WO2023035098A1 - Procédé de préparation de noir de carbone blanc pour renforcement et son utilisation - Google Patents

Procédé de préparation de noir de carbone blanc pour renforcement et son utilisation Download PDF

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Publication number
WO2023035098A1
WO2023035098A1 PCT/CN2021/116856 CN2021116856W WO2023035098A1 WO 2023035098 A1 WO2023035098 A1 WO 2023035098A1 CN 2021116856 W CN2021116856 W CN 2021116856W WO 2023035098 A1 WO2023035098 A1 WO 2023035098A1
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Prior art keywords
treatment
preparation
carbon black
white carbon
reinforcement
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PCT/CN2021/116856
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English (en)
Chinese (zh)
Inventor
陈南飞
卢爱平
王明贺
陈辰
陈家树
史彤
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无锡恒诚硅业有限公司
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Priority to PCT/CN2021/116856 priority Critical patent/WO2023035098A1/fr
Priority to CN202180002655.0A priority patent/CN113924271B/zh
Publication of WO2023035098A1 publication Critical patent/WO2023035098A1/fr

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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
    • 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
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/22—Expanded, porous or hollow particles
    • C08K7/24—Expanded, porous or hollow particles inorganic
    • C08K7/26—Silicon- containing compounds
    • 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
    • C01P2006/12—Surface area
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/006—Additives being defined by their surface area
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
    • Y02T10/00—Road transport of goods or passengers
    • Y02T10/80—Technologies aiming to reduce greenhouse gasses emissions common to all road transportation technologies
    • Y02T10/86—Optimisation of rolling resistance, e.g. weight reduction 

Definitions

  • the present application relates to the field of white carbon black, in particular to a preparation method and application of white carbon black for reinforcement.
  • silica is widely used in various fields due to its good specific surface properties, and the preparation method of silica has obvious influence on its properties.
  • CN107140643A is a kind of preparation method of high-strength and easily dispersible white carbon black, it uses fluosilicic acid as silicon raw material, is ammoniation agent step by step to carry out ammoniation reaction with gas ammonia, and in the second ammoniation reaction With the addition of dispersant, the prepared white carbon black is easy to disperse and has high reinforcing performance.
  • CN1337355A discloses a method for producing high-reinforcing white carbon black by ammoniating sodium fluorosilicate.
  • the specific surface area of white carbon black obtained by the current process method is low, and the transparency and reinforcement in rubber compounds are poor, so it is difficult to be used as high-reinforcing white carbon black. Strong white carbon black is used, and the process is long and the production cost is high.
  • a Na 2 SiF 6 step-by-step ammoniation treatment process is proposed. Firstly, the total amount of 25-50% Na 2 SiF 6 and 5-20% ammonia water are reacted at 30-45°C, which is beneficial to the tiny glue core.
  • the product of this application can be adjusted within the range of 130-220m 2 /g, and the DBP oil absorption value can be adjusted within the range of 2.0-3.3.
  • the product can be used as a reinforcing material for shoemaking and tires.
  • the current white carbon black for reinforcement still has problems such as poor reinforcement performance and small specific surface area.
  • This application provides a preparation method and application of white carbon black for reinforcement. Through the adjustment of the process in the preparation process, the poor reinforcing performance and small specific surface area of the white carbon black for reinforcement prepared by the current process are solved. The problem.
  • the application provides a method for preparing white carbon black for reinforcement, the preparation method comprising the steps of:
  • step (2) performing the second treatment after mixing the slurry obtained in step (1) with the second treatment liquid, and obtaining the white carbon black for reinforcement through solid-liquid separation;
  • the first treatment liquid includes chloroacetic acid and ammonium citrate
  • the second treatment liquid includes hydrochloric acid and acetic acid.
  • the scheme provided by this application realizes the preparation of high-performance white carbon black through the design of the preparation process and multiple treatments with a specific composition, and the specific surface area of the prepared white carbon black can reach 200-230cm 2 /g At the same time, the reinforcing performance of silica when used as a reinforcing material is significantly improved, and the mechanical properties of rubber products after reinforcement have achieved a good improvement.
  • the combination of chloroacetic acid and ammonium citrate is used in the first treatment to pretreat the water glass solution to provide a good environment for the second treatment, and then high-performance white carbon can be directly obtained under the treatment of hydrochloric acid and acetic acid Black product, when used as a reinforcing material, the mechanical properties of the reinforced material are greatly improved.
  • the introduction of ammonium citrate can regulate the precipitation rate of silica and then reduce the content of impurity elements in the product
  • a specific combination of hydrochloric acid and acetic acid is used to reduce the amount of silica produced under an ammonia atmosphere. The aggregation between the particles ensures that the obtained silica has good dispersibility.
  • the modulus of the water glass solution described in step (1) is 1.5-2, such as can be 1.5, 1.6, 1.7, 1.8, 1.9 or 2, etc., but not limited to the numerical values listed, the Other unrecited combinations within the scope are also applicable.
  • the mol ratio of chloroacetic acid and ammonium citrate in the first treatment liquid described in step (1) is 1:(0.3-0.5), such as 1:0.3, 1:0.31, 1:0. 0.32, 1:0.33, 1:0.34, 1:0.35, 1:0.36, 1:0.37, 1:0.38, 1:0.39, 1:0.4, 1:0.41, 1:0.42, 1:0.43, 1:0.44, 1:0.45, 1:0.46, 1:0.47, 1:0.48, 1:0.49 or 1:0.5, etc., but not limited to the listed values, other unlisted combinations within this range are also applicable.
  • the volume ratio of the water glass solution and the first treatment liquid in step (1) is 1:(2-3), such as 1:2, 1:2.1, 1:2.2, 1:2.3, 1:2.4, 1:2.5, 1:2.6, 1:2.7, 1:2.8, 1:2.9 or 1:3, etc., but not limited to the listed values, other unlisted combinations within this range are also applicable.
  • the first treatment in step (1) is carried out under a protective atmosphere.
  • the gas in the protective atmosphere includes carbon dioxide gas.
  • the first treatment can control the hydrolysis speed of silicon element in the solution under the protective atmosphere of carbon dioxide gas, and at the same time cooperate with the treatment liquid to make the liquid phase reach a good liquid phase condition after the first treatment of the liquid phase, which is the next second treatment.
  • a good foundation is laid and the pre-precipitation of silicon in the liquid phase is realized.
  • the volume content of carbon dioxide gas in the protective atmosphere is 2-7%, such as 2%, 2.2%, 2.4%, 2.6%, 2.8%, 3%, 3.2%, 3.4%, 3.6%, 3.8% %, 4%, 4.2%, 4.4%, 4.6%, 4.8%, 5%, 5.2%, 5.4%, 5.6%, 5.8%, 6%, 6.2%, 6.4%, 6.6%, 6.8% or 7%, etc. , but not limited to the listed values, other unlisted combinations within this range are also applicable.
  • the remaining gas volume can be made up with other inert components, such as nitrogen, helium or argon.
  • the temperature of the first treatment in step (1) is 70-90°C, for example, it can be 70°C, 71°C, 72°C, 73°C, 74°C, 75°C, 76°C, 77°C °C, 78 °C, 79 °C, 80 °C, 81 °C, 82 °C, 83 °C, 84 °C, 85 °C, 86 °C, 87 °C, 88 °C, 89 °C or 90 °C, etc., but not limited to the listed values, Other unrecited combinations within this range are also applicable.
  • the first treatment time in step (1) is 70-90min, for example, 70min, 71min, 72min, 73min, 74min, 75min, 76min, 77min, 78min, 79min, 80min, 81min, 82min, 83min, 84min, 85min, 86min, 87min, 88min, 89min or 90min, etc., but not limited to the listed values, other unlisted combinations within this range are also applicable.
  • the volume ratio of the slurry and the second treatment liquid in step (2) is 1:(1.2-1.5), such as 1:1.2, 1:1.21, 1:1.22, 1 :1.23, 1:1.24, 1:1.25, 1:1.26, 1:1.27, 1:1.28, 1:1.29, 1:1.3, 1:1.31, 1:1.32, 1:1.33, 1:1.34, 1:1.35 , 1:1.36, 1:1.38, 1:1.4, 1:1.42, 1:1.44, 1:1.46, 1:1.48 or 1:1.5, etc., but not limited to the listed values, other unlisted combinations The same applies.
  • the molar ratio of hydrochloric acid and acetic acid in the second treatment liquid described in step (2) is 1:(1.2-1.5), such as can be 1:1.2, 1:1.21, 1:1.22, 1:1.23, 1: 1.24, 1:1.25, 1:1.26, 1:1.27, 1:1.28, 1:1.29, 1:1.3, 1:1.31, 1:1.32, 1:1.33, 1:1.34, 1:1.35, 1:1.36, 1:1.38, 1:1.4, 1:1.42, 1:1.44, 1:1.46, 1:1.48 or 1:1.5, etc., but not limited to the listed values, other unlisted combinations within this range are also applicable.
  • the second treatment in step (2) is carried out under an ammonia atmosphere.
  • the content of ammonia in the ammonia atmosphere is 25-30%, such as 25%, 25.2%, 25.4%, 25.6%, 25.8%, 26%, 26.2%, 26.4%, 26.8%, 27% %, 27.2%, 27.4%, 27.6%, 27.8%, 28%, 28.2%, 28.4%, 28.6%, 28.8%, 29%, 29.2%, 29.4%, 29.6%, 29.8% or 30%, etc., but not Limited to the listed values, other unlisted combinations within this range are also applicable.
  • the remaining gas volume can be made up with other inert components, such as nitrogen, helium or argon.
  • the introduction of ammonia gas atmosphere in the second treatment ensures that the silica formed in the second treatment has a good structure, avoids the aggregation of silica, and ensures that the prepared Silica has good dispersion performance and specific surface area.
  • the temperature of the second treatment in step (2) is 120-150°C, for example, it can be 120°C, 122°C, 124°C, 126°C, 128°C, 130°C, 132°C, 134°C °C, 136 °C, 138 °C, 140 °C, 142 °C, 144 °C, 146 °C, 148 °C or 150 °C, etc., but not limited to the listed values, and other unlisted combinations within this range are also applicable.
  • the time for the second treatment in step (2) is 30-45min, such as 30min, 31min, 32min, 33min, 34min, 35min, 36min, 37min, 38min, 39min, 40min, 41min, 42min, 43min, 44min or 45min, etc., but not limited to the listed values, other unlisted combinations within this range are also applicable.
  • the preparation method includes the following steps:
  • step (2) performing the second treatment after mixing the slurry obtained in step (1) with the second treatment liquid, and obtaining the white carbon black for reinforcement through solid-liquid separation;
  • the modulus of the water glass solution described in step (1) is 1.5-2;
  • the first treatment solution includes chloroacetic acid and ammonium citrate;
  • the mol ratio of chloroacetic acid and ammonium citrate in the first treatment solution is 1:(0.3-0.5);
  • the volume ratio of the water glass solution and the first treatment liquid is 1:(2-3);
  • the first treatment is carried out under a protective atmosphere;
  • the gas of the protective atmosphere includes Carbon dioxide gas;
  • the volume content of carbon dioxide gas in the protective atmosphere is 2-7%;
  • the temperature of the first treatment is 70-90°C;
  • the time of the first treatment is 70-90min;
  • the volume ratio of the slurry and the second treatment solution in step (2) is 1:(1.2-1.5); the second treatment solution includes hydrochloric acid and acetic acid; the mol ratio of hydrochloric acid and acetic acid in the second treatment solution It is 1: (1.2-1.5); the second treatment is carried out under an ammonia atmosphere; the content of ammonia in the ammonia atmosphere is 25-30%; the temperature of the second treatment is 120-150°C; The time of the second treatment is 30-45min.
  • the present application provides the application of the white carbon black for reinforcement obtained by the preparation method described in the first aspect, and the white carbon black for reinforcement is used for reinforcing rubber products.
  • the scheme provided by this application realizes the preparation of high-performance white carbon black through the design of the preparation process and multiple treatments with specific compositions, and the specific surface area of the prepared white carbon black can reach 200-230cm 2 /g, and at the same time, the reinforcing performance of silica when used as a reinforcing material is significantly improved, and the mechanical properties of rubber products after reinforcement have achieved a good improvement.
  • the reinforcement performance of the obtained silica is further enhanced by introducing specific atmosphere assistance in the multiple treatment processes.
  • the hardness JIS can reach more than 90
  • the tensile strength can reach more than 18.2MPa
  • the elongation can reach more than 660.5%.
  • This embodiment provides a preparation method of white carbon black for reinforcement, the preparation method comprising the following steps:
  • step (2) performing the second treatment after mixing the slurry obtained in step (1) with the second treatment liquid, and obtaining the white carbon black for reinforcement through solid-liquid separation;
  • the modulus of the described water glass solution of step (1) is 1.7; Described the first processing liquid comprises chloroacetic acid and ammonium citrate; The mol ratio of chloroacetic acid and ammonium citrate is 1:0.4 in the described first processing liquid; The volume ratio of the water glass solution and the first treatment liquid is 1:2.5; the first treatment is carried out under a protective atmosphere; the gas of the protective atmosphere includes carbon dioxide gas; the volume of carbon dioxide gas in the protective atmosphere The content is 4%; the temperature of the first treatment is 80°C; the time of the first treatment is 80min;
  • the volume ratio of the slurry and the second treatment solution in step (2) is 1:1.35; the second treatment solution includes hydrochloric acid and acetic acid; the molar ratio of hydrochloric acid and acetic acid in the second treatment solution is 1:1.35
  • the second treatment is carried out under an ammonia atmosphere; the content of ammonia in the ammonia atmosphere is 27%; the temperature of the second treatment is 130° C.; the time of the second treatment is 37 minutes.
  • This embodiment provides a preparation method of white carbon black for reinforcement, the preparation method comprising the following steps:
  • step (2) performing the second treatment after mixing the slurry obtained in step (1) with the second treatment liquid, and obtaining the white carbon black for reinforcement through solid-liquid separation;
  • the modulus of the described water glass solution of step (1) is 2; Described the first processing liquid comprises chloroacetic acid and ammonium citrate; The mol ratio of chloroacetic acid and ammonium citrate is 1:0.5 in the described first processing liquid; The volume ratio of the water glass solution and the first treatment liquid is 1:2; the first treatment is carried out under a protective atmosphere; the gas of the protective atmosphere includes carbon dioxide gas; the volume of carbon dioxide gas in the protective atmosphere The content is 2%; the temperature of the first treatment is 70°C; the time of the first treatment is 90min;
  • the volume ratio of the slurry and the second treatment solution in step (2) is 1:1.5; the second treatment solution includes hydrochloric acid and acetic acid; the molar ratio of hydrochloric acid and acetic acid in the second treatment solution is 1:1.2 ;
  • the second treatment is carried out under an ammonia atmosphere; the content of ammonia in the ammonia atmosphere is 25%; the temperature of the second treatment is 150° C.; the time of the second treatment is 45 minutes.
  • This embodiment provides a preparation method of white carbon black for reinforcement, the preparation method comprising the following steps:
  • step (2) performing the second treatment after mixing the slurry obtained in step (1) with the second treatment liquid, and obtaining the white carbon black for reinforcement through solid-liquid separation;
  • the modulus of the described water glass solution of step (1) is 1.5; Described the first processing liquid comprises chloroacetic acid and ammonium citrate; The mol ratio of chloroacetic acid and ammonium citrate is 1:0.5 in the described first processing liquid; The volume ratio of the water glass solution and the first treatment liquid is 1:3; the first treatment is carried out under a protective atmosphere; the gas of the protective atmosphere includes carbon dioxide gas; the volume of carbon dioxide gas in the protective atmosphere The content is 7%; the temperature of the first treatment is 90°C; the time of the first treatment is 70min;
  • the volume ratio of the slurry and the second treatment solution in step (2) is 1:1.2; the second treatment solution includes hydrochloric acid and acetic acid; the molar ratio of hydrochloric acid and acetic acid in the second treatment solution is 1:1.5 ;
  • the second treatment is carried out under an ammonia atmosphere; the content of ammonia in the ammonia atmosphere is 30%; the temperature of the second treatment is 120° C.; the time of the second treatment is 30 minutes.
  • This embodiment provides a preparation method of white carbon black for reinforcement, the preparation method comprising the following steps:
  • step (2) performing the second treatment after mixing the slurry obtained in step (1) with the second treatment liquid, and obtaining the white carbon black for reinforcement through solid-liquid separation;
  • the modulus of the described water glass solution of step (1) is 1.85; Described the first processing liquid comprises chloroacetic acid and ammonium citrate; The mol ratio of chloroacetic acid and ammonium citrate is 1:0.44 in the described first processing liquid; The volume ratio of the water glass solution and the first treatment liquid is 1:2.2; the first treatment is carried out under a protective atmosphere; the gas of the protective atmosphere includes carbon dioxide gas; the volume of carbon dioxide gas in the protective atmosphere The content is 5.5%; the temperature of the first treatment is 77°C; the time of the first treatment is 88min;
  • the volume ratio of the slurry and the second treatment solution in step (2) is 1:1.33; the second treatment solution includes hydrochloric acid and acetic acid; the molar ratio of hydrochloric acid and acetic acid in the second treatment solution is 1:1.44
  • the second treatment is carried out under an ammonia atmosphere; the content of ammonia in the ammonia atmosphere is 28%; the temperature of the second treatment is 140° C.; the time of the second treatment is 42 minutes.
  • Example 1 The difference from Example 1 is only that the first treatment solution in step (1) is replaced with sulfuric acid of the same concentration and the same amount, and the performance and application effect of the obtained white carbon black for reinforcement are shown in Table 1.
  • Example 1 The difference from Example 1 is only that the second treatment liquid in step (2) is replaced with sulfuric acid of the same concentration and the same amount, and the performance and application effect of the obtained white carbon black for reinforcement are shown in Table 1.
  • Example 1 The difference from Example 1 is only that the protective atmosphere in the first treatment in step (1) does not contain carbon dioxide gas, and the same amount of ammonia gas is used instead, the performance and application effect of the obtained reinforcing silica See Table 1 for details.
  • Example 1 The difference from Example 1 is only that the protective atmosphere in the second treatment in step (1) does not contain ammonia, and is replaced by inert gas argon, and the performance and application effect of the obtained white carbon black for reinforcement are detailed in Table 1.
  • Example 1 The difference from Example 1 is only that the acetic acid in step (2) is replaced with sulfuric acid of the same concentration and the same amount, and the performance and application effect of the obtained white carbon black for reinforcement are shown in Table 1.
  • Example 1 The difference from Example 1 is only that the chloroacetic acid in step (1) is replaced by an equivalent amount of hydrochloric acid, and the properties and application effects of the obtained reinforcing silica are shown in Table 1.
  • the scheme provided by the present application realizes the preparation of high-performance white carbon black through the design of the preparation process and the treatment of specific compositions for multiple times, and the prepared white carbon black
  • the specific surface area can reach 200-230cm 2 /g, and at the same time, the reinforcing performance of silica when used as a reinforcing material is significantly improved, and the mechanical properties of rubber products after reinforcement have been well improved.

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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)
  • Tires In General (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

Procédé de préparation de noir de carbone blanc pour renforcement et son utilisation. Le procédé de préparation comprend les étapes suivantes consistant : (1) à mélanger une solution de verre soluble avec un premier liquide de traitement, puis à la soumettre à un premier traitement pour obtenir une suspension épaisse, le premier liquide de traitement comprenant de l'acide chloroacétique et du citrate d'ammonium ; et (2) à mélanger la suspension épaisse obtenue à l'étape (1) avec un second liquide de traitement, puis à la soumettre à un second traitement suivi d'une séparation solide-liquide pour obtenir du noir de carbone blanc pour renforcement, le second liquide de traitement comprenant de l'acide chlorhydrique et de l'acide acétique. Au moyen de la conception du procédé de préparation, la préparation du noir de carbone blanc à haute performance est réalisée au moyen d'un traitement secondaire à l'aide de liquides de traitement présentant des constituants spécifiques. La surface spécifique du noir de carbone blanc préparé peut atteindre 200 à 230 cm2/g, et la performance de renforcement du noir de carbone blanc lorsqu'elle est utilisée en tant que matériau de renforcement est également considérablement améliorée. Les propriétés mécaniques des produits en caoutchouc après renforcement sont améliorées.
PCT/CN2021/116856 2021-09-07 2021-09-07 Procédé de préparation de noir de carbone blanc pour renforcement et son utilisation WO2023035098A1 (fr)

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PCT/CN2021/116856 WO2023035098A1 (fr) 2021-09-07 2021-09-07 Procédé de préparation de noir de carbone blanc pour renforcement et son utilisation
CN202180002655.0A CN113924271B (zh) 2021-09-07 2021-09-07 一种补强用白炭黑的制备方法及应用

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CN1807239A (zh) * 2006-02-09 2006-07-26 侯振海 沉淀法生产白炭黑的新工艺
CN102320615B (zh) * 2011-09-11 2015-11-18 中国科学院过程工程研究所 一种以微硅粉为原料碳化制备沉淀白炭黑的方法
CN103922346B (zh) * 2013-01-14 2016-05-18 上海华明高技术（集团）有限公司 高分散沉淀白炭黑的制备方法

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Publication number Priority date Publication date Assignee Title
US20100083876A1 (en) * 2006-06-27 2010-04-08 Pierre-Yves Lahary Precipitated silica and paper industry/other applications thereof
CN103936015A (zh) * 2014-04-28 2014-07-23 北京化工大学 一种喷雾法制备白炭黑浆液的方法
CN109231222A (zh) * 2018-11-05 2019-01-18 无锡恒诚硅业有限公司 一种高结构性、高补强的白炭黑及其制备方法和应用
CN109231223A (zh) * 2018-11-05 2019-01-18 无锡恒诚硅业有限公司 一种高结构性、高补强白炭黑及其制备方法和应用
CN111440358A (zh) * 2020-05-07 2020-07-24 江苏麒祥高新材料有限公司 一种用于橡胶补强纳米二氧化硅及其制备方法
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