配制成密度为1.20g/cm 3的硅酸钠溶液，将浓硫酸用水稀释配制成浓度为2.5mol/L的稀硫酸；
(2)将硅酸钠溶液加热至90℃后，在搅拌下，先向硅酸钠溶液中加入辛基酚聚氧乙烯醚、硫酸铝和硫酸镁，混匀后，再加入稀硫酸，至体系的pH值为5，反应10min，得到母液，辛基酚聚氧乙烯醚的质量浓度为0.5％，硫酸铝的用量为硅酸钠质量的1.5％，硫酸镁的用量为硅酸钠质量的0.5％；
(3)向步骤(2)的母液中加入硅酸钠溶液，将体系的pH值调节至7，反应10min后，继续加入硅酸钠溶液将pH值调节至9，反应10min后，再继续加入硅酸钠溶液将pH值调节至11，反应10min；
(4)向经步骤(3)处理的母液中加入稀硫酸，将体系的pH值调节至9，反应10min后，继续加稀硫酸将pH调节至7，反应10min后，再继续加稀硫酸将pH调节至5，反应10min；
(5)步骤(4)反应完毕后的母液用板框过滤机过滤洗涤，然后喷雾干燥(入口温度400℃)，得到高分散高导热白炭黑，导热系数在15w/m·k以上，分散度等级＞9.7。
最后应说明的是：以上所述仅为本发明的优选实施例而已，并不用于限制本发明，尽管参照前述实施例对本发明进行了详细的说明，对于本领域的技术人员来说，其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (8)

  1. 一种高分散高导热白炭黑的制备方法，包括以下步骤：
    (1)配制硅酸钠溶液和酸溶液；
    (2)向硅酸钠溶液中加入表面活性剂、铝盐、镁盐和酸溶液，至体系的pH值为5，得到母液；
    (3)向母液中加入硅酸钠溶液，将体系的pH值由5梯度调节至11，然后向母液中加入酸溶液，将体系的pH值由11梯度调节至5；
    (4)母液经分离、干燥，得到白炭黑。
  2. 根据权利要求1所述的制备方法，其特征在于：步骤(2)中，所述的表面活性剂在母液中的质量百分比浓度为0.2～2％。
  3. 根据权利要求2所述的制备方法，其特征在于：所述的表面活性剂为非离子型表面活性剂。
  4. 根据权利要求3所述的制备方法，其特征在于：所述的非离子型表面活性剂为辛基酚聚氧乙烯醚、壬基酚聚氧乙烯醚和/或月桂醇聚氧乙烯醚。
  5. 根据权利要求1所述的制备方法，其特征在于：步骤(2)中，按硅酸钠质量的0.2～2％加入铝盐，按硅酸钠质量的0.2～2％加入镁盐。
  6. 根据权利要求5所述的制备方法，其特征在于：所述铝盐为硫酸铝或氯化铝，所述镁盐为硫酸镁或氯化镁。
  7. 根据权利要求1至6任一所述的制备方法，其特征在于：
    所述的硅酸钠溶液的密度为1.1～1.25g/cm 3，硅酸钠的模数为2～4；
    所述的酸溶液为浓度为1～3mol/L的硫酸；
    所述的体系的pH值由5梯度调节至11是按pH值为5→7→9→11的梯度进行调节，每次调节后反应5～15min；
    所述的体系的pH值由11梯度调节至5是按pH值为11→9→7→5的梯度进行调节，每次调节后反应5～15min。
  8. 根据权利要求1所述的制备方法，其特征在于：步骤(4)中，干燥温度为200～500℃。
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